data_{[Co(tmphen)2]3[Fe(CN)6]2}_30K #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author ; Kim R. Dunbar Department of Chemistry Texas A&M University, College Station, TX United States of America ; _publ_contact_author_email 'dunbar@mail.chem.tamu.edu' _publ_contact_author_fax '(979)845-7177' _publ_contact_author_phone '(979)845-5235' _publ_requested_journal 'Journal of the American Chemical Society' _publ_requested_category 'Coordination Chemistry' _publ_requested_coeditor_name ? _publ_contact_letter ; ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; 'A Charge-Transfer-Induced Spin-Transition in a Discrete Complex: The Role of Extrinsic Factors in Stabilizing Three Electronic Isomeric Forms of a Cyanide-Bridged Co/Fe Cluster' ; loop_ _publ_author_name _publ_author_address 'Berlinguette, Curtis P.' ; Department of Chemistry Texas A&M University, College Station, TX United States of America ; 'Dragulescu-Andrasi, Alina' ; Department of Chemistry Carnegie Mellon University, Pittsburgh, PA United States of America ; 'Achim, Catalina' ; Department of Chemistry Carnegie Mellon University, Pittsburgh, PA United States of America ; 'Sieber, Andreas' ; Department of Chemistry and Biochemistry University of Berne, Berne Switzerland ; 'Gudel, Hans-Ulrich' ; Department of Chemistry and Biochemistry University of Berne, Berne Switzerland ; 'Dunbar, Kim R.' ; Department of Chemistry Texas A&M University, College Station, TX United States of America ; #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; '((Co(tmphen)2)3(Fe(CN)6)2).9H2O ; _chemical_name_common '((Co(tmphen)2)3(Fe(CN)6)2).9H2O' _chemical_melting_point ? _chemical_formula_moiety 'C108 H114 Co3 Fe2 N24 O9' _chemical_formula_sum 'C108 H114 Co3 Fe2 N24 O9' _chemical_formula_weight 2180.7 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.940(10) _cell_length_b 24.79(2) _cell_length_c 24.330(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.77(9) _cell_angle_gamma 90.00 _cell_volume 11319(12) _cell_formula_units_Z 4 _cell_measurement_temperature 30(2) _cell_measurement_reflns_used 11827 _cell_measurement_theta_min 2.195 _cell_measurement_theta_max 22.05 _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4468 _exptl_absorpt_coefficient_mu 0.745 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8653 _exptl_absorpt_correction_T_max 0.9029 _exptl_absorpt_process_details 'SADABS: Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 30(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART 1000' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60425 _diffrn_reflns_av_R_equivalents 0.1374 _diffrn_reflns_av_sigmaI/netI 0.1156 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 20.82 _reflns_number_total 11827 _reflns_number_gt 5841 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER, 2000)' _computing_cell_refinement 'SAINT (BRUKER, 2001)' _computing_data_reduction 'SAINT (BRUKER, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00031(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11827 _refine_ls_number_parameters 1371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2097 _refine_ls_R_factor_gt 0.1255 _refine_ls_wR_factor_ref 0.3514 _refine_ls_wR_factor_gt 0.3021 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.136 _refine_ls_shift/su_mean 0.008 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.06313(6) 0.37308(5) 0.61708(5) 0.0717(4) Uani 1 1 d . A -1 Co2 Co 0.29577(6) 0.36817(4) 0.83339(5) 0.0679(4) Uani 1 1 d . A -1 Co3 Co 0.35841(6) 0.54742(4) 0.66339(5) 0.0618(4) Uani 1 1 d . A -1 Fe1 Fe 0.32540(6) 0.35220(5) 0.63610(5) 0.0701(4) Uani 1 1 d . A -1 Fe2 Fe 0.14588(7) 0.51918(5) 0.75611(5) 0.0764(4) Uani 1 1 d . A -1 O1S O 0.2998(8) 0.5249(6) 0.9806(6) 0.119(5) Uiso 0.50 1 d P B -1 O2S O 0.2766(8) 0.6700(6) 0.9400(6) 0.131(5) Uiso 0.50 1 d P C -2 O3S O 0.3592(18) 0.7289(13) 0.8863(13) 0.149(11) Uiso 0.25 1 d P D -3 O4S O 0.272(3) 0.754(2) 0.823(2) 0.24(2) Uiso 0.25 1 d P E -4 O5S O -0.0681(11) 0.5855(8) 0.8633(8) 0.071(6) Uiso 0.25 1 d P F -5 O6S O -0.1394(14) 0.5719(10) 0.8426(10) 0.107(8) Uiso 0.25 1 d P G -6 O7S O 0.2669(8) 0.6814(6) 0.7930(6) 0.133(5) Uiso 0.50 1 d P H -7 O8S O -0.1352(14) 0.4619(10) 0.7680(10) 0.107(8) Uiso 0.25 1 d P I -8 O9S O 0.2164(11) 0.7116(8) 0.6916(8) 0.189(8) Uiso 0.50 1 d P J -9 O10S O 0.2059(19) 0.8044(14) 0.6159(14) 0.164(13) Uiso 0.25 1 d P K -10 O11S O 0.2606(18) 0.8089(13) 0.5496(13) 0.148(12) Uiso 0.25 1 d P L -11 O12S O -0.212(2) 0.0478(14) 0.4362(15) 0.171(14) Uiso 0.25 1 d P M -12 O13S O -0.144(2) 0.0537(14) 0.4215(14) 0.167(13) Uiso 0.25 1 d P N -13 O14S O 0.4472(16) 0.2256(12) 0.5528(12) 0.130(10) Uiso 0.25 1 d P O -14 O15S O 0.6350(12) 0.3365(9) 0.6606(9) 0.077(6) Uiso 0.25 1 d P P -15 O16S O 0.6453(11) 0.3694(9) 0.6761(9) 0.073(6) Uiso 0.25 1 d P Q -16 O17S O 0.6270(12) 0.3988(9) 0.6836(9) 0.075(7) Uiso 0.25 1 d P R -17 O19S O 0.7337(16) 0.3842(12) 0.7634(12) 0.135(11) Uiso 0.25 1 d P S -19 O20S O 0.3130(10) 0.1872(7) 0.9060(7) 0.054(5) Uiso 0.25 1 d P T -20 O21S O 0.5309(9) 0.2901(7) 1.0734(7) 0.153(6) Uiso 0.50 1 d P U -21 O22S O 0.7946(19) 0.5700(14) 0.8071(14) 0.156(12) Uiso 0.25 1 d P V -22 O23S O 0.7688(16) 0.5666(12) 0.7441(12) 0.132(10) Uiso 0.25 1 d P W -23 O24S O 0.7346(18) 0.5959(14) 0.7080(14) 0.155(12) Uiso 0.25 1 d P X -24 O26S O 0.1229(7) 0.4845(5) 0.9264(5) 0.114(4) Uiso 0.50 1 d P Y -26 O27S O 0.0868(8) 0.4436(6) 0.9681(6) 0.138(5) Uiso 0.50 1 d P Z -27 O28S O 0.0706(9) 0.4178(7) 1.0014(7) 0.146(6) Uiso 0.50 1 d P A -28 O29S O 0.2297(16) 0.8264(12) 0.5883(13) 0.125(10) Uiso 0.25 1 d P B -29 O30S O 0.6946(11) 0.6760(8) 0.7346(8) 0.066(6) Uiso 0.25 1 d P C -30 N1 N 0.3097(4) 0.3246(3) 0.5122(3) 0.097(3) Uani 1 1 d . A -1 N2 N 0.3248(4) 0.2311(3) 0.6546(4) 0.107(3) Uani 1 1 d . A -1 N3 N 0.4882(4) 0.3597(3) 0.6391(3) 0.092(3) Uani 1 1 d . A -1 N4 N 0.1621(3) 0.3432(3) 0.6284(3) 0.076(2) Uani 1 1 d . A -1 N5 N 0.3271(3) 0.3684(2) 0.7615(3) 0.077(2) Uani 1 1 d . A -1 N6 N 0.3303(3) 0.4761(3) 0.6313(3) 0.066(2) Uani 1 1 d . A -1 N7 N 0.0953(3) 0.4429(3) 0.6592(3) 0.078(2) Uani 1 1 d . A -1 N8 N 0.2194(3) 0.4198(2) 0.8123(3) 0.067(2) Uani 1 1 d . A -1 N9 N 0.2834(4) 0.5446(2) 0.7091(3) 0.066(2) Uani 1 1 d . A -1 N10 N 0.0942(4) 0.6243(3) 0.6941(3) 0.103(3) Uani 1 1 d . A -1 N11 N -0.0014(5) 0.4957(5) 0.7950(4) 0.163(4) Uani 1 1 d . A -1 N12 N 0.1985(5) 0.5845(3) 0.8617(3) 0.115(3) Uani 1 1 d . A -1 N13 N 0.0729(3) 0.3956(2) 0.5349(3) 0.068(2) Uani 1 1 d . A -1 N14 N -0.0376(3) 0.4080(3) 0.5874(3) 0.071(2) Uani 1 1 d . A -1 N15 N 0.0139(3) 0.2973(3) 0.5903(2) 0.069(2) Uani 1 1 d . A -1 N16 N 0.0321(4) 0.3410(3) 0.6885(3) 0.088(3) Uani 1 1 d . A -1 N17 N 0.2290(4) 0.3057(3) 0.8110(3) 0.075(2) Uani 1 1 d . A -1 N18 N 0.2638(4) 0.3570(3) 0.9055(3) 0.094(3) Uani 1 1 d . A -1 N19 N 0.3784(4) 0.3227(3) 0.8613(3) 0.097(3) Uani 1 1 d . A -1 N20 N 0.3635(4) 0.4265(3) 0.8609(3) 0.078(2) Uani 1 1 d . A -1 N21 N 0.4342(3) 0.5193(2) 0.7223(3) 0.065(2) Uani 1 1 d . A -1 N22 N 0.3957(3) 0.6184(2) 0.6983(3) 0.069(2) Uani 1 1 d . A -1 N23 N 0.4303(3) 0.5520(2) 0.6124(3) 0.074(2) Uani 1 1 d . A -1 N24 N 0.3026(3) 0.5904(3) 0.6037(3) 0.075(2) Uani 1 1 d . A -1 C1 C 0.3168(5) 0.3351(4) 0.5588(4) 0.090(4) Uani 1 1 d . A -1 C2 C 0.3258(5) 0.2777(4) 0.6454(4) 0.089(3) Uani 1 1 d . A -1 C3 C 0.4268(4) 0.3547(3) 0.6398(3) 0.071(3) Uani 1 1 d . A -1 C4 C 0.2241(5) 0.3484(3) 0.6310(3) 0.069(3) Uani 1 1 d . A -1 C5 C 0.3290(4) 0.3635(3) 0.7135(4) 0.077(3) Uani 1 1 d . A -1 C6 C 0.3261(4) 0.4286(3) 0.6292(3) 0.064(3) Uani 1 1 d . A -1 C7 C 0.1157(4) 0.4747(3) 0.6948(3) 0.069(3) Uani 1 1 d . A -1 C8 C 0.1877(4) 0.4572(3) 0.7914(3) 0.073(3) Uani 1 1 d . A -1 C9 C 0.2317(5) 0.5338(3) 0.7295(3) 0.069(3) Uani 1 1 d . A -1 C10 C 0.1108(5) 0.5835(4) 0.7197(4) 0.089(3) Uani 1 1 d . A -1 C11 C 0.0548(6) 0.5057(4) 0.7798(4) 0.112(4) Uani 1 1 d . A -1 C12 C 0.1767(5) 0.5589(4) 0.8193(4) 0.098(3) Uani 1 1 d . A -1 C13 C 0.4951(4) 0.5320(3) 0.6142(4) 0.076(3) Uani 1 1 d . A -1 H13 H 0.5117 0.5118 0.6466 0.091 Uiso 1 1 calc R A -1 C14 C 0.5416(5) 0.5361(3) 0.5767(4) 0.079(3) Uani 1 1 d . A -1 C15 C 0.5189(4) 0.5644(3) 0.5280(4) 0.073(3) Uani 1 1 d . A -1 C16 C 0.4489(5) 0.5872(3) 0.5216(4) 0.080(3) Uani 1 1 d . A -1 C17 C 0.4214(5) 0.6189(3) 0.4754(4) 0.086(3) Uani 1 1 d . A -1 H17 H 0.4490 0.6242 0.4461 0.104 Uiso 1 1 calc R A -1 C18 C 0.3532(6) 0.6428(4) 0.4724(4) 0.101(4) Uani 1 1 d . A -1 H18 H 0.3361 0.6641 0.4409 0.121 Uiso 1 1 calc R A -1 C19 C 0.3088(5) 0.6360(4) 0.5156(3) 0.082(3) Uani 1 1 d . A -1 C20 C 0.2408(5) 0.6592(4) 0.5169(3) 0.084(3) Uani 1 1 d . A -1 C21 C 0.2063(5) 0.6484(3) 0.5602(3) 0.076(3) Uani 1 1 d . A -1 C22 C 0.2371(5) 0.6117(4) 0.6021(4) 0.086(3) Uani 1 1 d . A -1 H22 H 0.2096 0.6018 0.6304 0.103 Uiso 1 1 calc R A -1 C23 C 0.3373(4) 0.6029(3) 0.5624(3) 0.069(3) Uani 1 1 d . A -1 C24 C 0.4088(4) 0.5801(3) 0.5662(3) 0.065(3) Uani 1 1 d . A -1 C25 C 0.6137(4) 0.5137(4) 0.5872(5) 0.112(4) Uani 1 1 d . A -1 H25A H 0.6188 0.4848 0.5605 0.167 Uiso 1 1 calc R A -1 H25B H 0.6221 0.4992 0.6250 0.167 Uiso 1 1 calc R A -1 H25C H 0.6485 0.5422 0.5831 0.167 Uiso 1 1 calc R A -1 C26 C 0.5668(5) 0.5703(4) 0.4840(4) 0.109(4) Uani 1 1 d . A -1 H26A H 0.6069 0.5939 0.4975 0.164 Uiso 1 1 calc R A -1 H26B H 0.5399 0.5860 0.4506 0.164 Uiso 1 1 calc R A -1 H26C H 0.5848 0.5347 0.4751 0.164 Uiso 1 1 calc R A -1 C27 C 0.2084(5) 0.6957(4) 0.4721(4) 0.113(4) Uani 1 1 d . A -1 H27A H 0.1575 0.6876 0.4633 0.170 Uiso 1 1 calc R A -1 H27B H 0.2318 0.6904 0.4390 0.170 Uiso 1 1 calc R A -1 H27C H 0.2144 0.7332 0.4845 0.170 Uiso 1 1 calc R A -1 C28 C 0.1331(4) 0.6725(4) 0.5676(4) 0.089(3) Uani 1 1 d . A -1 H28A H 0.1374 0.7117 0.5719 0.133 Uiso 1 1 calc R A -1 H28B H 0.1166 0.6569 0.6006 0.133 Uiso 1 1 calc R A -1 H28C H 0.0987 0.6641 0.5348 0.133 Uiso 1 1 calc R A -1 C29 C 0.3743(5) 0.6688(3) 0.6872(4) 0.087(3) Uani 1 1 d . A -1 H29 H 0.3322 0.6745 0.6619 0.104 Uiso 1 1 calc R A -1 C30 C 0.4106(5) 0.7132(3) 0.7109(4) 0.094(4) Uani 1 1 d . A -1 C31 C 0.4712(5) 0.7092(3) 0.7444(4) 0.108(4) Uani 1 1 d . A -1 C32 C 0.4955(5) 0.6557(3) 0.7590(4) 0.094(4) Uani 1 1 d . A -1 C33 C 0.5593(5) 0.6431(4) 0.7944(4) 0.108(4) Uani 1 1 d . A -1 H33 H 0.5862 0.6717 0.8128 0.130 Uiso 1 1 calc R A -1 C34 C 0.5833(6) 0.5914(3) 0.8031(4) 0.107(4) Uani 1 1 d . A -1 H34 H 0.6292 0.5851 0.8230 0.129 Uiso 1 1 calc R A -1 C35 C 0.5404(5) 0.5473(3) 0.7826(4) 0.081(3) Uani 1 1 d . A -1 C36 C 0.5614(5) 0.4922(3) 0.7923(4) 0.091(4) Uani 1 1 d . A -1 C37 C 0.5147(5) 0.4532(3) 0.7701(3) 0.075(3) Uani 1 1 d . A -1 C38 C 0.4518(4) 0.4677(3) 0.7347(3) 0.066(3) Uani 1 1 d . A -1 H38 H 0.4209 0.4399 0.7191 0.080 Uiso 1 1 calc R A -1 C39 C 0.4780(4) 0.5582(3) 0.7465(3) 0.068(3) Uani 1 1 d . A -1 C40 C 0.4563(4) 0.6113(3) 0.7341(4) 0.071(3) Uani 1 1 d . A -1 C41 C 0.3752(6) 0.7695(4) 0.6951(5) 0.121(4) Uani 1 1 d . A -1 H41A H 0.3551 0.7841 0.7270 0.181 Uiso 1 1 calc R A -1 H41B H 0.3372 0.7650 0.6638 0.181 Uiso 1 1 calc R A -1 H41C H 0.4113 0.7944 0.6846 0.181 Uiso 1 1 calc R A -1 C42 C 0.5092(7) 0.7569(4) 0.7702(5) 0.153(5) Uani 1 1 d . A -1 H42A H 0.5514 0.7641 0.7522 0.230 Uiso 1 1 calc R A -1 H42B H 0.5238 0.7499 0.8098 0.230 Uiso 1 1 calc R A -1 H42C H 0.4775 0.7883 0.7659 0.230 Uiso 1 1 calc R A -1 C43 C 0.6297(5) 0.4774(4) 0.8266(4) 0.115(4) Uani 1 1 d . A -1 H43A H 0.6200 0.4541 0.8572 0.172 Uiso 1 1 calc R A -1 H43B H 0.6541 0.5102 0.8415 0.172 Uiso 1 1 calc R A -1 H43C H 0.6601 0.4581 0.8035 0.172 Uiso 1 1 calc R A -1 C44 C 0.5300(5) 0.3939(3) 0.7784(4) 0.087(3) Uani 1 1 d . A -1 H44A H 0.5715 0.3842 0.7604 0.130 Uiso 1 1 calc R A -1 H44B H 0.4886 0.3730 0.7621 0.130 Uiso 1 1 calc R A -1 H44C H 0.5401 0.3862 0.8182 0.130 Uiso 1 1 calc R A -1 C45 C 0.1260(5) 0.3908(3) 0.5055(4) 0.080(3) Uani 1 1 d . A -1 H45 H 0.1688 0.3760 0.5244 0.096 Uiso 1 1 calc R A -1 C46 C 0.1273(5) 0.4051(3) 0.4489(4) 0.086(3) Uani 1 1 d . A -1 C47 C 0.0670(5) 0.4284(3) 0.4203(4) 0.086(3) Uani 1 1 d . A -1 C48 C 0.0091(5) 0.4350(3) 0.4506(4) 0.081(3) Uani 1 1 d . A -1 C49 C -0.0585(5) 0.4611(3) 0.4259(4) 0.094(4) Uani 1 1 d . A -1 H49 H -0.0636 0.4728 0.3884 0.112 Uiso 1 1 calc R A -1 C50 C -0.1111(5) 0.4680(3) 0.4549(4) 0.083(3) Uani 1 1 d . A -1 H50 H -0.1530 0.4849 0.4370 0.100 Uiso 1 1 calc R A -1 C51 C -0.1102(4) 0.4525(3) 0.5097(4) 0.075(3) Uani 1 1 d . A -1 C52 C -0.1640(5) 0.4557(4) 0.5392(4) 0.096(4) Uani 1 1 d . A -1 C53 C -0.1612(5) 0.4367(4) 0.5920(4) 0.084(3) Uani 1 1 d . A -1 C54 C -0.0901(5) 0.4127(4) 0.6174(4) 0.094(4) Uani 1 1 d . A -1 H54 H -0.0838 0.4011 0.6550 0.113 Uiso 1 1 calc R A -1 C55 C -0.0455(4) 0.4255(3) 0.5366(4) 0.070(3) Uani 1 1 d . A -1 C56 C 0.0134(4) 0.4192(3) 0.5066(4) 0.070(3) Uani 1 1 d . A -1 C57 C 0.1911(5) 0.3964(4) 0.4229(4) 0.105(4) Uani 1 1 d . A -1 H57A H 0.1800 0.3722 0.3911 0.158 Uiso 1 1 calc R A -1 H57B H 0.2282 0.3801 0.4498 0.158 Uiso 1 1 calc R A -1 H57C H 0.2081 0.4310 0.4104 0.158 Uiso 1 1 calc R A -1 C58 C 0.0597(5) 0.4475(4) 0.3620(4) 0.096(4) Uani 1 1 d . A -1 H58A H 0.1063 0.4466 0.3488 0.144 Uiso 1 1 calc R A -1 H58B H 0.0414 0.4845 0.3599 0.144 Uiso 1 1 calc R A -1 H58C H 0.0265 0.4240 0.3387 0.144 Uiso 1 1 calc R A -1 C59 C -0.2363(5) 0.4848(4) 0.5152(4) 0.112(4) Uani 1 1 d . A -1 H59A H -0.2278 0.5237 0.5122 0.168 Uiso 1 1 calc R A -1 H59B H -0.2719 0.4787 0.5402 0.168 Uiso 1 1 calc R A -1 H59C H -0.2537 0.4702 0.4785 0.168 Uiso 1 1 calc R A -1 C60 C -0.2174(5) 0.4402(5) 0.6304(5) 0.142(5) Uani 1 1 d . A -1 H60A H -0.2265 0.4781 0.6383 0.213 Uiso 1 1 calc R A -1 H60B H -0.2007 0.4213 0.6651 0.213 Uiso 1 1 calc R A -1 H60C H -0.2616 0.4233 0.6127 0.213 Uiso 1 1 calc R A -1 C61 C 0.0081(4) 0.2768(3) 0.5397(4) 0.072(3) Uani 1 1 d . A -1 H61 H 0.0269 0.2968 0.5117 0.087 Uiso 1 1 calc R A -1 C62 C -0.0253(4) 0.2254(4) 0.5249(3) 0.079(3) Uani 1 1 d . A -1 C63 C -0.0550(4) 0.1980(3) 0.5639(3) 0.072(3) Uani 1 1 d . A -1 C64 C -0.0500(4) 0.2208(4) 0.6175(4) 0.078(3) Uani 1 1 d . A -1 C65 C -0.0807(5) 0.1961(4) 0.6610(4) 0.094(3) Uani 1 1 d . A -1 H65 H -0.1055 0.1629 0.6542 0.113 Uiso 1 1 calc R A -1 C66 C -0.0754(5) 0.2189(4) 0.7129(4) 0.104(4) Uani 1 1 d . A -1 H66 H -0.0963 0.2015 0.7416 0.125 Uiso 1 1 calc R A -1 C67 C -0.0379(5) 0.2693(4) 0.7235(3) 0.081(3) Uani 1 1 d . A -1 C68 C -0.0247(5) 0.2919(4) 0.7763(3) 0.093(3) Uani 1 1 d . A -1 C69 C 0.0166(5) 0.3379(3) 0.7864(3) 0.079(3) Uani 1 1 d . A -1 C70 C 0.0417(4) 0.3590(3) 0.7401(4) 0.080(3) Uani 1 1 d . A -1 H70 H 0.0697 0.3908 0.7462 0.096 Uiso 1 1 calc R A -1 C71 C -0.0080(4) 0.2930(3) 0.6815(3) 0.070(3) Uani 1 1 d . A -1 C72 C -0.0148(4) 0.2714(3) 0.6287(3) 0.065(3) Uani 1 1 d . A -1 C73 C -0.0266(5) 0.2064(4) 0.4675(4) 0.100(4) Uani 1 1 d . A -1 H73A H 0.0112 0.1796 0.4660 0.151 Uiso 1 1 calc R A -1 H73B H -0.0189 0.2370 0.4435 0.151 Uiso 1 1 calc R A -1 H73C H -0.0730 0.1899 0.4548 0.151 Uiso 1 1 calc R A -1 C74 C -0.0908(5) 0.1432(4) 0.5489(4) 0.103(4) Uani 1 1 d . A -1 H74A H -0.1408 0.1489 0.5335 0.154 Uiso 1 1 calc R A -1 H74B H -0.0884 0.1208 0.5823 0.154 Uiso 1 1 calc R A -1 H74C H -0.0660 0.1249 0.5213 0.154 Uiso 1 1 calc R A -1 C75 C -0.0605(7) 0.2686(4) 0.8260(4) 0.143(5) Uani 1 1 d . A -1 H75A H -0.0281 0.2427 0.8469 0.215 Uiso 1 1 calc R A -1 H75B H -0.1051 0.2504 0.8116 0.215 Uiso 1 1 calc R A -1 H75C H -0.0706 0.2982 0.8506 0.215 Uiso 1 1 calc R A -1 C76 C 0.0346(5) 0.3663(4) 0.8399(3) 0.096(4) Uani 1 1 d . A -1 H76A H 0.0574 0.4008 0.8337 0.144 Uiso 1 1 calc R A -1 H76B H 0.0673 0.3440 0.8651 0.144 Uiso 1 1 calc R A -1 H76C H -0.0091 0.3728 0.8564 0.144 Uiso 1 1 calc R A -1 C77 C 0.2103(5) 0.2831(4) 0.7613(3) 0.085(3) Uani 1 1 d . A -1 H77 H 0.2293 0.2976 0.7303 0.102 Uiso 1 1 calc R A -1 C78 C 0.1640(5) 0.2391(3) 0.7528(3) 0.074(3) Uani 1 1 d . A -1 C79 C 0.1337(5) 0.2195(4) 0.7947(4) 0.087(3) Uani 1 1 d . A -1 C80 C 0.1498(5) 0.2423(3) 0.8469(4) 0.078(3) Uani 1 1 d . A -1 C81 C 0.1250(5) 0.2266(4) 0.8971(4) 0.092(3) Uani 1 1 d . A -1 H81 H 0.0923 0.1975 0.8953 0.110 Uiso 1 1 calc R A -1 C82 C 0.1441(5) 0.2497(4) 0.9469(4) 0.097(4) Uani 1 1 d . A -1 H82 H 0.1258 0.2354 0.9783 0.116 Uiso 1 1 calc R A -1 C83 C 0.1912(5) 0.2952(4) 0.9539(4) 0.084(3) Uani 1 1 d . A -1 C84 C 0.2104(5) 0.3222(5) 1.0045(4) 0.114(4) Uani 1 1 d . A -1 C85 C 0.2575(5) 0.3656(5) 1.0034(4) 0.110(4) Uani 1 1 d . A -1 C86 C 0.2802(5) 0.3806(4) 0.9528(4) 0.097(4) Uani 1 1 d . A -1 H86 H 0.3106 0.4111 0.9535 0.116 Uiso 1 1 calc R A -1 C87 C 0.2188(5) 0.3125(3) 0.9065(3) 0.077(3) Uani 1 1 d . A -1 C88 C 0.1982(5) 0.2867(3) 0.8546(3) 0.072(3) Uani 1 1 d . A -1 C89 C 0.1526(5) 0.2168(4) 0.6960(4) 0.099(4) Uani 1 1 d . A -1 H89A H 0.1755 0.1813 0.6958 0.149 Uiso 1 1 calc R A -1 H89B H 0.1735 0.2411 0.6708 0.149 Uiso 1 1 calc R A -1 H89C H 0.1014 0.2130 0.6838 0.149 Uiso 1 1 calc R A -1 C90 C 0.0839(5) 0.1706(4) 0.7879(4) 0.104(4) Uani 1 1 d . A -1 H90A H 0.0533 0.1728 0.7521 0.157 Uiso 1 1 calc R A -1 H90B H 0.0543 0.1702 0.8180 0.157 Uiso 1 1 calc R A -1 H90C H 0.1123 0.1375 0.7893 0.157 Uiso 1 1 calc R A -1 C91 C 0.1848(6) 0.3048(5) 1.0561(4) 0.133(5) Uani 1 1 d . A -1 H91A H 0.2033 0.2687 1.0661 0.199 Uiso 1 1 calc R A -1 H91B H 0.1326 0.3039 1.0506 0.199 Uiso 1 1 calc R A -1 H91C H 0.2015 0.3302 1.0859 0.199 Uiso 1 1 calc R A -1 C92 C 0.2816(7) 0.3973(6) 1.0568(5) 0.181(6) Uani 1 1 d . A -1 H92A H 0.2403 0.4150 1.0693 0.272 Uiso 1 1 calc R A -1 H92B H 0.3165 0.4247 1.0495 0.272 Uiso 1 1 calc R A -1 H92C H 0.3034 0.3726 1.0856 0.272 Uiso 1 1 calc R A -1 C93 C 0.3821(6) 0.2664(3) 0.8614(4) 0.119(4) Uani 1 1 d . A -1 H93 H 0.3422 0.2469 0.8438 0.143 Uiso 1 1 calc R A -1 C94 C 0.4396(8) 0.2383(4) 0.8850(5) 0.151(6) Uani 1 1 d . A -1 C95 C 0.4977(7) 0.2654(4) 0.9116(5) 0.133(5) Uani 1 1 d . A -1 C96 C 0.4960(7) 0.3258(4) 0.9154(4) 0.118(4) Uani 1 1 d . A -1 C97 C 0.5476(6) 0.3599(4) 0.9415(4) 0.119(4) Uani 1 1 d . A -1 H97 H 0.5892 0.3436 0.9608 0.143 Uiso 1 1 calc R A -1 C98 C 0.5446(6) 0.4137(4) 0.9420(4) 0.106(4) Uani 1 1 d . A -1 H98 H 0.5829 0.4345 0.9601 0.128 Uiso 1 1 calc R A -1 C99 C 0.4809(6) 0.4392(3) 0.9140(4) 0.094(4) Uani 1 1 d . A -1 C100 C 0.4715(5) 0.4955(4) 0.9095(4) 0.094(4) Uani 1 1 d . A -1 C101 C 0.4084(4) 0.5166(3) 0.8795(4) 0.077(3) Uani 1 1 d . A -1 C102 C 0.3565(5) 0.4803(3) 0.8558(3) 0.082(3) Uani 1 1 d . A -1 H102 H 0.3143 0.4944 0.8352 0.099 Uiso 1 1 calc R A -1 C103 C 0.4265(5) 0.4061(3) 0.8886(3) 0.078(3) Uani 1 1 d . A -1 C104 C 0.4318(5) 0.3494(3) 0.8896(4) 0.081(3) Uani 1 1 d . A -1 C105 C 0.4403(9) 0.1790(4) 0.8822(6) 0.199(8) Uani 1 1 d . A -1 H10A H 0.4664 0.1645 0.9166 0.299 Uiso 1 1 calc R A -1 H10B H 0.4638 0.1676 0.8506 0.299 Uiso 1 1 calc R A -1 H10C H 0.3913 0.1654 0.8776 0.299 Uiso 1 1 calc R A -1 C106 C 0.5675(8) 0.2398(5) 0.9407(5) 0.211(7) Uani 1 1 d . A -1 H10D H 0.5620 0.2311 0.9792 0.316 Uiso 1 1 calc R A -1 H10E H 0.6068 0.2654 0.9402 0.316 Uiso 1 1 calc R A -1 H10F H 0.5777 0.2068 0.9211 0.316 Uiso 1 1 calc R A -1 C107 C 0.5261(5) 0.5370(4) 0.9359(4) 0.108(4) Uani 1 1 d . A -1 H10G H 0.5587 0.5196 0.9654 0.162 Uiso 1 1 calc R A -1 H10H H 0.5012 0.5667 0.9516 0.162 Uiso 1 1 calc R A -1 H10I H 0.5534 0.5511 0.9075 0.162 Uiso 1 1 calc R A -1 C108 C 0.3940(5) 0.5771(3) 0.8703(4) 0.093(4) Uani 1 1 d . A -1 H10J H 0.3987 0.5956 0.9062 0.139 Uiso 1 1 calc R A -1 H10K H 0.3455 0.5823 0.8510 0.139 Uiso 1 1 calc R A -1 H10L H 0.4284 0.5921 0.8477 0.139 Uiso 1 1 calc R A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0461(6) 0.0834(8) 0.0839(8) 0.0126(7) 0.0026(6) -0.0042(6) Co2 0.0705(7) 0.0560(7) 0.0748(8) 0.0103(6) 0.0011(6) -0.0032(6) Co3 0.0534(6) 0.0483(6) 0.0824(8) 0.0061(6) 0.0044(6) -0.0007(5) Fe1 0.0573(7) 0.0641(8) 0.0859(9) 0.0112(7) -0.0006(7) 0.0012(6) Fe2 0.0797(8) 0.0737(8) 0.0778(8) 0.0117(7) 0.0173(7) 0.0234(7) N1 0.088(5) 0.097(5) 0.099(6) 0.002(5) -0.012(5) -0.020(5) N2 0.077(5) 0.084(5) 0.152(7) 0.016(5) -0.016(5) 0.006(4) N3 0.070(5) 0.100(5) 0.109(6) 0.007(4) 0.030(4) 0.012(4) N4 0.054(4) 0.089(5) 0.083(5) 0.013(4) 0.002(4) -0.011(4) N5 0.056(4) 0.050(4) 0.116(6) 0.024(4) -0.019(4) -0.008(3) N6 0.051(4) 0.073(4) 0.076(4) 0.021(4) 0.012(3) 0.018(3) N7 0.054(4) 0.087(5) 0.092(5) 0.041(4) 0.006(4) 0.007(4) N8 0.065(4) 0.065(4) 0.070(4) 0.009(3) 0.003(4) -0.012(4) N9 0.084(5) 0.031(3) 0.079(4) 0.006(3) -0.001(4) 0.009(3) N10 0.124(6) 0.074(5) 0.109(6) -0.007(4) 0.009(5) 0.038(5) N11 0.127(6) 0.236(10) 0.143(7) 0.057(7) 0.078(6) 0.072(7) N12 0.165(7) 0.087(6) 0.098(6) -0.003(4) 0.038(5) 0.033(5) N13 0.043(4) 0.070(4) 0.088(5) 0.007(4) -0.009(4) 0.005(3) N14 0.048(4) 0.084(5) 0.087(5) -0.005(4) 0.031(3) -0.014(3) N15 0.055(4) 0.103(5) 0.049(4) 0.015(4) 0.010(3) 0.011(4) N16 0.063(5) 0.100(5) 0.095(5) -0.031(4) -0.006(4) -0.002(4) N17 0.083(5) 0.079(5) 0.066(4) 0.020(4) 0.020(4) -0.016(4) N18 0.082(5) 0.085(5) 0.103(6) -0.023(4) -0.030(5) -0.004(4) N19 0.128(6) 0.082(5) 0.082(5) -0.001(4) 0.019(5) 0.012(5) N20 0.089(5) 0.066(4) 0.075(5) 0.019(4) -0.002(4) 0.021(4) N21 0.065(4) 0.038(3) 0.090(5) 0.009(3) 0.007(4) 0.001(3) N22 0.052(4) 0.049(4) 0.102(5) 0.011(4) -0.003(4) 0.006(3) N23 0.069(4) 0.043(4) 0.102(5) -0.002(4) -0.014(4) -0.003(3) N24 0.070(4) 0.083(5) 0.077(4) -0.005(4) 0.027(4) -0.018(4) C1 0.065(6) 0.085(6) 0.114(8) 0.007(6) -0.009(6) -0.012(5) C2 0.065(6) 0.096(7) 0.106(7) 0.027(6) 0.007(5) 0.008(5) C3 0.065(5) 0.064(5) 0.088(6) 0.010(5) 0.021(5) 0.008(5) C4 0.105(7) 0.038(4) 0.066(5) 0.028(4) 0.015(5) 0.010(5) C5 0.045(5) 0.031(4) 0.141(8) 0.021(5) -0.031(5) 0.004(4) C6 0.049(5) 0.074(5) 0.066(5) 0.020(4) -0.003(4) 0.011(4) C7 0.056(5) 0.070(5) 0.082(6) 0.018(5) 0.010(5) 0.017(4) C8 0.064(5) 0.073(6) 0.082(6) 0.005(5) 0.008(5) -0.013(5) C9 0.092(6) 0.037(5) 0.075(6) -0.005(4) 0.004(5) 0.011(4) C10 0.084(6) 0.090(7) 0.095(7) -0.008(5) 0.023(5) 0.016(6) C11 0.133(8) 0.120(7) 0.088(7) 0.029(6) 0.028(6) 0.076(6) C12 0.095(6) 0.102(7) 0.106(7) 0.025(6) 0.042(6) 0.051(5) C13 0.061(5) 0.053(5) 0.112(7) -0.019(5) 0.006(5) -0.012(4) C14 0.077(6) 0.066(5) 0.094(6) -0.009(5) 0.015(5) -0.020(5) C15 0.056(5) 0.057(5) 0.111(6) -0.032(5) 0.023(5) -0.025(4) C16 0.088(6) 0.061(5) 0.085(6) -0.013(5) -0.008(5) -0.017(5) C17 0.091(6) 0.071(6) 0.100(7) -0.012(5) 0.019(6) -0.028(5) C18 0.129(8) 0.102(7) 0.068(6) 0.004(5) -0.001(6) -0.034(7) C19 0.085(6) 0.103(7) 0.063(5) -0.003(5) 0.024(5) -0.027(5) C20 0.075(6) 0.118(7) 0.056(6) 0.011(5) 0.000(5) 0.008(6) C21 0.074(6) 0.080(6) 0.072(6) -0.004(5) 0.002(5) -0.008(5) C22 0.064(6) 0.102(7) 0.093(7) -0.017(5) 0.013(5) -0.025(5) C23 0.072(6) 0.058(5) 0.075(6) 0.010(4) 0.005(5) -0.010(4) C24 0.051(5) 0.062(5) 0.090(6) -0.020(4) 0.039(4) -0.007(4) C25 0.059(6) 0.092(7) 0.189(10) -0.044(7) 0.033(6) -0.015(5) C26 0.107(7) 0.093(7) 0.140(8) -0.016(6) 0.066(6) -0.038(6) C27 0.098(8) 0.139(9) 0.098(8) 0.019(7) -0.002(6) -0.011(7) C28 0.071(6) 0.090(6) 0.100(7) 0.007(6) -0.009(5) 0.003(5) C29 0.074(6) 0.066(6) 0.113(7) 0.030(5) -0.012(6) 0.010(5) C30 0.099(7) 0.030(5) 0.145(8) -0.003(5) -0.012(7) -0.014(5) C31 0.087(6) 0.064(6) 0.150(9) -0.001(6) -0.066(6) -0.020(5) C32 0.091(7) 0.050(5) 0.129(8) -0.013(5) -0.034(6) -0.012(5) C33 0.109(8) 0.064(6) 0.132(8) 0.013(6) -0.054(7) -0.012(6) C34 0.121(8) 0.056(6) 0.123(8) 0.006(5) -0.064(6) -0.003(6) C35 0.098(7) 0.045(5) 0.091(6) 0.003(5) -0.023(6) -0.013(5) C36 0.101(7) 0.059(6) 0.101(7) -0.004(5) -0.029(6) -0.007(5) C37 0.074(6) 0.060(5) 0.086(6) 0.001(5) -0.012(5) 0.005(5) C38 0.073(5) 0.047(5) 0.081(6) -0.008(4) 0.018(5) -0.001(4) C39 0.066(5) 0.042(5) 0.089(6) 0.012(4) -0.013(5) 0.008(4) C40 0.066(5) 0.042(5) 0.100(6) 0.001(4) -0.004(5) -0.008(4) C41 0.113(8) 0.077(7) 0.163(10) 0.015(7) -0.014(8) -0.003(6) C42 0.172(11) 0.073(7) 0.184(11) -0.011(7) -0.086(9) -0.002(7) C43 0.088(7) 0.069(6) 0.165(9) 0.004(6) -0.067(7) 0.014(5) C44 0.092(7) 0.027(4) 0.129(8) 0.016(5) -0.030(6) 0.010(4) C45 0.061(6) 0.079(6) 0.095(7) 0.003(5) -0.003(5) 0.002(5) C46 0.104(7) 0.062(5) 0.084(6) 0.031(5) -0.013(6) -0.001(5) C47 0.091(7) 0.068(6) 0.098(7) 0.015(5) 0.005(6) -0.016(5) C48 0.076(6) 0.066(6) 0.096(7) 0.009(5) -0.009(6) 0.000(5) C49 0.110(7) 0.072(6) 0.087(7) 0.007(5) -0.033(6) -0.014(6) C50 0.066(6) 0.065(6) 0.119(7) -0.002(5) 0.014(6) 0.002(5) C51 0.051(5) 0.064(5) 0.113(7) -0.017(5) 0.024(5) -0.017(4) C52 0.085(7) 0.075(6) 0.126(8) 0.010(6) 0.011(6) -0.020(5) C53 0.062(6) 0.083(6) 0.108(7) -0.003(6) 0.012(5) -0.005(5) C54 0.076(6) 0.099(7) 0.103(7) -0.015(6) 0.000(6) -0.022(6) C55 0.063(5) 0.063(5) 0.085(6) 0.012(5) 0.013(5) -0.018(4) C56 0.062(5) 0.053(5) 0.092(6) 0.015(5) 0.000(5) -0.014(4) C57 0.074(6) 0.147(9) 0.097(7) 0.045(6) 0.020(6) -0.005(6) C58 0.114(8) 0.084(6) 0.087(7) 0.017(5) 0.002(6) 0.012(6) C59 0.065(6) 0.107(8) 0.154(9) 0.008(7) -0.024(7) 0.011(6) C60 0.087(7) 0.163(11) 0.191(10) 0.016(8) 0.073(7) 0.010(7) C61 0.034(4) 0.095(6) 0.088(6) 0.025(5) 0.013(4) 0.012(4) C62 0.050(5) 0.119(7) 0.066(6) -0.004(5) 0.006(5) 0.013(5) C63 0.072(6) 0.097(6) 0.049(5) 0.001(5) 0.015(4) 0.009(5) C64 0.052(5) 0.089(6) 0.091(6) 0.016(5) 0.000(5) 0.005(5) C65 0.084(6) 0.109(7) 0.084(6) 0.018(6) -0.007(5) -0.041(6) C66 0.107(7) 0.119(7) 0.086(7) -0.008(6) 0.008(6) -0.063(6) C67 0.106(7) 0.096(6) 0.042(5) 0.002(5) 0.015(5) -0.028(6) C68 0.122(7) 0.090(6) 0.076(6) 0.030(5) 0.041(5) -0.043(5) C69 0.092(6) 0.078(6) 0.071(5) 0.025(5) 0.027(5) -0.017(5) C70 0.067(6) 0.078(6) 0.089(6) 0.017(5) -0.006(5) -0.030(5) C71 0.069(5) 0.086(6) 0.052(5) 0.007(5) 0.004(4) -0.017(5) C72 0.039(4) 0.092(6) 0.065(5) 0.016(5) 0.011(4) -0.005(4) C73 0.112(7) 0.109(7) 0.085(7) 0.003(6) 0.032(6) -0.008(6) C74 0.108(8) 0.097(7) 0.101(7) -0.015(6) 0.004(6) -0.020(6) C75 0.205(12) 0.114(8) 0.109(8) 0.016(7) 0.013(8) -0.071(8) C76 0.097(7) 0.113(7) 0.078(6) 0.008(6) 0.018(5) -0.017(6) C77 0.091(7) 0.099(7) 0.059(6) 0.003(5) -0.008(5) -0.024(6) C78 0.077(6) 0.084(6) 0.061(5) 0.001(5) 0.008(5) -0.015(5) C79 0.085(6) 0.101(7) 0.072(6) -0.008(5) 0.001(5) -0.012(6) C80 0.080(6) 0.063(5) 0.095(6) 0.034(5) 0.026(5) -0.006(5) C81 0.072(6) 0.084(6) 0.116(8) 0.003(6) -0.001(6) -0.022(5) C82 0.089(7) 0.093(7) 0.108(7) 0.018(6) 0.010(6) -0.017(6) C83 0.060(6) 0.115(7) 0.072(6) 0.020(5) -0.013(5) -0.002(5) C84 0.080(7) 0.171(10) 0.077(7) 0.010(7) -0.033(6) -0.015(7) C85 0.079(7) 0.166(10) 0.081(7) -0.029(7) -0.007(6) -0.031(7) C86 0.066(6) 0.122(8) 0.101(7) 0.005(6) 0.003(6) -0.027(6) C87 0.089(6) 0.078(6) 0.061(6) 0.004(5) -0.001(5) 0.003(5) C88 0.074(6) 0.081(6) 0.060(5) 0.015(5) 0.008(5) 0.013(5) C89 0.110(7) 0.094(7) 0.082(7) 0.003(5) -0.027(6) -0.027(6) C90 0.095(7) 0.098(7) 0.117(8) -0.003(6) 0.002(6) -0.049(6) C91 0.114(8) 0.228(13) 0.054(6) 0.019(7) 0.007(6) -0.037(9) C92 0.148(11) 0.263(15) 0.134(10) -0.049(10) 0.018(9) -0.082(11) C93 0.165(10) 0.048(6) 0.149(9) 0.026(6) 0.037(8) 0.018(6) C94 0.227(14) 0.068(7) 0.143(10) 0.019(7) -0.028(10) 0.032(8) C95 0.180(10) 0.073(6) 0.140(9) 0.017(6) 0.003(8) 0.069(7) C96 0.157(10) 0.103(8) 0.092(7) 0.025(6) 0.010(7) 0.025(7) C97 0.123(8) 0.104(7) 0.115(8) -0.008(6) -0.036(7) 0.057(6) C98 0.110(8) 0.104(8) 0.094(7) 0.004(6) -0.026(6) 0.026(6) C99 0.139(8) 0.047(5) 0.090(7) -0.004(5) -0.007(6) 0.029(6) C100 0.083(7) 0.110(7) 0.084(6) -0.031(6) -0.011(6) -0.011(6) C101 0.061(5) 0.047(5) 0.118(7) -0.007(5) 0.000(5) -0.003(4) C102 0.090(6) 0.081(6) 0.078(6) 0.009(5) 0.018(5) 0.024(5) C103 0.109(7) 0.055(5) 0.069(6) 0.009(5) 0.006(5) 0.005(5) C104 0.105(7) 0.058(5) 0.075(6) 0.007(5) -0.012(6) 0.028(5) C105 0.322(19) 0.050(7) 0.214(14) 0.017(8) -0.005(14) 0.051(9) C106 0.336(16) 0.136(8) 0.147(11) 0.040(8) -0.014(11) 0.157(9) C107 0.089(7) 0.117(8) 0.107(8) -0.029(6) -0.030(6) 0.009(6) C108 0.104(7) 0.060(6) 0.110(7) -0.012(5) 0.002(6) 0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N4 1.999(7) . ? Co1 N7 2.061(7) . ? Co1 N16 2.066(8) . ? Co1 N13 2.107(7) . ? Co1 N14 2.130(6) . ? Co1 N15 2.158(7) . ? Co2 N5 1.921(8) . ? Co2 N8 1.947(6) . ? Co2 N18 1.951(8) . ? Co2 N19 1.973(8) . ? Co2 N20 1.988(7) . ? Co2 N17 2.027(7) . ? Co3 N9 1.921(7) . ? Co3 N23 1.965(7) . ? Co3 N6 1.978(7) . ? Co3 N24 1.987(7) . ? Co3 N21 2.011(6) . ? Co3 N22 2.038(6) . ? Fe1 C2 1.862(10) . ? Fe1 C5 1.895(10) . ? Fe1 C6 1.902(8) . ? Fe1 C4 1.908(9) . ? Fe1 C3 1.911(9) . ? Fe1 C1 1.914(10) . ? Fe2 C12 1.853(10) . ? Fe2 C9 1.865(9) . ? Fe2 C7 1.881(8) . ? Fe2 C8 1.882(8) . ? Fe2 C10 1.900(9) . ? Fe2 C11 1.921(11) . ? N1 C1 1.153(12) . ? N2 C2 1.177(11) . ? N3 C3 1.172(10) . ? N4 C4 1.175(11) . ? N5 C5 1.180(11) . ? N6 C6 1.180(10) . ? N7 C7 1.195(10) . ? N8 C8 1.183(10) . ? N9 C9 1.186(11) . ? N10 C10 1.206(11) . ? N11 C11 1.198(13) . ? N12 C12 1.234(12) . ? N13 C45 1.317(11) . ? N13 C56 1.369(10) . ? N14 C55 1.301(10) . ? N14 C54 1.317(11) . ? N15 C72 1.311(10) . ? N15 C61 1.322(10) . ? N16 C70 1.322(11) . ? N16 C71 1.411(10) . ? N17 C77 1.336(10) . ? N17 C88 1.362(10) . ? N18 C86 1.291(12) . ? N18 C87 1.396(11) . ? N19 C104 1.321(11) . ? N19 C93 1.396(11) . ? N20 C102 1.345(10) . ? N20 C103 1.385(11) . ? N21 C38 1.346(9) . ? N21 C39 1.353(9) . ? N22 C29 1.329(10) . ? N22 C40 1.355(10) . ? N23 C13 1.319(10) . ? N23 C24 1.339(10) . ? N24 C23 1.309(10) . ? N24 C22 1.344(11) . ? C13 C14 1.355(12) . ? C14 C15 1.393(12) . ? C14 C25 1.464(12) . ? C15 C16 1.432(12) . ? C15 C26 1.501(12) . ? C16 C17 1.411(12) . ? C16 C24 1.417(12) . ? C17 C18 1.415(13) . ? C18 C19 1.443(13) . ? C19 C20 1.414(12) . ? C19 C23 1.447(11) . ? C20 C21 1.339(12) . ? C20 C27 1.484(12) . ? C21 C22 1.431(12) . ? C21 C28 1.542(12) . ? C23 C24 1.458(11) . ? C29 C30 1.382(12) . ? C30 C31 1.320(13) . ? C30 C41 1.572(12) . ? C31 C32 1.433(12) . ? C31 C42 1.479(13) . ? C32 C40 1.417(11) . ? C32 C33 1.421(13) . ? C33 C34 1.366(12) . ? C34 C35 1.412(12) . ? C35 C39 1.400(11) . ? C35 C36 1.434(11) . ? C36 C37 1.373(12) . ? C36 C43 1.487(12) . ? C37 C38 1.418(11) . ? C37 C44 1.505(10) . ? C39 C40 1.401(10) . ? C45 C46 1.425(12) . ? C46 C47 1.381(12) . ? C46 C57 1.455(13) . ? C47 C48 1.411(13) . ? C47 C58 1.485(12) . ? C48 C56 1.411(12) . ? C48 C49 1.487(12) . ? C49 C50 1.307(13) . ? C50 C51 1.386(12) . ? C51 C52 1.325(13) . ? C51 C55 1.471(11) . ? C52 C53 1.362(13) . ? C52 C59 1.587(13) . ? C53 C60 1.512(14) . ? C53 C54 1.524(12) . ? C55 C56 1.421(12) . ? C61 C62 1.448(12) . ? C62 C63 1.349(11) . ? C62 C73 1.470(12) . ? C63 C64 1.412(11) . ? C63 C74 1.540(12) . ? C64 C65 1.414(12) . ? C64 C72 1.430(11) . ? C65 C66 1.376(13) . ? C66 C67 1.444(12) . ? C67 C71 1.368(11) . ? C67 C68 1.392(11) . ? C68 C69 1.387(12) . ? C68 C75 1.575(14) . ? C69 C70 1.382(12) . ? C69 C76 1.478(12) . ? C71 C72 1.381(11) . ? C77 C78 1.396(12) . ? C78 C79 1.329(12) . ? C78 C89 1.476(12) . ? C79 C80 1.384(12) . ? C79 C90 1.531(13) . ? C80 C81 1.420(12) . ? C80 C88 1.429(12) . ? C81 C82 1.344(13) . ? C82 C83 1.434(13) . ? C83 C87 1.397(12) . ? C83 C84 1.404(13) . ? C84 C85 1.401(15) . ? C84 C91 1.471(14) . ? C85 C86 1.409(14) . ? C85 C92 1.532(15) . ? C87 C88 1.422(11) . ? C93 C94 1.354(16) . ? C94 C95 1.375(17) . ? C94 C105 1.472(14) . ? C95 C96 1.500(14) . ? C95 C106 1.547(17) . ? C96 C97 1.380(15) . ? C96 C104 1.417(14) . ? C97 C98 1.336(13) . ? C98 C99 1.447(13) . ? C99 C103 1.394(13) . ? C99 C100 1.410(12) . ? C100 C101 1.412(12) . ? C100 C107 1.537(13) . ? C101 C102 1.399(12) . ? C101 C108 1.536(11) . ? C103 C104 1.411(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N7 92.0(3) . . ? N4 Co1 N16 96.3(3) . . ? N7 Co1 N16 90.2(3) . . ? N4 Co1 N13 91.6(3) . . ? N7 Co1 N13 101.0(3) . . ? N16 Co1 N13 166.1(3) . . ? N4 Co1 N14 167.7(3) . . ? N7 Co1 N14 91.0(3) . . ? N16 Co1 N14 95.6(3) . . ? N13 Co1 N14 76.1(3) . . ? N4 Co1 N15 94.5(3) . . ? N7 Co1 N15 165.3(3) . . ? N16 Co1 N15 76.1(3) . . ? N13 Co1 N15 91.9(2) . . ? N14 Co1 N15 85.4(2) . . ? N5 Co2 N8 93.9(3) . . ? N5 Co2 N18 172.0(3) . . ? N8 Co2 N18 91.2(3) . . ? N5 Co2 N19 89.3(3) . . ? N8 Co2 N19 172.9(3) . . ? N18 Co2 N19 86.4(3) . . ? N5 Co2 N20 92.3(3) . . ? N8 Co2 N20 91.9(3) . . ? N18 Co2 N20 93.7(3) . . ? N19 Co2 N20 81.6(3) . . ? N5 Co2 N17 90.9(3) . . ? N8 Co2 N17 91.0(3) . . ? N18 Co2 N17 82.8(3) . . ? N19 Co2 N17 95.3(3) . . ? N20 Co2 N17 175.5(3) . . ? N9 Co3 N23 176.1(3) . . ? N9 Co3 N6 90.9(2) . . ? N23 Co3 N6 88.5(3) . . ? N9 Co3 N24 94.6(3) . . ? N23 Co3 N24 81.6(3) . . ? N6 Co3 N24 95.8(3) . . ? N9 Co3 N21 95.0(3) . . ? N23 Co3 N21 88.9(3) . . ? N6 Co3 N21 95.8(2) . . ? N24 Co3 N21 164.8(3) . . ? N9 Co3 N22 91.9(3) . . ? N23 Co3 N22 89.0(3) . . ? N6 Co3 N22 175.2(2) . . ? N24 Co3 N22 87.8(3) . . ? N21 Co3 N22 80.1(2) . . ? C2 Fe1 C5 91.6(4) . . ? C2 Fe1 C6 178.1(4) . . ? C5 Fe1 C6 86.6(3) . . ? C2 Fe1 C4 86.9(3) . . ? C5 Fe1 C4 88.4(3) . . ? C6 Fe1 C4 93.6(3) . . ? C2 Fe1 C3 92.2(4) . . ? C5 Fe1 C3 92.7(4) . . ? C6 Fe1 C3 87.3(3) . . ? C4 Fe1 C3 178.6(4) . . ? C2 Fe1 C1 84.1(4) . . ? C5 Fe1 C1 174.8(4) . . ? C6 Fe1 C1 97.7(4) . . ? C4 Fe1 C1 88.5(4) . . ? C3 Fe1 C1 90.3(4) . . ? C12 Fe2 C9 89.6(4) . . ? C12 Fe2 C7 176.2(4) . . ? C9 Fe2 C7 91.4(4) . . ? C12 Fe2 C8 89.4(4) . . ? C9 Fe2 C8 89.1(3) . . ? C7 Fe2 C8 87.0(4) . . ? C12 Fe2 C10 89.5(4) . . ? C9 Fe2 C10 86.6(4) . . ? C7 Fe2 C10 94.2(4) . . ? C8 Fe2 C10 175.6(4) . . ? C12 Fe2 C11 92.2(4) . . ? C9 Fe2 C11 176.9(4) . . ? C7 Fe2 C11 86.9(4) . . ? C8 Fe2 C11 93.5(4) . . ? C10 Fe2 C11 90.8(4) . . ? C4 N4 Co1 151.4(6) . . ? C5 N5 Co2 162.9(6) . . ? C6 N6 Co3 157.2(6) . . ? C7 N7 Co1 163.4(6) . . ? C8 N8 Co2 160.9(7) . . ? C9 N9 Co3 165.3(6) . . ? C45 N13 C56 113.7(7) . . ? C45 N13 Co1 131.5(5) . . ? C56 N13 Co1 114.8(5) . . ? C55 N14 C54 120.0(7) . . ? C55 N14 Co1 116.1(5) . . ? C54 N14 Co1 123.9(6) . . ? C72 N15 C61 118.9(7) . . ? C72 N15 Co1 114.5(5) . . ? C61 N15 Co1 126.5(5) . . ? C70 N16 C71 113.7(7) . . ? C70 N16 Co1 130.6(6) . . ? C71 N16 Co1 115.7(5) . . ? C77 N17 C88 118.0(7) . . ? C77 N17 Co2 130.1(6) . . ? C88 N17 Co2 111.9(5) . . ? C86 N18 C87 114.6(8) . . ? C86 N18 Co2 132.1(7) . . ? C87 N18 Co2 113.1(6) . . ? C104 N19 C93 117.6(8) . . ? C104 N19 Co2 114.1(6) . . ? C93 N19 Co2 127.5(7) . . ? C102 N20 C103 118.3(7) . . ? C102 N20 Co2 129.8(6) . . ? C103 N20 Co2 111.9(5) . . ? C38 N21 C39 117.4(6) . . ? C38 N21 Co3 128.4(5) . . ? C39 N21 Co3 113.6(5) . . ? C29 N22 C40 117.5(7) . . ? C29 N22 Co3 130.3(6) . . ? C40 N22 Co3 111.8(5) . . ? C13 N23 C24 113.6(7) . . ? C13 N23 Co3 132.7(6) . . ? C24 N23 Co3 113.6(5) . . ? C23 N24 C22 116.2(7) . . ? C23 N24 Co3 114.5(5) . . ? C22 N24 Co3 129.0(6) . . ? N1 C1 Fe1 178.2(8) . . ? N2 C2 Fe1 175.7(9) . . ? N3 C3 Fe1 174.5(7) . . ? N4 C4 Fe1 176.5(7) . . ? N5 C5 Fe1 175.4(7) . . ? N6 C6 Fe1 172.2(7) . . ? N7 C7 Fe2 174.1(7) . . ? N8 C8 Fe2 174.3(8) . . ? N9 C9 Fe2 175.1(7) . . ? N10 C10 Fe2 173.8(9) . . ? N11 C11 Fe2 178.0(9) . . ? N12 C12 Fe2 178.4(9) . . ? N23 C13 C14 129.5(8) . . ? C13 C14 C15 117.2(8) . . ? C13 C14 C25 122.0(8) . . ? C15 C14 C25 120.8(9) . . ? C14 C15 C16 117.8(8) . . ? C14 C15 C26 120.6(8) . . ? C16 C15 C26 121.6(8) . . ? C17 C16 C24 120.1(8) . . ? C17 C16 C15 122.9(9) . . ? C24 C16 C15 116.9(8) . . ? C16 C17 C18 120.7(9) . . ? C17 C18 C19 122.0(8) . . ? C20 C19 C18 126.1(8) . . ? C20 C19 C23 117.2(8) . . ? C18 C19 C23 116.7(8) . . ? C21 C20 C19 118.6(8) . . ? C21 C20 C27 120.0(9) . . ? C19 C20 C27 121.3(8) . . ? C20 C21 C22 119.5(8) . . ? C20 C21 C28 123.8(8) . . ? C22 C21 C28 116.7(8) . . ? N24 C22 C21 123.8(8) . . ? N24 C23 C19 124.4(8) . . ? N24 C23 C24 114.7(7) . . ? C19 C23 C24 120.9(8) . . ? N23 C24 C16 125.0(7) . . ? N23 C24 C23 115.5(7) . . ? C16 C24 C23 119.5(7) . . ? N22 C29 C30 122.9(8) . . ? C31 C30 C29 122.7(8) . . ? C31 C30 C41 121.6(8) . . ? C29 C30 C41 115.7(8) . . ? C30 C31 C32 116.5(8) . . ? C30 C31 C42 122.4(8) . . ? C32 C31 C42 120.9(8) . . ? C40 C32 C33 116.2(8) . . ? C40 C32 C31 118.8(8) . . ? C33 C32 C31 125.0(8) . . ? C34 C33 C32 122.6(8) . . ? C33 C34 C35 120.5(9) . . ? C39 C35 C34 117.9(7) . . ? C39 C35 C36 118.7(7) . . ? C34 C35 C36 123.1(8) . . ? C37 C36 C35 117.2(8) . . ? C37 C36 C43 120.9(8) . . ? C35 C36 C43 121.9(8) . . ? C36 C37 C38 120.2(7) . . ? C36 C37 C44 122.1(8) . . ? C38 C37 C44 117.5(7) . . ? N21 C38 C37 122.8(7) . . ? N21 C39 C40 115.5(7) . . ? N21 C39 C35 123.5(7) . . ? C40 C39 C35 121.0(7) . . ? N22 C40 C39 117.3(7) . . ? N22 C40 C32 121.6(7) . . ? C39 C40 C32 121.1(8) . . ? N13 C45 C46 128.0(8) . . ? C47 C46 C45 118.1(9) . . ? C47 C46 C57 121.4(8) . . ? C45 C46 C57 120.4(8) . . ? C46 C47 C48 115.7(8) . . ? C46 C47 C58 125.4(9) . . ? C48 C47 C58 118.9(8) . . ? C47 C48 C56 121.6(8) . . ? C47 C48 C49 121.9(8) . . ? C56 C48 C49 116.5(8) . . ? C50 C49 C48 121.1(9) . . ? C49 C50 C51 124.9(8) . . ? C52 C51 C50 126.5(8) . . ? C52 C51 C55 116.3(8) . . ? C50 C51 C55 117.0(8) . . ? C51 C52 C53 123.7(9) . . ? C51 C52 C59 121.1(9) . . ? C53 C52 C59 115.2(9) . . ? C52 C53 C60 128.5(9) . . ? C52 C53 C54 116.0(9) . . ? C60 C53 C54 115.3(8) . . ? N14 C54 C53 120.1(8) . . ? N14 C55 C56 117.0(7) . . ? N14 C55 C51 123.8(8) . . ? C56 C55 C51 119.2(8) . . ? N13 C56 C48 122.8(8) . . ? N13 C56 C55 116.0(7) . . ? C48 C56 C55 121.2(8) . . ? N15 C61 C62 123.3(8) . . ? C63 C62 C61 118.6(8) . . ? C63 C62 C73 123.4(8) . . ? C61 C62 C73 118.0(8) . . ? C62 C63 C64 117.7(8) . . ? C62 C63 C74 119.3(8) . . ? C64 C63 C74 123.0(8) . . ? C63 C64 C65 122.3(8) . . ? C63 C64 C72 120.0(8) . . ? C65 C64 C72 117.7(8) . . ? C66 C65 C64 121.6(9) . . ? C65 C66 C67 119.5(9) . . ? C71 C67 C68 118.5(8) . . ? C71 C67 C66 118.8(8) . . ? C68 C67 C66 122.4(8) . . ? C69 C68 C67 121.4(8) . . ? C69 C68 C75 117.2(8) . . ? C67 C68 C75 121.2(8) . . ? C70 C69 C68 114.5(8) . . ? C70 C69 C76 118.3(8) . . ? C68 C69 C76 127.2(8) . . ? N16 C70 C69 128.9(8) . . ? C67 C71 C72 122.2(8) . . ? C67 C71 N16 122.9(7) . . ? C72 C71 N16 114.9(7) . . ? N15 C72 C71 118.5(8) . . ? N15 C72 C64 121.5(8) . . ? C71 C72 C64 120.0(8) . . ? N17 C77 C78 123.2(8) . . ? C79 C78 C77 119.9(8) . . ? C79 C78 C89 123.9(8) . . ? C77 C78 C89 116.3(8) . . ? C78 C79 C80 119.4(9) . . ? C78 C79 C90 122.0(8) . . ? C80 C79 C90 118.6(8) . . ? C79 C80 C81 128.3(8) . . ? C79 C80 C88 119.5(8) . . ? C81 C80 C88 112.2(8) . . ? C82 C81 C80 125.4(9) . . ? C81 C82 C83 121.9(9) . . ? C87 C83 C84 119.7(9) . . ? C87 C83 C82 116.0(8) . . ? C84 C83 C82 124.2(9) . . ? C85 C84 C83 116.2(9) . . ? C85 C84 C91 121.6(9) . . ? C83 C84 C91 122.2(10) . . ? C84 C85 C86 119.2(9) . . ? C84 C85 C92 119.8(10) . . ? C86 C85 C92 121.0(10) . . ? N18 C86 C85 126.6(9) . . ? N18 C87 C83 123.7(8) . . ? N18 C87 C88 115.7(8) . . ? C83 C87 C88 120.5(8) . . ? N17 C88 C87 116.2(8) . . ? N17 C88 C80 119.9(7) . . ? C87 C88 C80 123.9(8) . . ? C94 C93 N19 123.6(10) . . ? C93 C94 C95 119.7(10) . . ? C93 C94 C105 120.5(12) . . ? C95 C94 C105 119.8(12) . . ? C94 C95 C96 119.5(10) . . ? C94 C95 C106 126.5(10) . . ? C96 C95 C106 113.9(10) . . ? C97 C96 C104 117.6(9) . . ? C97 C96 C95 128.2(10) . . ? C104 C96 C95 114.2(10) . . ? C98 C97 C96 125.9(10) . . ? C97 C98 C99 117.8(9) . . ? C103 C99 C100 118.0(9) . . ? C103 C99 C98 118.0(8) . . ? C100 C99 C98 123.9(9) . . ? C99 C100 C101 119.8(8) . . ? C99 C100 C107 124.0(8) . . ? C101 C100 C107 116.3(8) . . ? C102 C101 C100 118.2(8) . . ? C102 C101 C108 117.8(7) . . ? C100 C101 C108 124.0(8) . . ? N20 C102 C101 123.1(8) . . ? N20 C103 C99 122.6(7) . . ? N20 C103 C104 115.2(8) . . ? C99 C103 C104 122.2(8) . . ? N19 C104 C103 116.3(8) . . ? N19 C104 C96 125.1(8) . . ? C103 C104 C96 118.3(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.031 _refine_diff_density_min -0.691 _refine_diff_density_rms 0.199 #end============= data_{[Co(tmphen)2]3[Fe(CN)6]2}_90K #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; '{Co(tmphen)2)3(Fe(CN)6)2}.12H2O' ; _chemical_name_common '{Co(tmphen)2)3(Fe(CN)6)2}.12H2O' _chemical_melting_point ? _chemical_formula_moiety 'C108 H120 Co3 Fe2 N24 O12' _chemical_formula_sum 'C108 H120 Co3 Fe2 N24 O12' _chemical_formula_weight 2234.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.04(4) _cell_length_b 24.77(5) _cell_length_c 24.56(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.72(9) _cell_angle_gamma 90.00 _cell_volume 11487(42) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 12006 _cell_measurement_theta_min 2.165 _cell_measurement_theta_max 27.788 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4564 _exptl_absorpt_coefficient_mu 0.738 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.7669 _exptl_absorpt_correction_T_max 0.8546 _exptl_absorpt_process_details 'SADABS: Bruker,2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART 1000 CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51873 _diffrn_reflns_av_R_equivalents 0.0860 _diffrn_reflns_av_sigmaI/netI 0.0739 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 20.81 _reflns_number_total 12006 _reflns_number_gt 8020 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER, 2000)' _computing_cell_refinement 'SAINT (BRUKER, 2001)' _computing_data_reduction 'SAINT (BRUKER, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1728P)^2^+21.46P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00040(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12006 _refine_ls_number_parameters 1387 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1204 _refine_ls_R_factor_gt 0.0835 _refine_ls_wR_factor_ref 0.2645 _refine_ls_wR_factor_gt 0.2368 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.095 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.06305(3) 0.37373(3) 0.61567(3) 0.0388(2) Uani 1 1 d . . . Co2 Co 0.29518(4) 0.36749(3) 0.83091(3) 0.0385(2) Uani 1 1 d . . . Co3 Co 0.35844(3) 0.54819(3) 0.66481(3) 0.0357(2) Uani 1 1 d . . . Fe1 Fe 0.32554(4) 0.35436(3) 0.63558(3) 0.0416(2) Uani 1 1 d . . . Fe2 Fe 0.14580(4) 0.51775(3) 0.75522(3) 0.0461(2) Uani 1 1 d . . . N1 N 0.3091(3) 0.3296(2) 0.51178(19) 0.0685(18) Uani 1 1 d . . . N2 N 0.3260(2) 0.2317(2) 0.6540(2) 0.0645(17) Uani 1 1 d . . . N3 N 0.4886(2) 0.3621(2) 0.6395(2) 0.0627(17) Uani 1 1 d . . . N4 N 0.1638(2) 0.34514(17) 0.62610(16) 0.0400(13) Uani 1 1 d . . . N5 N 0.3255(2) 0.36928(16) 0.75926(17) 0.0413(13) Uani 1 1 d . . . N6 N 0.3310(2) 0.47862(17) 0.63242(16) 0.0381(12) Uani 1 1 d . . . N7 N 0.0951(2) 0.44229(18) 0.65840(17) 0.0449(13) Uani 1 1 d . . . N8 N 0.2184(2) 0.41892(17) 0.80983(16) 0.0396(13) Uani 1 1 d . . . N9 N 0.2835(2) 0.54368(15) 0.71066(16) 0.0375(13) Uani 1 1 d . . . N10 N 0.0935(3) 0.6224(2) 0.69634(19) 0.0649(17) Uani 1 1 d . . . N11 N -0.0003(3) 0.4954(3) 0.7909(2) 0.095(2) Uani 1 1 d . . . N12 N 0.1939(3) 0.5819(2) 0.8597(2) 0.0769(19) Uani 1 1 d . . . N13 N 0.0724(2) 0.39713(18) 0.53348(17) 0.0436(13) Uani 1 1 d . . . N14 N -0.0385(2) 0.40811(18) 0.58772(17) 0.0425(13) Uani 1 1 d . . . N15 N 0.0150(2) 0.29853(17) 0.58778(14) 0.0356(12) Uani 1 1 d . . . N16 N 0.0306(2) 0.33972(18) 0.68759(15) 0.0396(13) Uani 1 1 d . . . N17 N 0.2295(2) 0.30595(17) 0.80939(15) 0.0391(13) Uani 1 1 d . . . N18 N 0.2638(2) 0.35388(19) 0.90461(17) 0.0518(15) Uani 1 1 d . . . N19 N 0.3777(3) 0.32150(19) 0.85811(19) 0.0627(16) Uani 1 1 d . . . N20 N 0.3622(2) 0.42579(17) 0.85905(16) 0.0428(13) Uani 1 1 d . . . N21 N 0.4337(2) 0.51923(15) 0.72302(15) 0.0330(12) Uani 1 1 d . . . N22 N 0.3951(2) 0.61762(16) 0.69997(18) 0.0429(13) Uani 1 1 d . . . N23 N 0.4311(2) 0.55281(17) 0.61359(17) 0.0399(13) Uani 1 1 d . . . N24 N 0.3024(2) 0.59124(18) 0.60537(17) 0.0453(14) Uani 1 1 d . . . C1 C 0.3156(3) 0.3403(2) 0.5576(2) 0.0504(18) Uani 1 1 d . . . C2 C 0.3283(3) 0.2779(3) 0.6470(2) 0.0519(18) Uani 1 1 d . . . C3 C 0.4274(3) 0.3575(2) 0.6382(2) 0.0480(18) Uani 1 1 d . . . C4 C 0.2245(3) 0.3499(2) 0.62987(19) 0.0372(15) Uani 1 1 d . . . C5 C 0.3286(2) 0.3642(2) 0.7127(2) 0.0395(16) Uani 1 1 d . . . C6 C 0.3251(2) 0.4322(2) 0.62985(19) 0.0403(16) Uani 1 1 d . . . C7 C 0.1156(2) 0.4736(2) 0.6940(2) 0.0394(16) Uani 1 1 d . . . C8 C 0.1881(3) 0.4557(2) 0.7900(2) 0.0380(16) Uani 1 1 d . . . C9 C 0.2322(3) 0.53232(19) 0.7282(2) 0.0381(16) Uani 1 1 d . . . C10 C 0.1116(3) 0.5808(2) 0.7190(2) 0.0543(18) Uani 1 1 d . . . C11 C 0.0544(3) 0.5050(3) 0.7782(2) 0.066(2) Uani 1 1 d . . . C12 C 0.1746(3) 0.5580(3) 0.8198(2) 0.062(2) Uani 1 1 d . . . C13 C 0.4952(3) 0.5323(2) 0.6169(2) 0.0499(18) Uani 1 1 d . . . H13 H 0.5113 0.5128 0.6485 0.060 Uiso 1 1 calc R . . C14 C 0.5407(3) 0.5369(2) 0.5780(2) 0.0505(18) Uani 1 1 d . . . C15 C 0.5179(3) 0.5640(2) 0.5303(2) 0.0555(17) Uani 1 1 d . . . C16 C 0.4486(3) 0.5885(2) 0.5241(2) 0.0509(18) Uani 1 1 d . . . C17 C 0.4192(3) 0.6192(2) 0.4780(2) 0.0554(18) Uani 1 1 d . . . H17 H 0.4449 0.6236 0.4486 0.067 Uiso 1 1 calc R . . C18 C 0.3534(3) 0.6429(3) 0.4756(2) 0.067(2) Uani 1 1 d . . . H18 H 0.3363 0.6637 0.4452 0.081 Uiso 1 1 calc R . . C19 C 0.3101(3) 0.6360(2) 0.5195(2) 0.0527(18) Uani 1 1 d . . . C20 C 0.2419(3) 0.6595(2) 0.5199(2) 0.057(2) Uani 1 1 d . . . C21 C 0.2055(3) 0.6476(2) 0.5639(2) 0.0539(19) Uani 1 1 d . . . C22 C 0.2367(3) 0.6122(2) 0.6047(2) 0.0510(18) Uani 1 1 d . . . H22 H 0.2109 0.6026 0.6328 0.061 Uiso 1 1 calc R . . C23 C 0.3385(3) 0.6035(2) 0.5631(2) 0.0423(16) Uani 1 1 d . . . C24 C 0.4078(2) 0.5814(2) 0.5671(2) 0.0426(16) Uani 1 1 d . . . C25 C 0.6126(3) 0.5124(3) 0.5880(3) 0.071(2) Uani 1 1 d . . . H25A H 0.6174 0.4860 0.5601 0.107 Uiso 1 1 calc R . . H25B H 0.6191 0.4953 0.6234 0.107 Uiso 1 1 calc R . . H25C H 0.6477 0.5400 0.5870 0.107 Uiso 1 1 calc R . . C26 C 0.5650(3) 0.5704(3) 0.4875(3) 0.076(2) Uani 1 1 d . . . H26A H 0.6031 0.5946 0.5005 0.115 Uiso 1 1 calc R . . H26B H 0.5385 0.5850 0.4549 0.115 Uiso 1 1 calc R . . H26C H 0.5841 0.5359 0.4795 0.115 Uiso 1 1 calc R . . C27 C 0.2079(4) 0.6945(3) 0.4751(3) 0.081(3) Uani 1 1 d . . . H27A H 0.1661 0.6771 0.4571 0.122 Uiso 1 1 calc R . . H27B H 0.2403 0.7008 0.4491 0.122 Uiso 1 1 calc R . . H27C H 0.1952 0.7284 0.4902 0.122 Uiso 1 1 calc R . . C28 C 0.1340(3) 0.6708(3) 0.5695(2) 0.059(2) Uani 1 1 d . . . H28A H 0.1186 0.6578 0.6028 0.088 Uiso 1 1 calc R . . H28B H 0.1006 0.6601 0.5386 0.088 Uiso 1 1 calc R . . H28C H 0.1371 0.7095 0.5708 0.088 Uiso 1 1 calc R . . C29 C 0.3729(3) 0.6684(2) 0.6898(2) 0.0540(19) Uani 1 1 d . . . H29 H 0.3317 0.6732 0.6654 0.065 Uiso 1 1 calc R . . C30 C 0.4054(3) 0.7132(2) 0.7123(3) 0.063(2) Uani 1 1 d . . . C31 C 0.4668(4) 0.7079(2) 0.7492(3) 0.072(2) Uani 1 1 d . . . C32 C 0.4934(3) 0.6544(2) 0.7620(2) 0.060(2) Uani 1 1 d . . . C33 C 0.5563(3) 0.6424(3) 0.7974(3) 0.072(2) Uani 1 1 d . . . H33 H 0.5831 0.6706 0.8145 0.086 Uiso 1 1 calc R . . C34 C 0.5783(3) 0.5915(2) 0.8069(3) 0.070(2) Uani 1 1 d . . . H34 H 0.6207 0.5853 0.8296 0.084 Uiso 1 1 calc R . . C35 C 0.5388(3) 0.5468(2) 0.7834(2) 0.0503(18) Uani 1 1 d . . . C36 C 0.5588(3) 0.4920(2) 0.7930(2) 0.059(2) Uani 1 1 d . . . C37 C 0.5119(3) 0.4531(2) 0.7689(2) 0.0475(18) Uani 1 1 d . . . C38 C 0.4509(3) 0.4686(2) 0.7341(2) 0.0376(16) Uani 1 1 d . . . H38 H 0.4210 0.4417 0.7179 0.045 Uiso 1 1 calc R . . C39 C 0.4762(3) 0.5579(2) 0.7478(2) 0.0392(16) Uani 1 1 d . . . C40 C 0.4556(3) 0.6118(2) 0.7363(2) 0.0397(16) Uani 1 1 d . . . C41 C 0.3739(4) 0.7681(2) 0.6990(3) 0.087(3) Uani 1 1 d . . . H41A H 0.3644 0.7853 0.7323 0.131 Uiso 1 1 calc R . . H41B H 0.3305 0.7644 0.6745 0.131 Uiso 1 1 calc R . . H41C H 0.4067 0.7897 0.6819 0.131 Uiso 1 1 calc R . . C42 C 0.5065(4) 0.7553(3) 0.7759(3) 0.111(3) Uani 1 1 d . . . H42A H 0.5356 0.7707 0.7509 0.166 Uiso 1 1 calc R . . H42B H 0.5359 0.7436 0.8085 0.166 Uiso 1 1 calc R . . H42C H 0.4735 0.7818 0.7853 0.166 Uiso 1 1 calc R . . C43 C 0.6255(3) 0.4764(3) 0.8290(3) 0.084(3) Uani 1 1 d . . . H43A H 0.6158 0.4719 0.8661 0.126 Uiso 1 1 calc R . . H43B H 0.6604 0.5042 0.8278 0.126 Uiso 1 1 calc R . . H43C H 0.6432 0.4431 0.8162 0.126 Uiso 1 1 calc R . . C44 C 0.5268(3) 0.3938(2) 0.7773(2) 0.061(2) Uani 1 1 d . . . H44A H 0.5655 0.3835 0.7581 0.092 Uiso 1 1 calc R . . H44B H 0.4854 0.3734 0.7633 0.092 Uiso 1 1 calc R . . H44C H 0.5390 0.3865 0.8158 0.092 Uiso 1 1 calc R . . C45 C 0.1263(3) 0.3916(2) 0.5040(2) 0.0454(17) Uani 1 1 d . . . H45 H 0.1678 0.3763 0.5217 0.054 Uiso 1 1 calc R . . C46 C 0.1257(3) 0.4068(2) 0.4487(2) 0.0435(17) Uani 1 1 d . . . C47 C 0.0650(3) 0.4296(2) 0.4211(2) 0.0512(18) Uani 1 1 d . . . C48 C 0.0067(3) 0.4363(2) 0.4492(2) 0.0450(17) Uani 1 1 d . . . C49 C -0.0589(3) 0.4607(2) 0.4262(2) 0.0495(18) Uani 1 1 d . . . H49 H -0.0639 0.4718 0.3897 0.059 Uiso 1 1 calc R . . C50 C -0.1121(3) 0.4681(2) 0.4541(2) 0.0446(17) Uani 1 1 d . . . H50 H -0.1526 0.4853 0.4369 0.054 Uiso 1 1 calc R . . C51 C -0.1106(3) 0.4510(2) 0.5095(2) 0.0425(17) Uani 1 1 d . . . C52 C -0.1664(3) 0.4559(2) 0.5396(2) 0.0527(19) Uani 1 1 d . . . C53 C -0.1593(3) 0.4359(2) 0.5931(2) 0.0535(19) Uani 1 1 d . . . C54 C -0.0930(3) 0.4131(2) 0.6148(2) 0.0555(19) Uani 1 1 d . . . H54 H -0.0879 0.4008 0.6509 0.067 Uiso 1 1 calc R . . C55 C -0.0471(3) 0.4264(2) 0.5356(2) 0.0449(17) Uani 1 1 d . . . C56 C 0.0122(3) 0.4194(2) 0.5057(2) 0.0432(17) Uani 1 1 d . . . C57 C 0.1911(3) 0.3975(3) 0.4222(2) 0.066(2) Uani 1 1 d . . . H57A H 0.2281 0.3837 0.4490 0.099 Uiso 1 1 calc R . . H57B H 0.2061 0.4309 0.4077 0.099 Uiso 1 1 calc R . . H57C H 0.1810 0.3718 0.3929 0.099 Uiso 1 1 calc R . . C58 C 0.0607(3) 0.4485(2) 0.3632(2) 0.060(2) Uani 1 1 d . . . H58A H 0.1068 0.4468 0.3516 0.090 Uiso 1 1 calc R . . H58B H 0.0438 0.4850 0.3606 0.090 Uiso 1 1 calc R . . H58C H 0.0286 0.4257 0.3399 0.090 Uiso 1 1 calc R . . C59 C -0.2357(3) 0.4830(3) 0.5136(3) 0.064(2) Uani 1 1 d . . . H59A H -0.2284 0.5213 0.5113 0.096 Uiso 1 1 calc R . . H59B H -0.2723 0.4761 0.5360 0.096 Uiso 1 1 calc R . . H59C H -0.2495 0.4687 0.4775 0.096 Uiso 1 1 calc R . . C60 C -0.2171(3) 0.4386(3) 0.6287(3) 0.079(2) Uani 1 1 d . . . H60A H -0.2274 0.4757 0.6358 0.119 Uiso 1 1 calc R . . H60B H -0.2021 0.4205 0.6629 0.119 Uiso 1 1 calc R . . H60C H -0.2588 0.4214 0.6103 0.119 Uiso 1 1 calc R . . C61 C 0.0075(3) 0.2763(2) 0.5380(2) 0.0436(16) Uani 1 1 d . . . H61 H 0.0256 0.2956 0.5105 0.052 Uiso 1 1 calc R . . C62 C -0.0250(3) 0.2270(2) 0.52301(19) 0.0390(16) Uani 1 1 d . . . C63 C -0.0551(3) 0.1990(2) 0.5612(2) 0.0462(17) Uani 1 1 d . . . C64 C -0.0511(3) 0.2215(2) 0.6153(2) 0.0428(17) Uani 1 1 d . . . C65 C -0.0798(3) 0.1958(3) 0.6593(2) 0.0605(19) Uani 1 1 d . . . H65 H -0.1035 0.1631 0.6532 0.073 Uiso 1 1 calc R . . C66 C -0.0730(3) 0.2182(3) 0.7096(2) 0.063(2) Uani 1 1 d . . . H66 H -0.0938 0.2011 0.7371 0.075 Uiso 1 1 calc R . . C67 C -0.0351(3) 0.2671(2) 0.7222(2) 0.0495(18) Uani 1 1 d . . . C68 C -0.0253(3) 0.2910(2) 0.7755(2) 0.0498(18) Uani 1 1 d . . . C69 C 0.0148(3) 0.3369(2) 0.7841(2) 0.0446(17) Uani 1 1 d . . . C70 C 0.0417(3) 0.3592(2) 0.7379(2) 0.0475(18) Uani 1 1 d . . . H70 H 0.0694 0.3901 0.7436 0.057 Uiso 1 1 calc R . . C71 C -0.0066(3) 0.2925(2) 0.68056(19) 0.0382(16) Uani 1 1 d . . . C72 C -0.0150(2) 0.2703(2) 0.62628(18) 0.0344(15) Uani 1 1 d . . . C73 C -0.0261(3) 0.2067(3) 0.4656(2) 0.062(2) Uani 1 1 d . . . H73A H 0.0007 0.1738 0.4662 0.092 Uiso 1 1 calc R . . H73B H -0.0056 0.2332 0.4441 0.092 Uiso 1 1 calc R . . H73C H -0.0742 0.1999 0.4498 0.092 Uiso 1 1 calc R . . C74 C -0.0904(3) 0.1459(2) 0.5469(2) 0.063(2) Uani 1 1 d . . . H74A H -0.1355 0.1520 0.5252 0.095 Uiso 1 1 calc R . . H74B H -0.0972 0.1272 0.5799 0.095 Uiso 1 1 calc R . . H74C H -0.0611 0.1246 0.5263 0.095 Uiso 1 1 calc R . . C75 C -0.0561(4) 0.2641(3) 0.8221(2) 0.079(2) Uani 1 1 d . . . H75A H -0.0294 0.2744 0.8564 0.118 Uiso 1 1 calc R . . H75B H -0.0541 0.2256 0.8180 0.118 Uiso 1 1 calc R . . H75C H -0.1046 0.2751 0.8214 0.118 Uiso 1 1 calc R . . C76 C 0.0324(3) 0.3630(2) 0.8380(2) 0.0544(19) Uani 1 1 d . . . H76A H -0.0099 0.3774 0.8497 0.082 Uiso 1 1 calc R . . H76B H 0.0656 0.3917 0.8352 0.082 Uiso 1 1 calc R . . H76C H 0.0531 0.3369 0.8643 0.082 Uiso 1 1 calc R . . C77 C 0.2109(3) 0.2845(2) 0.7605(2) 0.0460(17) Uani 1 1 d . . . H77 H 0.2292 0.2997 0.7308 0.055 Uiso 1 1 calc R . . C78 C 0.1658(3) 0.2409(2) 0.7506(2) 0.0460(17) Uani 1 1 d . . . C79 C 0.1344(3) 0.2189(2) 0.7931(2) 0.0447(17) Uani 1 1 d . . . C80 C 0.1519(3) 0.2423(2) 0.8454(2) 0.0458(17) Uani 1 1 d . . . C81 C 0.1250(3) 0.2248(3) 0.8945(2) 0.0575(19) Uani 1 1 d . . . H81 H 0.0922 0.1968 0.8921 0.069 Uiso 1 1 calc R . . C82 C 0.1458(3) 0.2477(2) 0.9437(2) 0.0535(18) Uani 1 1 d . . . H82 H 0.1289 0.2336 0.9745 0.064 Uiso 1 1 calc R . . C83 C 0.1922(3) 0.2921(2) 0.9504(2) 0.0504(18) Uani 1 1 d . . . C84 C 0.2155(3) 0.3186(3) 1.0013(2) 0.073(2) Uani 1 1 d . . . C85 C 0.2603(3) 0.3621(3) 1.0009(2) 0.083(3) Uani 1 1 d . . . C86 C 0.2836(3) 0.3780(3) 0.9520(3) 0.076(2) Uani 1 1 d . . . H86 H 0.3147 0.4070 0.9529 0.091 Uiso 1 1 calc R . . C87 C 0.2190(3) 0.3109(2) 0.9037(2) 0.0422(16) Uani 1 1 d . . . C88 C 0.1990(3) 0.2856(2) 0.85117(19) 0.0392(16) Uani 1 1 d . . . C89 C 0.1532(3) 0.2186(3) 0.6927(2) 0.060(2) Uani 1 1 d . . . H89A H 0.1798 0.1858 0.6909 0.091 Uiso 1 1 calc R . . H89B H 0.1683 0.2446 0.6677 0.091 Uiso 1 1 calc R . . H89C H 0.1037 0.2112 0.6827 0.091 Uiso 1 1 calc R . . C90 C 0.0876(3) 0.1703(2) 0.7844(2) 0.060(2) Uani 1 1 d . . . H90A H 0.0581 0.1731 0.7496 0.090 Uiso 1 1 calc R . . H90B H 0.0584 0.1681 0.8132 0.090 Uiso 1 1 calc R . . H90C H 0.1163 0.1384 0.7847 0.090 Uiso 1 1 calc R . . C91 C 0.1889(3) 0.2984(3) 1.0527(2) 0.081(3) Uani 1 1 d . . . H91A H 0.2075 0.3207 1.0832 0.121 Uiso 1 1 calc R . . H91B H 0.2041 0.2618 1.0596 0.121 Uiso 1 1 calc R . . H91C H 0.1380 0.2998 1.0480 0.121 Uiso 1 1 calc R . . C92 C 0.2866(4) 0.3937(4) 1.0536(3) 0.143(4) Uani 1 1 d . . . H92A H 0.3035 0.3689 1.0824 0.215 Uiso 1 1 calc R . . H92B H 0.2484 0.4146 1.0643 0.215 Uiso 1 1 calc R . . H92C H 0.3245 0.4173 1.0468 0.215 Uiso 1 1 calc R . . C93 C 0.3827(4) 0.2682(3) 0.8548(3) 0.089(3) Uani 1 1 d . . . H93 H 0.3451 0.2490 0.8360 0.107 Uiso 1 1 calc R . . C94 C 0.4427(6) 0.2401(3) 0.8787(3) 0.135(4) Uani 1 1 d . . . C95 C 0.5006(5) 0.2672(3) 0.9066(3) 0.109(3) Uani 1 1 d . . . C96 C 0.4948(4) 0.3244(3) 0.9101(3) 0.088(3) Uani 1 1 d . . . C97 C 0.5468(4) 0.3590(3) 0.9362(3) 0.091(3) Uani 1 1 d . . . H97 H 0.5883 0.3436 0.9538 0.109 Uiso 1 1 calc R . . C98 C 0.5409(4) 0.4133(3) 0.9374(3) 0.082(3) Uani 1 1 d . . . H98 H 0.5774 0.4338 0.9560 0.098 Uiso 1 1 calc R . . C99 C 0.4785(3) 0.4399(3) 0.9103(2) 0.060(2) Uani 1 1 d . . . C100 C 0.4682(3) 0.4967(3) 0.9078(2) 0.059(2) Uani 1 1 d . . . C101 C 0.4057(3) 0.5150(2) 0.8785(2) 0.0487(17) Uani 1 1 d . . . C102 C 0.3542(3) 0.4783(2) 0.8544(2) 0.0460(17) Uani 1 1 d . . . H102 H 0.3130 0.4918 0.8345 0.055 Uiso 1 1 calc R . . C103 C 0.4237(3) 0.4064(2) 0.8853(2) 0.0563(19) Uani 1 1 d . . . C104 C 0.4316(3) 0.3488(3) 0.8845(2) 0.063(2) Uani 1 1 d . . . C105 C 0.4382(6) 0.1775(3) 0.8748(4) 0.158(5) Uani 1 1 d . . . H10G H 0.4802 0.1638 0.8621 0.237 Uiso 1 1 calc R . . H10H H 0.3974 0.1674 0.8495 0.237 Uiso 1 1 calc R . . H10I H 0.4341 0.1628 0.9104 0.237 Uiso 1 1 calc R . . C106 C 0.5668(5) 0.2404(3) 0.9362(4) 0.154(4) Uani 1 1 d . . . H10J H 0.5573 0.2029 0.9421 0.231 Uiso 1 1 calc R . . H10K H 0.5803 0.2578 0.9709 0.231 Uiso 1 1 calc R . . H10L H 0.6046 0.2435 0.9142 0.231 Uiso 1 1 calc R . . C107 C 0.5202(4) 0.5355(3) 0.9350(3) 0.086(3) Uani 1 1 d . . . H10D H 0.5455 0.5520 0.9081 0.129 Uiso 1 1 calc R . . H10E H 0.5531 0.5169 0.9616 0.129 Uiso 1 1 calc R . . H10F H 0.4960 0.5628 0.9530 0.129 Uiso 1 1 calc R . . C108 C 0.3894(3) 0.5750(2) 0.8711(3) 0.065(2) Uani 1 1 d . . . H10A H 0.3871 0.5912 0.9063 0.097 Uiso 1 1 calc R . . H10B H 0.3448 0.5796 0.8483 0.097 Uiso 1 1 calc R . . H10C H 0.4262 0.5921 0.8540 0.097 Uiso 1 1 calc R . . O20S O 0.6973(6) 0.4795(5) 1.0163(5) 0.115(4) Uiso 0.50 1 d P A -20 O23S O 0.1218(6) 0.4815(5) 0.9223(4) 0.107(3) Uiso 0.50 1 d P B -23 O21S O 0.0884(6) 0.4488(5) 0.9609(5) 0.115(4) Uiso 0.50 1 d P C -24 O2S O -0.2747(7) 0.1676(5) 0.5590(5) 0.128(4) Uiso 0.50 1 d P D -2 O16S O 0.6390(6) 0.3535(5) 0.6648(5) 0.111(4) Uiso 0.50 1 d P E -16 O30S O 0.2637(6) 0.6778(5) 0.7907(5) 0.120(4) Uiso 0.50 1 d P F -30 O5S O 0.0691(7) 0.0814(5) 0.4950(5) 0.132(4) Uiso 0.50 1 d P G -5 O25S O -0.0667(6) 0.5858(5) 0.8673(5) 0.118(4) Uiso 0.50 1 d P H -25 O9S O 0.3073(5) 0.1793(4) 0.7618(4) 0.094(3) Uiso 0.50 1 d P I -9 O13S O 0.5313(14) 0.2854(11) 1.0825(11) 0.139(9) Uiso 0.25 1 d P J -13 O32S O 0.2251(9) 0.8201(7) 0.5932(7) 0.068(5) Uiso 0.25 1 d P K -32 O10S O 0.3151(5) 0.1918(4) 0.9091(4) 0.086(3) Uiso 0.50 1 d P L -10 O11S O 0.4360(8) 0.2481(6) 0.5469(6) 0.161(5) Uiso 0.50 1 d P M -11 O1S O -0.2156(6) 0.2052(5) 0.8059(5) 0.120(4) Uiso 0.50 1 d P N -1 O26S O -0.1301(7) 0.4560(6) 0.7661(6) 0.144(5) Uiso 0.50 1 d P O -26 O31S O 0.2752(19) 0.7300(15) 0.8154(14) 0.195(14) Uiso 0.25 1 d P P -31 O4S O -0.1048(14) 0.0512(11) 0.4213(10) 0.135(9) Uiso 0.25 1 d P Q -4 O18S O 0.7345(9) 0.3826(7) 0.7614(7) 0.189(7) Uiso 0.50 1 d P R -18 O19S O 0.7396(15) 0.3138(12) 0.9462(11) 0.147(10) Uiso 0.25 1 d P S -19 O6S O 0.1342(10) 0.0715(8) 0.6506(8) 0.086(6) Uiso 0.25 1 d P T -6 O24S O 0.2138(14) 0.5450(11) 1.0608(11) 0.139(9) Uiso 0.25 1 d P U -24 O22S O 0.1909(14) 0.4860(11) 0.9561(11) 0.139(9) Uiso 0.25 1 d P V -22 O33S O 0.3444(13) 0.7617(11) 0.3823(10) 0.130(9) Uiso 0.25 1 d P . . O29S O 0.2547(15) 0.7921(12) 0.8275(12) 0.148(10) Uiso 0.25 1 d P W -29 O8S O 0.2273(15) 0.0633(12) 0.7451(11) 0.146(10) Uiso 0.25 1 d P X -8 O28S O -0.2765(14) 0.6051(11) 0.7010(11) 0.137(9) Uiso 0.25 1 d P Y -28 O17S O 0.6317(7) 0.3949(6) 0.6829(6) 0.145(5) Uiso 0.50 1 d P Z -17 O14S O 0.5629(12) 0.2987(9) 1.0725(9) 0.101(7) Uiso 0.25 1 d P A -14 O15S O 0.6259(10) 0.3168(9) 0.6505(8) 0.090(6) Uiso 0.25 1 d P B -15 O12S O 0.4915(9) 0.2934(7) 1.0596(6) 0.163(6) Uiso 0.50 1 d P C -12 O7S O 0.1945(12) 0.0695(9) 0.6730(9) 0.107(7) Uiso 0.25 1 d P D -7 O34S O 0.3988(13) 0.2097(11) 0.5350(10) 0.127(8) Uiso 0.25 1 d P E -34 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0297(4) 0.0558(5) 0.0312(4) 0.0088(4) 0.0052(3) -0.0030(3) Co2 0.0490(4) 0.0348(4) 0.0315(4) 0.0063(3) 0.0049(3) -0.0007(3) Co3 0.0357(4) 0.0348(4) 0.0378(4) 0.0038(3) 0.0090(3) -0.0008(3) Fe1 0.0359(4) 0.0474(5) 0.0414(4) 0.0100(4) 0.0046(4) 0.0013(4) Fe2 0.0598(5) 0.0452(5) 0.0362(4) 0.0075(4) 0.0169(4) 0.0147(4) N1 0.072(3) 0.094(4) 0.040(3) 0.010(3) 0.008(3) -0.010(3) N2 0.050(3) 0.054(3) 0.085(4) 0.011(3) -0.005(3) 0.005(3) N3 0.038(3) 0.083(4) 0.068(3) -0.003(3) 0.010(2) 0.002(3) N4 0.040(2) 0.051(3) 0.027(2) 0.013(2) -0.0037(19) -0.010(2) N5 0.043(2) 0.036(3) 0.043(3) 0.007(2) -0.001(2) -0.002(2) N6 0.034(2) 0.041(3) 0.041(2) 0.016(2) 0.0115(19) 0.003(2) N7 0.034(2) 0.053(3) 0.048(3) 0.027(2) 0.007(2) 0.007(2) N8 0.040(2) 0.046(3) 0.035(2) 0.004(2) 0.011(2) -0.004(2) N9 0.061(3) 0.020(2) 0.031(2) 0.0049(19) -0.001(2) 0.002(2) N10 0.087(3) 0.063(3) 0.045(3) -0.019(3) 0.012(3) 0.023(3) N11 0.085(3) 0.115(5) 0.095(4) 0.046(3) 0.054(3) 0.042(3) N12 0.120(4) 0.061(4) 0.055(3) -0.005(3) 0.031(3) 0.014(3) N13 0.027(2) 0.052(3) 0.048(3) 0.016(2) -0.006(2) -0.002(2) N14 0.034(2) 0.054(3) 0.043(3) -0.004(2) 0.016(2) -0.012(2) N15 0.038(2) 0.057(3) 0.012(2) 0.003(2) 0.0057(18) 0.004(2) N16 0.040(2) 0.055(3) 0.021(2) 0.005(2) -0.0008(19) -0.005(2) N17 0.046(2) 0.045(3) 0.026(2) -0.002(2) 0.003(2) -0.008(2) N18 0.055(3) 0.060(3) 0.039(3) 0.002(2) 0.003(2) -0.011(3) N19 0.102(4) 0.035(3) 0.052(3) 0.002(2) 0.016(3) 0.016(3) N20 0.053(3) 0.041(3) 0.036(2) 0.008(2) 0.013(2) 0.006(2) N21 0.041(2) 0.026(2) 0.034(2) 0.0008(19) 0.0123(19) -0.0016(19) N22 0.041(2) 0.032(3) 0.055(3) 0.004(2) 0.003(2) 0.002(2) N23 0.030(2) 0.040(3) 0.049(3) -0.002(2) 0.004(2) -0.008(2) N24 0.039(2) 0.049(3) 0.049(3) -0.008(2) 0.009(2) -0.008(2) C1 0.039(3) 0.053(4) 0.058(4) 0.018(3) 0.001(3) 0.000(3) C2 0.035(3) 0.060(4) 0.061(4) 0.010(3) 0.004(3) 0.009(3) C3 0.057(3) 0.051(4) 0.035(3) 0.001(3) 0.002(3) 0.002(3) C4 0.042(3) 0.041(3) 0.026(3) 0.011(2) -0.003(2) 0.002(3) C5 0.027(3) 0.041(3) 0.047(3) 0.010(3) -0.007(3) -0.009(2) C6 0.028(3) 0.065(4) 0.031(3) 0.020(3) 0.016(2) 0.011(3) C7 0.033(3) 0.054(3) 0.034(3) 0.018(3) 0.019(2) 0.004(3) C8 0.041(3) 0.041(3) 0.031(3) -0.001(3) -0.001(2) -0.002(3) C9 0.063(3) 0.022(3) 0.030(3) 0.008(2) 0.010(3) -0.002(3) C10 0.070(4) 0.046(4) 0.049(3) 0.000(3) 0.016(3) 0.016(3) C11 0.081(4) 0.062(4) 0.060(4) 0.017(3) 0.032(3) 0.031(3) C12 0.086(4) 0.062(4) 0.038(3) 0.002(3) 0.016(3) 0.034(3) C13 0.039(3) 0.050(4) 0.062(4) -0.012(3) 0.011(3) -0.007(3) C14 0.046(3) 0.060(4) 0.049(3) -0.012(3) 0.023(3) -0.013(3) C15 0.060(3) 0.057(4) 0.058(3) -0.026(3) 0.038(3) -0.035(3) C16 0.060(3) 0.046(3) 0.049(3) -0.003(3) 0.016(3) -0.019(3) C17 0.068(3) 0.062(4) 0.042(3) -0.017(3) 0.031(3) -0.023(3) C18 0.088(4) 0.070(4) 0.044(4) 0.004(3) 0.008(3) -0.023(4) C19 0.053(3) 0.064(4) 0.044(3) -0.007(3) 0.018(3) -0.019(3) C20 0.072(4) 0.057(4) 0.040(3) 0.002(3) -0.005(3) -0.005(3) C21 0.065(4) 0.054(4) 0.039(3) -0.003(3) -0.011(3) -0.012(3) C22 0.047(3) 0.055(4) 0.051(4) -0.007(3) 0.008(3) -0.009(3) C23 0.057(3) 0.040(3) 0.031(3) 0.002(3) 0.008(3) -0.017(3) C24 0.030(3) 0.048(3) 0.051(3) -0.012(3) 0.013(3) -0.011(3) C25 0.036(3) 0.078(5) 0.104(5) -0.029(4) 0.030(3) -0.011(3) C26 0.081(4) 0.076(5) 0.079(4) -0.024(4) 0.036(4) -0.027(4) C27 0.078(4) 0.089(5) 0.072(5) 0.019(4) -0.005(4) -0.007(4) C28 0.042(3) 0.068(4) 0.064(4) 0.001(3) -0.004(3) 0.006(3) C29 0.049(3) 0.047(4) 0.061(4) 0.006(3) -0.008(3) 0.000(3) C30 0.058(4) 0.036(3) 0.086(5) 0.006(3) -0.023(3) -0.006(3) C31 0.081(4) 0.033(3) 0.095(5) -0.002(3) -0.013(4) -0.017(3) C32 0.069(4) 0.045(4) 0.061(4) 0.008(3) -0.009(3) 0.000(3) C33 0.073(4) 0.047(4) 0.083(5) 0.009(3) -0.033(4) -0.014(3) C34 0.073(4) 0.046(4) 0.079(4) 0.011(3) -0.028(4) -0.001(3) C35 0.054(3) 0.035(3) 0.059(4) 0.002(3) -0.004(3) -0.003(3) C36 0.065(4) 0.054(4) 0.053(4) 0.000(3) -0.010(3) 0.005(3) C37 0.060(3) 0.038(3) 0.043(3) -0.003(3) 0.000(3) 0.002(3) C38 0.046(3) 0.032(3) 0.035(3) 0.004(3) 0.006(3) 0.001(3) C39 0.043(3) 0.031(3) 0.043(3) 0.007(3) 0.005(3) -0.002(3) C40 0.045(3) 0.034(3) 0.039(3) 0.005(3) 0.002(3) -0.004(3) C41 0.080(4) 0.044(4) 0.123(6) 0.017(4) -0.042(4) -0.009(4) C42 0.121(6) 0.042(4) 0.145(7) 0.009(4) -0.067(5) -0.004(4) C43 0.078(4) 0.070(5) 0.091(5) 0.006(4) -0.032(4) 0.026(4) C44 0.072(4) 0.044(4) 0.063(4) 0.002(3) -0.009(3) 0.012(3) C45 0.033(3) 0.047(3) 0.057(4) 0.003(3) 0.010(3) -0.004(3) C46 0.057(3) 0.045(3) 0.028(3) 0.010(3) 0.003(3) -0.006(3) C47 0.059(3) 0.055(4) 0.039(3) 0.011(3) 0.005(3) -0.012(3) C48 0.065(4) 0.030(3) 0.037(3) 0.007(3) -0.003(3) -0.010(3) C49 0.059(3) 0.036(3) 0.049(3) 0.008(3) -0.008(3) 0.002(3) C50 0.041(3) 0.048(3) 0.043(3) 0.007(3) -0.001(3) 0.005(3) C51 0.033(3) 0.036(3) 0.058(4) -0.008(3) 0.005(3) -0.009(3) C52 0.042(3) 0.054(4) 0.060(4) -0.008(3) -0.002(3) -0.008(3) C53 0.028(3) 0.061(4) 0.074(4) 0.003(3) 0.017(3) -0.001(3) C54 0.044(3) 0.066(4) 0.057(4) -0.005(3) 0.008(3) -0.011(3) C55 0.041(3) 0.045(3) 0.048(3) 0.007(3) 0.005(3) -0.003(3) C56 0.046(3) 0.037(3) 0.046(3) 0.004(3) 0.003(3) -0.008(3) C57 0.076(4) 0.072(4) 0.055(4) 0.009(3) 0.026(3) -0.012(4) C58 0.086(4) 0.049(4) 0.044(3) 0.013(3) 0.008(3) 0.016(3) C59 0.044(3) 0.070(4) 0.076(4) -0.015(4) 0.002(3) 0.002(3) C60 0.062(4) 0.103(6) 0.079(4) 0.005(4) 0.032(3) 0.003(4) C61 0.036(3) 0.062(4) 0.036(3) 0.018(3) 0.015(2) 0.007(3) C62 0.044(3) 0.052(3) 0.022(3) 0.002(3) 0.008(2) 0.000(3) C63 0.045(3) 0.059(4) 0.037(3) -0.006(3) 0.014(3) -0.001(3) C64 0.034(3) 0.070(4) 0.025(3) 0.002(3) 0.007(2) -0.006(3) C65 0.081(4) 0.071(4) 0.034(3) -0.011(3) 0.022(3) -0.036(3) C66 0.084(4) 0.075(4) 0.032(3) 0.009(3) 0.023(3) -0.034(4) C67 0.069(4) 0.052(4) 0.029(3) 0.007(3) 0.011(3) -0.026(3) C68 0.083(4) 0.041(3) 0.028(3) 0.006(3) 0.018(3) -0.015(3) C69 0.063(3) 0.048(3) 0.022(3) 0.001(3) 0.003(3) -0.013(3) C70 0.047(3) 0.055(4) 0.040(3) 0.004(3) 0.004(3) -0.013(3) C71 0.045(3) 0.046(3) 0.025(3) 0.000(3) 0.007(2) -0.012(3) C72 0.033(3) 0.052(3) 0.020(3) 0.003(3) 0.005(2) -0.011(3) C73 0.072(4) 0.078(4) 0.038(3) -0.002(3) 0.019(3) -0.003(4) C74 0.073(4) 0.070(4) 0.045(4) -0.007(3) 0.002(3) -0.030(3) C75 0.126(5) 0.085(5) 0.031(3) 0.001(3) 0.032(3) -0.041(4) C76 0.083(4) 0.051(4) 0.032(3) 0.000(3) 0.019(3) -0.017(3) C77 0.050(3) 0.053(4) 0.034(3) 0.007(3) 0.001(3) -0.019(3) C78 0.051(3) 0.055(4) 0.032(3) 0.005(3) 0.005(3) -0.004(3) C79 0.045(3) 0.043(3) 0.045(3) -0.005(3) 0.001(3) -0.007(3) C80 0.044(3) 0.049(4) 0.046(3) 0.014(3) 0.010(3) -0.005(3) C81 0.059(4) 0.064(4) 0.050(4) 0.010(3) 0.008(3) -0.012(3) C82 0.052(3) 0.066(4) 0.045(3) 0.011(3) 0.015(3) -0.004(3) C83 0.044(3) 0.065(4) 0.040(3) 0.008(3) -0.003(3) -0.002(3) C84 0.058(4) 0.125(6) 0.039(3) -0.001(4) 0.016(3) -0.012(4) C85 0.072(4) 0.145(6) 0.035(3) -0.024(4) 0.015(3) -0.047(4) C86 0.065(4) 0.108(5) 0.057(4) -0.027(4) 0.012(3) -0.035(4) C87 0.038(3) 0.055(4) 0.034(3) 0.008(3) 0.008(2) -0.002(3) C88 0.047(3) 0.052(3) 0.020(3) 0.006(3) 0.007(2) -0.003(3) C89 0.064(4) 0.073(4) 0.046(3) -0.003(3) 0.010(3) -0.024(3) C90 0.071(4) 0.062(4) 0.048(4) -0.008(3) 0.015(3) -0.018(3) C91 0.074(4) 0.131(6) 0.037(4) 0.015(4) 0.010(3) -0.018(4) C92 0.128(6) 0.247(9) 0.060(5) -0.074(5) 0.035(4) -0.104(6) C93 0.145(6) 0.047(4) 0.079(5) 0.010(4) 0.027(5) 0.016(4) C94 0.230(10) 0.074(6) 0.087(6) -0.007(5) -0.023(7) 0.047(6) C95 0.169(7) 0.082(5) 0.077(5) 0.024(4) 0.018(5) 0.084(5) C96 0.121(6) 0.073(5) 0.064(4) 0.002(4) -0.006(4) 0.029(5) C97 0.095(5) 0.096(6) 0.075(5) 0.007(4) -0.015(4) 0.035(4) C98 0.082(5) 0.080(5) 0.075(5) -0.004(4) -0.020(4) 0.003(4) C99 0.072(4) 0.058(4) 0.046(4) 0.005(3) -0.005(3) 0.015(3) C100 0.057(4) 0.071(4) 0.046(4) -0.001(3) -0.001(3) -0.006(3) C101 0.060(3) 0.042(3) 0.047(3) 0.000(3) 0.018(3) -0.009(3) C102 0.055(3) 0.040(3) 0.047(3) 0.009(3) 0.020(3) -0.003(3) C103 0.066(4) 0.058(4) 0.044(3) 0.008(3) 0.002(3) 0.004(3) C104 0.086(4) 0.052(4) 0.049(4) 0.013(3) -0.003(3) 0.023(4) C105 0.265(11) 0.037(4) 0.152(8) -0.001(5) -0.049(8) 0.058(6) C106 0.234(9) 0.098(6) 0.118(7) 0.004(5) -0.020(7) 0.112(6) C107 0.096(5) 0.086(5) 0.070(5) 0.005(4) -0.009(4) -0.005(4) C108 0.074(4) 0.050(4) 0.070(4) 0.002(3) 0.013(3) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N4 2.030(6) . ? Co1 N7 2.046(6) . ? Co1 N16 2.123(5) . ? Co1 N13 2.131(6) . ? Co1 N14 2.140(6) . ? Co1 N15 2.147(6) . ? Co2 N5 1.925(6) . ? Co2 N8 1.955(5) . ? Co2 N19 1.983(6) . ? Co2 N20 1.989(5) . ? Co2 N17 1.997(5) . ? Co2 N18 2.010(6) . ? Co3 N9 1.937(5) . ? Co3 N6 1.940(5) . ? Co3 N23 1.994(5) . ? Co3 N24 1.998(5) . ? Co3 N22 2.007(5) . ? Co3 N21 2.015(5) . ? Fe1 C5 1.904(7) . ? Fe1 C2 1.914(7) . ? Fe1 C4 1.914(7) . ? Fe1 C1 1.930(7) . ? Fe1 C6 1.933(7) . ? Fe1 C3 1.934(7) . ? Fe2 C10 1.871(7) . ? Fe2 C8 1.886(6) . ? Fe2 C7 1.886(6) . ? Fe2 C9 1.891(7) . ? Fe2 C12 1.892(7) . ? Fe2 C11 1.926(8) . ? N1 C1 1.147(7) . ? N2 C2 1.158(8) . ? N3 C3 1.167(7) . ? N4 C4 1.152(7) . ? N5 C5 1.159(7) . ? N6 C6 1.156(7) . ? N7 C7 1.194(7) . ? N8 C8 1.151(6) . ? N9 C9 1.153(7) . ? N10 C10 1.199(7) . ? N11 C11 1.152(8) . ? N12 C12 1.161(7) . ? N13 C45 1.339(7) . ? N13 C56 1.370(7) . ? N14 C54 1.313(7) . ? N14 C55 1.348(7) . ? N15 C61 1.330(7) . ? N15 C72 1.362(6) . ? N16 C70 1.317(7) . ? N16 C71 1.367(7) . ? N17 C77 1.318(7) . ? N17 C88 1.344(7) . ? N18 C86 1.318(8) . ? N18 C87 1.363(7) . ? N19 C104 1.324(8) . ? N19 C93 1.326(8) . ? N20 C102 1.314(7) . ? N20 C103 1.348(7) . ? N21 C38 1.316(7) . ? N21 C39 1.344(6) . ? N22 C29 1.338(7) . ? N22 C40 1.367(7) . ? N23 C13 1.315(7) . ? N23 C24 1.365(7) . ? N24 C22 1.352(7) . ? N24 C23 1.355(7) . ? C13 C14 1.377(8) . ? C14 C15 1.370(8) . ? C14 C25 1.488(8) . ? C15 C16 1.443(8) . ? C15 C26 1.479(9) . ? C16 C24 1.405(8) . ? C16 C17 1.416(8) . ? C17 C18 1.377(9) . ? C18 C19 1.452(9) . ? C19 C23 1.390(8) . ? C19 C20 1.424(9) . ? C20 C21 1.393(9) . ? C20 C27 1.480(9) . ? C21 C22 1.401(8) . ? C21 C28 1.501(9) . ? C23 C24 1.420(8) . ? C29 C30 1.353(8) . ? C30 C31 1.386(9) . ? C30 C41 1.503(9) . ? C31 C32 1.439(9) . ? C31 C42 1.499(9) . ? C32 C40 1.380(8) . ? C32 C33 1.415(9) . ? C33 C34 1.339(9) . ? C34 C35 1.418(8) . ? C35 C39 1.409(7) . ? C35 C36 1.421(9) . ? C36 C37 1.390(8) . ? C36 C43 1.498(9) . ? C37 C38 1.400(7) . ? C37 C44 1.506(8) . ? C39 C40 1.411(8) . ? C45 C46 1.409(8) . ? C46 C47 1.379(8) . ? C46 C57 1.500(9) . ? C47 C48 1.395(8) . ? C47 C58 1.490(8) . ? C48 C49 1.433(8) . ? C48 C56 1.439(8) . ? C49 C50 1.312(8) . ? C50 C51 1.422(8) . ? C51 C52 1.378(8) . ? C51 C55 1.426(7) . ? C52 C53 1.395(9) . ? C52 C59 1.541(8) . ? C53 C54 1.419(8) . ? C53 C60 1.496(9) . ? C55 C56 1.437(8) . ? C61 C62 1.396(8) . ? C62 C63 1.355(8) . ? C62 C73 1.494(8) . ? C63 C64 1.434(8) . ? C63 C74 1.495(8) . ? C64 C72 1.397(8) . ? C64 C65 1.426(8) . ? C65 C66 1.344(8) . ? C66 C67 1.424(8) . ? C67 C71 1.372(8) . ? C67 C68 1.425(8) . ? C68 C69 1.370(8) . ? C68 C75 1.509(8) . ? C69 C70 1.419(8) . ? C69 C76 1.471(7) . ? C71 C72 1.431(7) . ? C77 C78 1.382(8) . ? C78 C79 1.382(8) . ? C78 C89 1.515(8) . ? C79 C80 1.408(8) . ? C79 C90 1.498(8) . ? C80 C88 1.393(8) . ? C80 C81 1.439(8) . ? C81 C82 1.346(8) . ? C82 C83 1.407(8) . ? C83 C87 1.395(8) . ? C83 C84 1.429(8) . ? C84 C85 1.376(10) . ? C84 C91 1.508(9) . ? C85 C86 1.392(9) . ? C85 C92 1.536(10) . ? C87 C88 1.440(7) . ? C93 C94 1.398(12) . ? C94 C95 1.392(13) . ? C94 C105 1.554(12) . ? C95 C96 1.425(11) . ? C95 C106 1.520(12) . ? C96 C97 1.398(11) . ? C96 C104 1.416(10) . ? C97 C98 1.351(11) . ? C98 C99 1.441(9) . ? C99 C103 1.408(9) . ? C99 C100 1.419(9) . ? C100 C101 1.383(8) . ? C100 C107 1.475(9) . ? C101 C102 1.406(8) . ? C101 C108 1.524(9) . ? C103 C104 1.434(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N7 90.75(19) . . ? N4 Co1 N16 97.61(19) . . ? N7 Co1 N16 90.1(2) . . ? N4 Co1 N13 90.93(18) . . ? N7 Co1 N13 101.7(2) . . ? N16 Co1 N13 165.32(15) . . ? N4 Co1 N14 167.93(16) . . ? N7 Co1 N14 91.6(2) . . ? N16 Co1 N14 94.2(2) . . ? N13 Co1 N14 77.00(18) . . ? N4 Co1 N15 95.4(2) . . ? N7 Co1 N15 165.67(16) . . ? N16 Co1 N15 76.23(18) . . ? N13 Co1 N15 91.16(18) . . ? N14 Co1 N15 85.1(2) . . ? N5 Co2 N8 92.76(19) . . ? N5 Co2 N19 90.0(2) . . ? N8 Co2 N19 173.64(19) . . ? N5 Co2 N20 92.51(19) . . ? N8 Co2 N20 92.3(2) . . ? N19 Co2 N20 81.8(2) . . ? N5 Co2 N17 91.69(19) . . ? N8 Co2 N17 90.5(2) . . ? N19 Co2 N17 95.2(2) . . ? N20 Co2 N17 174.83(16) . . ? N5 Co2 N18 171.66(19) . . ? N8 Co2 N18 92.6(2) . . ? N19 Co2 N18 85.3(2) . . ? N20 Co2 N18 93.6(2) . . ? N17 Co2 N18 81.89(19) . . ? N9 Co3 N6 90.49(18) . . ? N9 Co3 N23 176.48(16) . . ? N6 Co3 N23 87.90(18) . . ? N9 Co3 N24 95.3(2) . . ? N6 Co3 N24 95.0(2) . . ? N23 Co3 N24 81.7(2) . . ? N9 Co3 N22 92.29(19) . . ? N6 Co3 N22 175.16(17) . . ? N23 Co3 N22 89.54(19) . . ? N24 Co3 N22 88.7(2) . . ? N9 Co3 N21 94.4(2) . . ? N6 Co3 N21 95.81(19) . . ? N23 Co3 N21 88.9(2) . . ? N24 Co3 N21 165.45(17) . . ? N22 Co3 N21 80.0(2) . . ? C5 Fe1 C2 89.1(2) . . ? C5 Fe1 C4 88.6(2) . . ? C2 Fe1 C4 87.8(2) . . ? C5 Fe1 C1 175.1(2) . . ? C2 Fe1 C1 88.0(3) . . ? C4 Fe1 C1 87.3(2) . . ? C5 Fe1 C6 86.8(2) . . ? C2 Fe1 C6 175.7(2) . . ? C4 Fe1 C6 93.3(2) . . ? C1 Fe1 C6 96.2(2) . . ? C5 Fe1 C3 93.7(2) . . ? C2 Fe1 C3 91.6(2) . . ? C4 Fe1 C3 177.5(2) . . ? C1 Fe1 C3 90.3(2) . . ? C6 Fe1 C3 87.5(2) . . ? C10 Fe2 C8 175.0(3) . . ? C10 Fe2 C7 93.2(3) . . ? C8 Fe2 C7 87.4(3) . . ? C10 Fe2 C9 86.4(3) . . ? C8 Fe2 C9 88.6(2) . . ? C7 Fe2 C9 91.0(2) . . ? C10 Fe2 C12 90.1(3) . . ? C8 Fe2 C12 89.6(3) . . ? C7 Fe2 C12 176.0(3) . . ? C9 Fe2 C12 91.5(3) . . ? C10 Fe2 C11 90.3(3) . . ? C8 Fe2 C11 94.7(3) . . ? C7 Fe2 C11 87.0(3) . . ? C9 Fe2 C11 176.1(2) . . ? C12 Fe2 C11 90.7(3) . . ? C4 N4 Co1 153.6(4) . . ? C5 N5 Co2 163.8(4) . . ? C6 N6 Co3 157.6(4) . . ? C7 N7 Co1 163.8(4) . . ? C8 N8 Co2 160.5(4) . . ? C9 N9 Co3 163.3(4) . . ? C45 N13 C56 115.0(5) . . ? C45 N13 Co1 130.7(3) . . ? C56 N13 Co1 114.2(4) . . ? C54 N14 C55 116.5(5) . . ? C54 N14 Co1 128.1(4) . . ? C55 N14 Co1 115.4(3) . . ? C61 N15 C72 115.0(5) . . ? C61 N15 Co1 129.8(3) . . ? C72 N15 Co1 115.2(3) . . ? C70 N16 C71 116.6(4) . . ? C70 N16 Co1 127.4(4) . . ? C71 N16 Co1 116.0(3) . . ? C77 N17 C88 117.0(5) . . ? C77 N17 Co2 129.1(4) . . ? C88 N17 Co2 113.8(3) . . ? C86 N18 C87 118.2(5) . . ? C86 N18 Co2 129.5(4) . . ? C87 N18 Co2 112.2(3) . . ? C104 N19 C93 118.8(6) . . ? C104 N19 Co2 113.5(4) . . ? C93 N19 Co2 127.7(5) . . ? C102 N20 C103 118.5(5) . . ? C102 N20 Co2 128.9(4) . . ? C103 N20 Co2 112.5(4) . . ? C38 N21 C39 117.8(4) . . ? C38 N21 Co3 128.3(3) . . ? C39 N21 Co3 113.3(3) . . ? C29 N22 C40 115.9(4) . . ? C29 N22 Co3 129.9(4) . . ? C40 N22 Co3 113.9(3) . . ? C13 N23 C24 116.5(5) . . ? C13 N23 Co3 131.0(4) . . ? C24 N23 Co3 112.5(3) . . ? C22 N24 C23 118.0(5) . . ? C22 N24 Co3 128.1(4) . . ? C23 N24 Co3 113.7(4) . . ? N1 C1 Fe1 176.9(5) . . ? N2 C2 Fe1 176.2(5) . . ? N3 C3 Fe1 176.8(5) . . ? N4 C4 Fe1 177.4(5) . . ? N5 C5 Fe1 175.2(4) . . ? N6 C6 Fe1 171.3(4) . . ? N7 C7 Fe2 174.3(5) . . ? N8 C8 Fe2 175.0(5) . . ? N9 C9 Fe2 176.5(4) . . ? N10 C10 Fe2 176.3(5) . . ? N11 C11 Fe2 177.3(6) . . ? N12 C12 Fe2 178.2(6) . . ? N23 C13 C14 126.2(5) . . ? C15 C14 C13 118.5(5) . . ? C15 C14 C25 121.3(5) . . ? C13 C14 C25 120.2(5) . . ? C14 C15 C16 118.5(5) . . ? C14 C15 C26 120.6(5) . . ? C16 C15 C26 120.8(5) . . ? C24 C16 C17 118.0(5) . . ? C24 C16 C15 117.2(5) . . ? C17 C16 C15 124.7(5) . . ? C18 C17 C16 121.5(6) . . ? C17 C18 C19 121.6(6) . . ? C23 C19 C20 119.5(5) . . ? C23 C19 C18 116.0(5) . . ? C20 C19 C18 124.5(5) . . ? C21 C20 C19 117.9(5) . . ? C21 C20 C27 119.1(6) . . ? C19 C20 C27 122.9(6) . . ? C20 C21 C22 118.7(6) . . ? C20 C21 C28 122.8(5) . . ? C22 C21 C28 118.5(5) . . ? N24 C22 C21 123.5(5) . . ? N24 C23 C19 122.3(5) . . ? N24 C23 C24 115.1(5) . . ? C19 C23 C24 122.6(5) . . ? N23 C24 C16 123.0(5) . . ? N23 C24 C23 116.9(5) . . ? C16 C24 C23 120.1(5) . . ? N22 C29 C30 125.5(5) . . ? C29 C30 C31 119.1(5) . . ? C29 C30 C41 120.5(5) . . ? C31 C30 C41 120.3(5) . . ? C30 C31 C32 118.2(5) . . ? C30 C31 C42 122.9(6) . . ? C32 C31 C42 118.9(6) . . ? C40 C32 C33 117.9(5) . . ? C40 C32 C31 117.2(5) . . ? C33 C32 C31 124.9(6) . . ? C34 C33 C32 121.6(6) . . ? C33 C34 C35 121.9(6) . . ? C39 C35 C34 117.4(5) . . ? C39 C35 C36 118.3(5) . . ? C34 C35 C36 124.3(5) . . ? C37 C36 C35 116.7(5) . . ? C37 C36 C43 121.2(6) . . ? C35 C36 C43 122.0(5) . . ? C36 C37 C38 120.2(5) . . ? C36 C37 C44 121.3(5) . . ? C38 C37 C44 118.5(5) . . ? N21 C38 C37 123.4(5) . . ? N21 C39 C35 123.4(5) . . ? N21 C39 C40 116.7(4) . . ? C35 C39 C40 119.9(5) . . ? N22 C40 C32 124.1(5) . . ? N22 C40 C39 114.6(4) . . ? C32 C40 C39 121.3(5) . . ? N13 C45 C46 125.9(5) . . ? C47 C46 C45 118.8(5) . . ? C47 C46 C57 122.7(5) . . ? C45 C46 C57 118.5(5) . . ? C46 C47 C48 118.4(5) . . ? C46 C47 C58 122.2(5) . . ? C48 C47 C58 119.3(5) . . ? C47 C48 C49 124.3(5) . . ? C47 C48 C56 118.8(5) . . ? C49 C48 C56 116.8(5) . . ? C50 C49 C48 123.1(5) . . ? C49 C50 C51 122.7(5) . . ? C52 C51 C50 124.6(5) . . ? C52 C51 C55 117.7(5) . . ? C50 C51 C55 117.7(5) . . ? C51 C52 C53 119.3(5) . . ? C51 C52 C59 119.8(5) . . ? C53 C52 C59 120.9(5) . . ? C52 C53 C54 117.6(5) . . ? C52 C53 C60 123.3(5) . . ? C54 C53 C60 119.0(6) . . ? N14 C54 C53 124.8(6) . . ? N14 C55 C51 123.9(5) . . ? N14 C55 C56 116.1(5) . . ? C51 C55 C56 119.9(5) . . ? N13 C56 C55 117.2(5) . . ? N13 C56 C48 123.0(5) . . ? C55 C56 C48 119.7(5) . . ? N15 C61 C62 126.4(5) . . ? C63 C62 C61 118.7(5) . . ? C63 C62 C73 121.7(5) . . ? C61 C62 C73 119.6(5) . . ? C62 C63 C64 117.7(5) . . ? C62 C63 C74 120.4(5) . . ? C64 C63 C74 121.8(5) . . ? C72 C64 C65 117.9(5) . . ? C72 C64 C63 118.7(5) . . ? C65 C64 C63 123.4(5) . . ? C66 C65 C64 120.9(6) . . ? C65 C66 C67 122.3(5) . . ? C71 C67 C66 117.8(5) . . ? C71 C67 C68 118.6(5) . . ? C66 C67 C68 123.5(5) . . ? C69 C68 C67 119.2(5) . . ? C69 C68 C75 121.0(5) . . ? C67 C68 C75 119.8(5) . . ? C68 C69 C70 116.9(5) . . ? C68 C69 C76 124.0(5) . . ? C70 C69 C76 119.1(5) . . ? N16 C70 C69 125.4(5) . . ? N16 C71 C67 123.2(5) . . ? N16 C71 C72 116.0(4) . . ? C67 C71 C72 120.8(5) . . ? N15 C72 C64 123.4(4) . . ? N15 C72 C71 116.4(5) . . ? C64 C72 C71 120.2(5) . . ? N17 C77 C78 124.1(5) . . ? C79 C78 C77 119.7(5) . . ? C79 C78 C89 122.5(5) . . ? C77 C78 C89 117.8(5) . . ? C78 C79 C80 117.1(5) . . ? C78 C79 C90 121.2(5) . . ? C80 C79 C90 121.6(5) . . ? C88 C80 C79 118.6(5) . . ? C88 C80 C81 116.4(5) . . ? C79 C80 C81 125.0(5) . . ? C82 C81 C80 122.0(6) . . ? C81 C82 C83 122.6(6) . . ? C87 C83 C82 117.3(5) . . ? C87 C83 C84 117.4(6) . . ? C82 C83 C84 125.2(6) . . ? C85 C84 C83 118.3(6) . . ? C85 C84 C91 122.9(6) . . ? C83 C84 C91 118.7(6) . . ? C84 C85 C86 119.7(6) . . ? C84 C85 C92 121.8(6) . . ? C86 C85 C92 118.5(7) . . ? N18 C86 C85 123.3(6) . . ? N18 C87 C83 123.0(5) . . ? N18 C87 C88 116.4(5) . . ? C83 C87 C88 120.6(5) . . ? N17 C88 C80 123.4(5) . . ? N17 C88 C87 115.6(5) . . ? C80 C88 C87 121.0(5) . . ? N19 C93 C94 122.1(7) . . ? C95 C94 C93 121.0(8) . . ? C95 C94 C105 123.1(8) . . ? C93 C94 C105 115.8(9) . . ? C94 C95 C96 116.5(7) . . ? C94 C95 C106 125.1(7) . . ? C96 C95 C106 118.2(7) . . ? C97 C96 C104 116.8(7) . . ? C97 C96 C95 125.4(7) . . ? C104 C96 C95 117.8(7) . . ? C98 C97 C96 124.3(7) . . ? C97 C98 C99 120.8(6) . . ? C103 C99 C100 118.4(5) . . ? C103 C99 C98 116.6(6) . . ? C100 C99 C98 125.0(6) . . ? C101 C100 C99 116.9(5) . . ? C101 C100 C107 120.1(6) . . ? C99 C100 C107 123.0(6) . . ? C100 C101 C102 120.6(5) . . ? C100 C101 C108 121.9(5) . . ? C102 C101 C108 117.5(5) . . ? N20 C102 C101 122.5(5) . . ? N20 C103 C99 122.9(6) . . ? N20 C103 C104 115.7(5) . . ? C99 C103 C104 121.3(5) . . ? N19 C104 C96 123.8(6) . . ? N19 C104 C103 116.1(5) . . ? C96 C104 C103 120.2(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.925 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.120 #end===================================================================== data_{[Co(tmphen)2]3[Fe(CN)6]2}_110K #=================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; {[Co(tmphen)2]3[Fe(CN)6]2}.13H2O ; _chemical_name_common '{[Co(tmphen)2]3[Fe(CN)6]2}.13H2O' _chemical_formula_moiety 'C108 H122 Co3 Fe2 N24 O13' _chemical_formula_sum 'C108 H122 Co3 Fe2 N24 O13' _chemical_formula_weight 2252.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.02(1) _cell_length_b 25.03(2) _cell_length_c 24.65(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.86(2) _cell_angle_gamma 90.00 _cell_volume 11626(15) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 58251 _cell_measurement_theta_min 2.1885 _cell_measurement_theta_max 21.3595 _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4596 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8738 _exptl_absorpt_correction_T_max 0.9176 _exptl_absorpt_process_details 'SADABS: Bruker,2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'BRUKER APEX' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45873 _diffrn_reflns_av_R_equivalents 0.0953 _diffrn_reflns_av_sigmaI/netI 0.0908 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 20.81 _reflns_number_total 12158 _reflns_number_gt 7750 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER, 2000)' _computing_cell_refinement 'SAINT (BRUKER, 2001)' _computing_data_reduction 'SAINT (BRUKER, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1371P)^2^+5.25P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00060(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12158 _refine_ls_number_parameters 1399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1219 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.2358 _refine_ls_wR_factor_gt 0.2058 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.06323(6) 0.37300(5) 0.61496(5) 0.0431(4) Uani 1 1 d . A -1 Co2 Co 0.29338(6) 0.36651(5) 0.83001(5) 0.0424(4) Uani 1 1 d . A -1 Co3 Co 0.35751(6) 0.54801(5) 0.66510(5) 0.0395(4) Uani 1 1 d . A -1 Fe1 Fe 0.32562(6) 0.35432(5) 0.63580(5) 0.0433(4) Uani 1 1 d . A -1 Fe2 Fe 0.14453(7) 0.51633(6) 0.75475(5) 0.0504(5) Uani 1 1 d . A -1 O5S O 0.401(3) 0.217(3) 0.529(2) 0.15(2) Uiso 0.20 1 d P B -5 O6S O 0.4396(12) 0.2477(9) 0.5473(9) 0.127(7) Uiso 0.50 1 d P C -6 O7S O 0.4944(14) 0.2109(10) 0.5613(9) 0.136(7) Uiso 0.50 1 d P D -7 O8S O 0.546(2) 0.1891(15) 0.5615(15) 0.117(12) Uiso 0.30 1 d P E -8 O9S O 0.561(2) 0.2135(18) 0.5863(18) 0.150(15) Uiso 0.30 1 d P F -9 O10S O 0.280(2) 0.1109(17) 0.8032(16) 0.147(13) Uiso 0.30 1 d P G -10 O11S O 0.3064(9) 0.1779(7) 0.7620(7) 0.101(5) Uiso 0.50 1 d P H -11 O12S O 0.3168(10) 0.1940(8) 0.9099(8) 0.123(6) Uiso 0.50 1 d P I -12 O13S O 0.6364(12) 0.3506(10) 0.6607(10) 0.148(8) Uiso 0.50 1 d P J -13 O14S O 0.6348(9) 0.3894(8) 0.6802(7) 0.102(6) Uiso 0.50 1 d P K -14 O15S O 0.7249(16) 0.2657(14) 0.6686(13) 0.220(13) Uiso 0.50 1 d P L -15 O16S O 0.7275(17) 0.3872(14) 0.7611(13) 0.127(11) Uiso 0.30 1 d P M -16 O17S O 0.8620(19) 0.4546(14) 0.7679(14) 0.138(12) Uiso 0.30 1 d P N -17 O18S O 0.860(3) 0.5692(19) 0.8502(19) 0.114(15) Uiso 0.20 1 d P O -18 O19S O 0.9362(12) 0.5843(9) 0.8661(9) 0.145(8) Uiso 0.50 1 d P P -19 O20S O 0.916(2) 0.5968(16) 0.9333(17) 0.161(14) Uiso 0.30 1 d P Q -20 O21S O 0.2805(12) 0.8359(9) 0.4465(9) 0.147(8) Uiso 0.50 1 d P R -21 O22S O 0.271(3) 0.806(2) 0.539(2) 0.15(2) Uiso 0.20 1 d P S -22 O23S O 0.2318(12) 0.8156(10) 0.5891(10) 0.143(8) Uiso 0.50 1 d P T -23 O24S O 0.214(3) 0.858(2) 0.617(2) 0.22(2) Uiso 0.30 1 d P U -24 O25S O 0.2734(18) 0.7032(15) 0.8122(15) 0.124(11) Uiso 0.30 1 d P V -25 O26S O 0.2504(13) 0.6753(11) 0.7790(10) 0.158(9) Uiso 0.50 1 d P W -26 O27S O 0.279(2) 0.5978(19) 0.9792(18) 0.181(16) Uiso 0.30 1 d P X -27 O28S O 0.2897(17) 0.5293(13) 0.9884(12) 0.168(13) Uiso 0.50 1 d P Y -28 O29S O 0.3216(17) 0.5156(12) 0.9916(12) 0.121(10) Uiso 0.40 1 d P Z -29 O30S O 0.192(2) 0.4879(19) 0.9583(19) 0.185(17) Uiso 0.30 1 d P A -39 N1 N 0.3097(5) 0.3282(4) 0.5120(4) 0.072(3) Uani 1 1 d . A -1 N2 N 0.3274(4) 0.2315(4) 0.6549(4) 0.074(3) Uani 1 1 d . A -1 N3 N 0.4893(5) 0.3630(4) 0.6389(4) 0.071(3) Uani 1 1 d . A -1 N4 N 0.1639(4) 0.3442(3) 0.6258(3) 0.0421(19) Uani 1 1 d . A -1 N5 N 0.3234(4) 0.3688(3) 0.7590(4) 0.045(2) Uani 1 1 d . A -1 N6 N 0.3304(4) 0.4780(4) 0.6332(3) 0.046(2) Uani 1 1 d . A -1 N7 N 0.0955(4) 0.4419(4) 0.6577(3) 0.051(2) Uani 1 1 d . A -1 N8 N 0.2165(4) 0.4174(3) 0.8095(3) 0.045(2) Uani 1 1 d . A -1 N9 N 0.2834(4) 0.5435(3) 0.7116(3) 0.0416(19) Uani 1 1 d . A -1 N10 N 0.0923(5) 0.6217(4) 0.6972(4) 0.073(3) Uani 1 1 d . A -1 N11 N -0.0050(6) 0.4928(5) 0.7880(5) 0.112(4) Uani 1 1 d . A -1 N12 N 0.1889(6) 0.5798(4) 0.8610(4) 0.087(3) Uani 1 1 d . A -1 N13 N 0.0730(4) 0.3970(3) 0.5331(3) 0.048(2) Uani 1 1 d . A -1 N14 N -0.0396(4) 0.4071(3) 0.5862(4) 0.051(2) Uani 1 1 d . A -1 N15 N 0.0142(3) 0.2975(3) 0.5865(3) 0.0388(18) Uani 1 1 d . A -1 N16 N 0.0303(4) 0.3387(3) 0.6867(3) 0.0446(19) Uani 1 1 d . A -1 N17 N 0.2285(4) 0.3056(3) 0.8079(3) 0.0441(19) Uani 1 1 d . A -1 N18 N 0.2619(4) 0.3522(3) 0.9026(3) 0.053(2) Uani 1 1 d . A -1 N19 N 0.3753(5) 0.3202(3) 0.8563(3) 0.065(3) Uani 1 1 d . A -1 N20 N 0.3597(4) 0.4246(3) 0.8574(3) 0.048(2) Uani 1 1 d . A -1 N21 N 0.4325(4) 0.5187(3) 0.7229(3) 0.0409(19) Uani 1 1 d . A -1 N22 N 0.3945(4) 0.6181(3) 0.6998(3) 0.047(2) Uani 1 1 d . A -1 N23 N 0.4295(4) 0.5534(3) 0.6134(3) 0.0425(19) Uani 1 1 d . A -1 N24 N 0.3005(4) 0.5908(3) 0.6065(3) 0.051(2) Uani 1 1 d . A -1 O33S O -0.123(3) 0.4479(19) 0.9141(19) 0.152(16) Uiso 0.25 1 d P B -33 O36S O 0.0709(13) 0.4149(11) 0.9943(11) 0.158(9) Uiso 0.50 1 d P C -36 O32S O 0.251(2) 0.0715(19) 0.780(2) 0.132(14) Uiso 0.25 1 d P D -32 C1 C 0.3163(5) 0.3399(4) 0.5573(5) 0.054(3) Uani 1 1 d . A -1 C2 C 0.3295(5) 0.2782(5) 0.6474(4) 0.055(3) Uani 1 1 d . A -1 C3 C 0.4276(6) 0.3584(4) 0.6386(4) 0.051(3) Uani 1 1 d . A -1 C4 C 0.2249(5) 0.3497(3) 0.6296(3) 0.039(2) Uani 1 1 d . A -1 C5 C 0.3283(4) 0.3644(3) 0.7128(4) 0.040(2) Uani 1 1 d . A -1 C6 C 0.3248(4) 0.4314(5) 0.6300(4) 0.045(2) Uani 1 1 d . A -1 C7 C 0.1153(4) 0.4723(4) 0.6933(4) 0.044(2) Uani 1 1 d . A -1 C8 C 0.1864(5) 0.4540(4) 0.7889(4) 0.043(2) Uani 1 1 d . A -1 C9 C 0.2315(5) 0.5319(3) 0.7286(3) 0.039(2) Uani 1 1 d . A -1 C10 C 0.1099(5) 0.5811(5) 0.7190(4) 0.057(3) Uani 1 1 d . A -1 C11 C 0.0510(7) 0.5021(5) 0.7771(4) 0.079(4) Uani 1 1 d . A -1 C12 C 0.1719(6) 0.5565(4) 0.8204(5) 0.065(3) Uani 1 1 d . A -1 C13 C 0.4940(5) 0.5323(4) 0.6178(4) 0.053(3) Uani 1 1 d . A -1 H13 H 0.5099 0.5133 0.6495 0.063 Uiso 1 1 calc R . . C14 C 0.5393(5) 0.5365(4) 0.5784(5) 0.056(3) Uani 1 1 d . A -1 C15 C 0.5172(6) 0.5640(4) 0.5309(5) 0.062(3) Uani 1 1 d . A -1 C16 C 0.4483(6) 0.5889(4) 0.5243(4) 0.055(3) Uani 1 1 d . A -1 C17 C 0.4183(6) 0.6199(4) 0.4791(5) 0.067(3) Uani 1 1 d . A -1 H17 H 0.4438 0.6247 0.4499 0.080 Uiso 1 1 calc R . . C18 C 0.3520(7) 0.6435(4) 0.4768(4) 0.073(3) Uani 1 1 d . A -1 H18 H 0.3348 0.6644 0.4468 0.088 Uiso 1 1 calc R . . C19 C 0.3086(5) 0.6360(4) 0.5210(4) 0.060(3) Uani 1 1 d . A -1 C20 C 0.2397(6) 0.6598(4) 0.5221(4) 0.064(3) Uani 1 1 d . A -1 C21 C 0.2044(5) 0.6463(4) 0.5664(4) 0.057(3) Uani 1 1 d . A -1 C22 C 0.2351(5) 0.6118(4) 0.6065(4) 0.051(3) Uani 1 1 d . A -1 H22 H 0.2096 0.6026 0.6347 0.061 Uiso 1 1 calc R . . C23 C 0.3367(5) 0.6039(4) 0.5642(4) 0.045(2) Uani 1 1 d . A -1 C24 C 0.4059(5) 0.5810(4) 0.5675(4) 0.044(2) Uani 1 1 d . A -1 C25 C 0.6126(5) 0.5140(4) 0.5882(5) 0.076(3) Uani 1 1 d . A -1 H25A H 0.6192 0.4898 0.5591 0.114 Uiso 1 1 calc R . . H25B H 0.6191 0.4952 0.6225 0.114 Uiso 1 1 calc R . . H25C H 0.6465 0.5425 0.5893 0.114 Uiso 1 1 calc R . . C26 C 0.5641(6) 0.5717(5) 0.4866(5) 0.084(4) Uani 1 1 d . A -1 H26A H 0.6004 0.5974 0.4987 0.126 Uiso 1 1 calc R . . H26B H 0.5360 0.5844 0.4538 0.126 Uiso 1 1 calc R . . H26C H 0.5857 0.5383 0.4793 0.126 Uiso 1 1 calc R . . C27 C 0.2054(6) 0.6959(5) 0.4769(4) 0.084(4) Uani 1 1 d . A -1 H27A H 0.1593 0.6822 0.4629 0.125 Uiso 1 1 calc R . . H27B H 0.2344 0.6971 0.4479 0.125 Uiso 1 1 calc R . . H27C H 0.2007 0.7312 0.4911 0.125 Uiso 1 1 calc R . . C28 C 0.1326(5) 0.6711(4) 0.5718(4) 0.063(3) Uani 1 1 d . A -1 H28A H 0.1155 0.6572 0.6039 0.094 Uiso 1 1 calc R . . H28B H 0.0995 0.6624 0.5400 0.094 Uiso 1 1 calc R . . H28C H 0.1374 0.7092 0.5748 0.094 Uiso 1 1 calc R . . C29 C 0.3710(5) 0.6689(4) 0.6896(4) 0.058(3) Uani 1 1 d . A -1 H29 H 0.3296 0.6739 0.6653 0.070 Uiso 1 1 calc R . . C30 C 0.4051(6) 0.7135(4) 0.7132(5) 0.072(3) Uani 1 1 d . A -1 C31 C 0.4655(6) 0.7081(4) 0.7506(5) 0.077(3) Uani 1 1 d . A -1 C32 C 0.4910(5) 0.6550(4) 0.7617(4) 0.063(3) Uani 1 1 d . A -1 C33 C 0.5552(6) 0.6430(5) 0.7973(5) 0.084(4) Uani 1 1 d . A -1 H33 H 0.5824 0.6708 0.8141 0.101 Uiso 1 1 calc R . . C34 C 0.5773(6) 0.5911(4) 0.8071(5) 0.083(4) Uani 1 1 d . A -1 H34 H 0.6195 0.5848 0.8300 0.100 Uiso 1 1 calc R . . C35 C 0.5375(6) 0.5470(4) 0.7832(4) 0.060(3) Uani 1 1 d . A -1 C36 C 0.5570(5) 0.4925(4) 0.7932(4) 0.066(3) Uani 1 1 d . A -1 C37 C 0.5112(5) 0.4534(4) 0.7693(4) 0.053(3) Uani 1 1 d . A -1 C38 C 0.4500(5) 0.4680(4) 0.7338(4) 0.044(2) Uani 1 1 d . A -1 H38 H 0.4206 0.4412 0.7174 0.052 Uiso 1 1 calc R . . C39 C 0.4749(5) 0.5577(4) 0.7476(4) 0.041(2) Uani 1 1 d . A -1 C40 C 0.4539(5) 0.6115(4) 0.7361(4) 0.050(3) Uani 1 1 d . A -1 C41 C 0.3729(7) 0.7684(4) 0.6978(6) 0.107(5) Uani 1 1 d . A -1 H41A H 0.3705 0.7889 0.7304 0.160 Uiso 1 1 calc R . . H41B H 0.3260 0.7640 0.6783 0.160 Uiso 1 1 calc R . . H41C H 0.4020 0.7868 0.6749 0.160 Uiso 1 1 calc R . . C42 C 0.5053(8) 0.7553(5) 0.7741(6) 0.133(6) Uani 1 1 d . A -1 H42A H 0.5398 0.7655 0.7510 0.199 Uiso 1 1 calc R . . H42B H 0.5290 0.7468 0.8100 0.199 Uiso 1 1 calc R . . H42C H 0.4730 0.7844 0.7766 0.199 Uiso 1 1 calc R . . C43 C 0.6253(6) 0.4763(4) 0.8284(5) 0.096(4) Uani 1 1 d . A -1 H43A H 0.6148 0.4638 0.8632 0.144 Uiso 1 1 calc R . . H43B H 0.6565 0.5065 0.8338 0.144 Uiso 1 1 calc R . . H43C H 0.6478 0.4483 0.8105 0.144 Uiso 1 1 calc R . . C44 C 0.5254(5) 0.3940(4) 0.7767(4) 0.067(3) Uani 1 1 d . A -1 H44A H 0.5659 0.3843 0.7595 0.101 Uiso 1 1 calc R . . H44B H 0.4847 0.3742 0.7603 0.101 Uiso 1 1 calc R . . H44C H 0.5346 0.3858 0.8151 0.101 Uiso 1 1 calc R . . C45 C 0.1273(5) 0.3906(4) 0.5045(4) 0.052(3) Uani 1 1 d . A -1 H45 H 0.1681 0.3744 0.5222 0.062 Uiso 1 1 calc R . . C46 C 0.1278(5) 0.4066(4) 0.4495(4) 0.053(3) Uani 1 1 d . A -1 C47 C 0.0680(6) 0.4292(4) 0.4207(4) 0.057(3) Uani 1 1 d . A -1 C48 C 0.0087(5) 0.4368(4) 0.4491(4) 0.053(3) Uani 1 1 d . A -1 C49 C -0.0567(6) 0.4607(4) 0.4249(4) 0.059(3) Uani 1 1 d . A -1 H49 H -0.0619 0.4711 0.3884 0.071 Uiso 1 1 calc R . . C50 C -0.1103(6) 0.4683(4) 0.4537(4) 0.055(3) Uani 1 1 d . A -1 H50 H -0.1503 0.4861 0.4367 0.066 Uiso 1 1 calc R . . C51 C -0.1104(5) 0.4516(4) 0.5075(5) 0.052(3) Uani 1 1 d . A -1 C52 C -0.1665(6) 0.4564(4) 0.5378(5) 0.065(3) Uani 1 1 d . A -1 C53 C -0.1610(5) 0.4362(4) 0.5906(5) 0.063(3) Uani 1 1 d . A -1 C54 C -0.0935(6) 0.4128(4) 0.6137(5) 0.071(3) Uani 1 1 d . A -1 H54 H -0.0882 0.4012 0.6499 0.085 Uiso 1 1 calc R . . C55 C -0.0462(5) 0.4257(4) 0.5345(5) 0.056(3) Uani 1 1 d . A -1 C56 C 0.0121(5) 0.4200(4) 0.5051(4) 0.053(3) Uani 1 1 d . A -1 C57 C 0.1938(6) 0.3971(5) 0.4235(5) 0.080(4) Uani 1 1 d . A -1 H57A H 0.2277 0.3777 0.4485 0.120 Uiso 1 1 calc R . . H57B H 0.2139 0.4308 0.4151 0.120 Uiso 1 1 calc R . . H57C H 0.1821 0.3769 0.3905 0.120 Uiso 1 1 calc R . . C58 C 0.0620(6) 0.4495(4) 0.3634(4) 0.073(3) Uani 1 1 d . A -1 H58A H 0.1073 0.4468 0.3505 0.109 Uiso 1 1 calc R . . H58B H 0.0470 0.4861 0.3624 0.109 Uiso 1 1 calc R . . H58C H 0.0277 0.4285 0.3403 0.109 Uiso 1 1 calc R . . C59 C -0.2360(5) 0.4843(5) 0.5124(5) 0.078(3) Uani 1 1 d . A -1 H59A H -0.2290 0.5223 0.5128 0.117 Uiso 1 1 calc R . . H59B H -0.2734 0.4755 0.5333 0.117 Uiso 1 1 calc R . . H59C H -0.2486 0.4724 0.4753 0.117 Uiso 1 1 calc R . . C60 C -0.2184(6) 0.4385(6) 0.6271(6) 0.106(5) Uani 1 1 d . A -1 H60A H -0.2293 0.4751 0.6339 0.158 Uiso 1 1 calc R . . H60B H -0.2022 0.4210 0.6612 0.158 Uiso 1 1 calc R . . H60C H -0.2602 0.4209 0.6094 0.158 Uiso 1 1 calc R . . C61 C 0.0076(4) 0.2751(4) 0.5364(4) 0.042(2) Uani 1 1 d . A -1 H61 H 0.0263 0.2939 0.5092 0.051 Uiso 1 1 calc R . . C62 C -0.0246(5) 0.2266(4) 0.5217(4) 0.045(2) Uani 1 1 d . A -1 C63 C -0.0543(5) 0.1978(4) 0.5598(4) 0.046(2) Uani 1 1 d . A -1 C64 C -0.0503(5) 0.2205(4) 0.6129(4) 0.050(3) Uani 1 1 d . A -1 C65 C -0.0802(6) 0.1950(4) 0.6575(4) 0.064(3) Uani 1 1 d . A -1 H65 H -0.1040 0.1627 0.6511 0.077 Uiso 1 1 calc R . . C66 C -0.0743(6) 0.2168(4) 0.7078(4) 0.067(3) Uani 1 1 d . A -1 H66 H -0.0948 0.1993 0.7350 0.081 Uiso 1 1 calc R . . C67 C -0.0370(5) 0.2671(4) 0.7211(4) 0.060(3) Uani 1 1 d . A -1 C68 C -0.0273(6) 0.2910(4) 0.7737(4) 0.059(3) Uani 1 1 d . A -1 C69 C 0.0129(5) 0.3359(4) 0.7821(3) 0.056(3) Uani 1 1 d . A -1 C70 C 0.0409(5) 0.3588(4) 0.7372(4) 0.057(3) Uani 1 1 d . A -1 H70 H 0.0682 0.3896 0.7432 0.068 Uiso 1 1 calc R . . C71 C -0.0070(5) 0.2924(4) 0.6795(4) 0.043(2) Uani 1 1 d . A -1 C72 C -0.0154(4) 0.2692(4) 0.6250(3) 0.041(2) Uani 1 1 d . A -1 C73 C -0.0257(5) 0.2064(4) 0.4644(4) 0.065(3) Uani 1 1 d . A -1 H73A H -0.0037 0.1719 0.4653 0.097 Uiso 1 1 calc R . . H73B H -0.0001 0.2307 0.4442 0.097 Uiso 1 1 calc R . . H73C H -0.0739 0.2038 0.4470 0.097 Uiso 1 1 calc R . . C74 C -0.0897(6) 0.1449(4) 0.5454(4) 0.075(3) Uani 1 1 d . A -1 H74A H -0.1327 0.1505 0.5208 0.113 Uiso 1 1 calc R . . H74B H -0.1008 0.1279 0.5782 0.113 Uiso 1 1 calc R . . H74C H -0.0583 0.1224 0.5282 0.113 Uiso 1 1 calc R . . C75 C -0.0591(7) 0.2643(5) 0.8201(4) 0.085(4) Uani 1 1 d . A -1 H75A H -0.0425 0.2822 0.8540 0.128 Uiso 1 1 calc R . . H75B H -0.0448 0.2275 0.8227 0.128 Uiso 1 1 calc R . . H75C H -0.1099 0.2665 0.8131 0.128 Uiso 1 1 calc R . . C76 C 0.0302(6) 0.3629(4) 0.8371(4) 0.071(3) Uani 1 1 d . A -1 H76A H -0.0124 0.3775 0.8480 0.106 Uiso 1 1 calc R . . H76B H 0.0637 0.3912 0.8345 0.106 Uiso 1 1 calc R . . H76C H 0.0503 0.3373 0.8638 0.106 Uiso 1 1 calc R . . C77 C 0.2110(5) 0.2839(4) 0.7592(4) 0.053(3) Uani 1 1 d . A -1 H77 H 0.2302 0.2985 0.7297 0.063 Uiso 1 1 calc R . . C78 C 0.1653(5) 0.2400(4) 0.7491(4) 0.050(3) Uani 1 1 d . A -1 C79 C 0.1341(5) 0.2183(4) 0.7919(4) 0.052(3) Uani 1 1 d . A -1 C80 C 0.1509(5) 0.2414(4) 0.8443(4) 0.050(3) Uani 1 1 d . A -1 C81 C 0.1238(5) 0.2234(4) 0.8932(4) 0.060(3) Uani 1 1 d . A -1 H81 H 0.0911 0.1956 0.8907 0.072 Uiso 1 1 calc R . . C82 C 0.1448(5) 0.2459(4) 0.9420(4) 0.058(3) Uani 1 1 d . A -1 H82 H 0.1275 0.2320 0.9725 0.070 Uiso 1 1 calc R . . C83 C 0.1924(5) 0.2902(4) 0.9497(4) 0.056(3) Uani 1 1 d . A -1 C84 C 0.2158(6) 0.3165(5) 1.0006(4) 0.071(3) Uani 1 1 d . A -1 C85 C 0.2608(6) 0.3606(5) 1.0000(4) 0.082(4) Uani 1 1 d . A -1 C86 C 0.2817(6) 0.3760(5) 0.9501(5) 0.074(3) Uani 1 1 d . A -1 H86 H 0.3118 0.4053 0.9504 0.089 Uiso 1 1 calc R . . C87 C 0.2175(5) 0.3093(4) 0.9024(4) 0.046(2) Uani 1 1 d . A -1 C88 C 0.1979(5) 0.2849(4) 0.8509(4) 0.040(2) Uani 1 1 d . A -1 C89 C 0.1530(5) 0.2179(4) 0.6913(4) 0.064(3) Uani 1 1 d . A -1 H89A H 0.1753 0.1835 0.6905 0.097 Uiso 1 1 calc R . . H89B H 0.1730 0.2418 0.6671 0.097 Uiso 1 1 calc R . . H89C H 0.1030 0.2143 0.6797 0.097 Uiso 1 1 calc R . . C90 C 0.0868(5) 0.1692(4) 0.7832(4) 0.066(3) Uani 1 1 d . A -1 H90A H 0.0603 0.1702 0.7471 0.100 Uiso 1 1 calc R . . H90B H 0.0545 0.1687 0.8099 0.100 Uiso 1 1 calc R . . H90C H 0.1156 0.1376 0.7870 0.100 Uiso 1 1 calc R . . C91 C 0.1899(6) 0.2958(5) 1.0519(4) 0.087(4) Uani 1 1 d . A -1 H91A H 0.2098 0.3170 1.0826 0.130 Uiso 1 1 calc R . . H91B H 0.2043 0.2593 1.0577 0.130 Uiso 1 1 calc R . . H91C H 0.1391 0.2980 1.0478 0.130 Uiso 1 1 calc R . . C92 C 0.2887(8) 0.3907(7) 1.0526(5) 0.131(6) Uani 1 1 d . A -1 H92A H 0.2539 0.3895 1.0773 0.197 Uiso 1 1 calc R . . H92B H 0.2980 0.4272 1.0439 0.197 Uiso 1 1 calc R . . H92C H 0.3318 0.3742 1.0695 0.197 Uiso 1 1 calc R . . C93 C 0.3813(8) 0.2672(5) 0.8532(5) 0.087(4) Uani 1 1 d . A -1 H93 H 0.3438 0.2481 0.8343 0.104 Uiso 1 1 calc R . . C94 C 0.4412(10) 0.2389(5) 0.8769(6) 0.117(6) Uani 1 1 d . A -1 C95 C 0.4976(9) 0.2663(6) 0.9045(6) 0.109(5) Uani 1 1 d . A -1 C96 C 0.4928(7) 0.3239(5) 0.9081(5) 0.090(4) Uani 1 1 d . A -1 C97 C 0.5450(7) 0.3584(6) 0.9359(5) 0.099(5) Uani 1 1 d . A -1 H97 H 0.5860 0.3434 0.9547 0.119 Uiso 1 1 calc R . . C98 C 0.5375(7) 0.4127(6) 0.9361(5) 0.096(4) Uani 1 1 d . A -1 H98 H 0.5740 0.4334 0.9542 0.115 Uiso 1 1 calc R . . C99 C 0.4750(6) 0.4385(5) 0.9092(4) 0.067(3) Uani 1 1 d . A -1 C100 C 0.4646(6) 0.4954(5) 0.9062(4) 0.069(3) Uani 1 1 d . A -1 C101 C 0.4012(6) 0.5151(4) 0.8768(4) 0.059(3) Uani 1 1 d . A -1 C102 C 0.3504(6) 0.4779(4) 0.8533(4) 0.056(3) Uani 1 1 d . A -1 H102 H 0.3084 0.4907 0.8339 0.067 Uiso 1 1 calc R . . C103 C 0.4217(6) 0.4057(4) 0.8834(4) 0.057(3) Uani 1 1 d . A -1 C104 C 0.4303(6) 0.3484(4) 0.8838(4) 0.064(3) Uani 1 1 d . A -1 C105 C 0.4396(10) 0.1780(5) 0.8742(6) 0.166(8) Uani 1 1 d . A -1 H10G H 0.4693 0.1658 0.8482 0.249 Uiso 1 1 calc R . . H10H H 0.3918 0.1661 0.8631 0.249 Uiso 1 1 calc R . . H10I H 0.4566 0.1636 0.9097 0.249 Uiso 1 1 calc R . . C106 C 0.5645(10) 0.2388(6) 0.9334(7) 0.173(9) Uani 1 1 d . A -1 H10J H 0.5578 0.2300 0.9702 0.259 Uiso 1 1 calc R . . H10K H 0.6043 0.2625 0.9340 0.259 Uiso 1 1 calc R . . H10L H 0.5732 0.2068 0.9140 0.259 Uiso 1 1 calc R . . C107 C 0.5179(7) 0.5345(5) 0.9338(5) 0.097(4) Uani 1 1 d . A -1 H10D H 0.5426 0.5512 0.9068 0.145 Uiso 1 1 calc R . . H10E H 0.5513 0.5161 0.9599 0.145 Uiso 1 1 calc R . . H10F H 0.4938 0.5613 0.9522 0.145 Uiso 1 1 calc R . . C108 C 0.3854(6) 0.5736(4) 0.8691(4) 0.072(3) Uani 1 1 d . A -1 H10A H 0.3879 0.5906 0.9042 0.108 Uiso 1 1 calc R . . H10B H 0.3387 0.5781 0.8493 0.108 Uiso 1 1 calc R . . H10C H 0.4196 0.5895 0.8488 0.108 Uiso 1 1 calc R . . O34S O -0.057(2) 0.4564(15) 0.9305(15) 0.116(12) Uiso 0.25 1 d P E -34 O35S O 0.013(2) 0.4703(17) 0.9307(16) 0.127(13) Uiso 0.25 1 d P F -35 O37S O 0.0850(12) 0.4453(10) 0.9612(10) 0.139(8) Uiso 0.50 1 d P G -37 O38S O 0.1188(11) 0.4812(8) 0.9218(8) 0.127(7) Uiso 0.50 1 d P H -38 O31S O 0.222(2) 0.0574(17) 0.740(2) 0.131(14) Uiso 0.25 1 d P I -31 O39S O 0.204(3) 0.069(2) 0.681(2) 0.158(17) Uiso 0.25 1 d P J -39 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0261(7) 0.0631(9) 0.0401(8) 0.0069(6) 0.0048(6) -0.0026(6) Co2 0.0488(8) 0.0404(8) 0.0377(8) 0.0058(6) 0.0046(6) -0.0016(6) Co3 0.0319(7) 0.0395(8) 0.0475(8) 0.0054(6) 0.0072(6) 0.0010(6) Fe1 0.0329(8) 0.0506(9) 0.0467(9) 0.0103(7) 0.0062(6) 0.0040(6) Fe2 0.0535(9) 0.0559(10) 0.0448(9) 0.0071(7) 0.0169(7) 0.0177(7) N1 0.084(7) 0.088(7) 0.044(6) 0.005(5) 0.009(5) -0.010(5) N2 0.060(6) 0.053(6) 0.106(8) 0.020(6) -0.002(5) 0.003(5) N3 0.045(6) 0.087(7) 0.081(7) 0.009(5) 0.013(5) 0.015(5) N4 0.035(5) 0.059(5) 0.031(4) 0.008(4) 0.001(4) 0.000(4) N5 0.044(5) 0.043(5) 0.047(5) 0.008(4) -0.002(4) -0.001(4) N6 0.034(5) 0.055(6) 0.049(5) 0.018(4) 0.012(4) 0.004(4) N7 0.031(5) 0.076(6) 0.047(6) 0.027(5) 0.004(4) 0.003(4) N8 0.042(5) 0.052(5) 0.040(5) 0.004(4) 0.008(4) -0.007(4) N9 0.045(5) 0.036(5) 0.043(5) 0.001(4) 0.004(4) 0.004(4) N10 0.086(7) 0.073(7) 0.061(6) -0.008(5) 0.013(5) 0.026(6) N11 0.082(8) 0.135(10) 0.134(10) 0.038(8) 0.072(8) 0.040(7) N12 0.148(10) 0.060(7) 0.059(7) -0.009(5) 0.033(7) 0.018(6) N13 0.025(5) 0.054(5) 0.062(5) 0.006(4) -0.004(4) -0.004(4) N14 0.024(5) 0.069(6) 0.063(6) -0.011(5) 0.014(4) -0.008(4) N15 0.025(4) 0.060(5) 0.033(5) 0.009(4) 0.007(4) 0.004(4) N16 0.041(5) 0.064(6) 0.029(5) 0.001(4) 0.006(4) -0.011(4) N17 0.048(5) 0.056(5) 0.030(5) 0.002(4) 0.008(4) -0.011(4) N18 0.057(5) 0.066(6) 0.036(5) -0.008(4) 0.005(4) -0.015(5) N19 0.110(8) 0.035(6) 0.051(6) 0.003(4) 0.017(5) 0.023(5) N20 0.055(6) 0.044(6) 0.047(5) 0.011(4) 0.011(4) 0.011(4) N21 0.039(5) 0.033(5) 0.050(5) -0.004(4) 0.004(4) -0.002(4) N22 0.033(5) 0.045(5) 0.060(5) 0.004(4) -0.006(4) -0.001(4) N23 0.023(5) 0.049(5) 0.057(6) 0.000(4) 0.009(4) -0.004(4) N24 0.039(5) 0.061(5) 0.053(5) -0.004(4) 0.008(4) -0.003(4) C1 0.040(6) 0.058(7) 0.066(8) 0.010(6) 0.009(6) 0.005(5) C2 0.030(6) 0.075(8) 0.059(7) 0.013(6) -0.004(5) 0.008(6) C3 0.051(7) 0.048(6) 0.052(7) 0.011(5) 0.007(5) 0.009(5) C4 0.041(6) 0.039(6) 0.035(6) 0.013(4) 0.003(5) 0.007(5) C5 0.033(6) 0.036(6) 0.050(7) 0.010(5) -0.001(5) -0.002(4) C6 0.029(6) 0.065(8) 0.044(6) 0.017(5) 0.010(4) -0.003(5) C7 0.022(5) 0.064(7) 0.045(7) 0.021(5) 0.006(5) 0.009(5) C8 0.043(6) 0.047(7) 0.042(6) 0.006(5) 0.013(5) -0.003(5) C9 0.043(6) 0.039(6) 0.033(6) 0.001(4) 0.004(5) 0.009(5) C10 0.064(7) 0.063(8) 0.047(7) -0.002(6) 0.014(5) 0.021(6) C11 0.076(9) 0.102(10) 0.065(8) 0.028(7) 0.032(7) 0.052(8) C12 0.085(8) 0.058(8) 0.056(8) 0.004(6) 0.024(7) 0.029(6) C13 0.038(7) 0.052(6) 0.070(8) -0.004(5) 0.011(6) -0.012(5) C14 0.047(7) 0.049(7) 0.074(8) -0.004(6) 0.016(6) -0.007(5) C15 0.049(7) 0.058(7) 0.089(9) -0.016(7) 0.045(7) -0.015(6) C16 0.062(8) 0.056(7) 0.047(7) 0.001(6) 0.011(6) -0.020(6) C17 0.066(8) 0.069(8) 0.071(9) -0.019(7) 0.032(7) -0.012(7) C18 0.100(10) 0.065(8) 0.055(7) 0.002(6) 0.011(7) -0.027(7) C19 0.050(7) 0.082(8) 0.047(7) 0.000(6) 0.008(6) -0.013(6) C20 0.063(8) 0.073(8) 0.050(7) 0.007(6) -0.008(6) -0.010(6) C21 0.042(7) 0.070(8) 0.056(7) -0.005(6) -0.002(6) -0.016(6) C22 0.044(7) 0.053(7) 0.054(7) 0.007(5) 0.000(5) -0.004(5) C23 0.043(7) 0.048(6) 0.045(6) 0.000(5) 0.010(5) -0.012(5) C24 0.039(6) 0.044(6) 0.051(7) -0.002(5) 0.011(5) -0.012(5) C25 0.046(7) 0.079(8) 0.110(10) -0.018(7) 0.034(6) -0.003(6) C26 0.090(9) 0.079(8) 0.095(9) -0.024(7) 0.058(8) -0.030(7) C27 0.077(8) 0.103(10) 0.070(8) 0.019(7) 0.007(7) 0.005(7) C28 0.042(6) 0.071(7) 0.072(7) 0.008(6) -0.004(5) 0.005(6) C29 0.051(7) 0.036(7) 0.082(8) 0.007(6) -0.013(6) 0.007(5) C30 0.058(7) 0.038(7) 0.111(10) -0.002(6) -0.022(7) -0.005(6) C31 0.068(8) 0.043(7) 0.106(9) -0.006(6) -0.035(7) -0.011(6) C32 0.060(7) 0.038(7) 0.084(8) 0.003(6) -0.013(6) 0.001(6) C33 0.085(9) 0.059(9) 0.095(9) 0.001(7) -0.036(8) -0.016(7) C34 0.077(8) 0.047(8) 0.109(10) 0.003(7) -0.047(7) -0.008(7) C35 0.068(8) 0.032(7) 0.075(8) 0.004(5) -0.007(6) -0.009(6) C36 0.056(7) 0.052(8) 0.083(8) -0.003(6) -0.023(6) 0.000(6) C37 0.056(7) 0.050(7) 0.050(6) 0.002(5) -0.008(6) 0.015(6) C38 0.046(6) 0.039(6) 0.046(6) 0.005(5) 0.004(5) 0.006(5) C39 0.033(6) 0.040(6) 0.046(6) 0.006(5) -0.006(5) 0.005(5) C40 0.044(6) 0.037(6) 0.065(7) 0.000(5) -0.008(6) -0.004(5) C41 0.107(10) 0.038(7) 0.156(13) -0.002(7) -0.052(9) -0.011(7) C42 0.140(13) 0.055(9) 0.171(15) 0.008(9) -0.095(11) -0.009(8) C43 0.082(9) 0.057(8) 0.130(11) 0.014(7) -0.054(8) 0.008(7) C44 0.064(7) 0.051(7) 0.079(8) 0.008(6) -0.020(6) 0.009(6) C45 0.033(6) 0.053(7) 0.069(8) 0.013(5) 0.002(6) 0.001(5) C46 0.044(7) 0.053(7) 0.056(7) 0.020(5) -0.013(6) -0.008(5) C47 0.056(7) 0.063(7) 0.055(7) 0.009(6) 0.011(6) -0.022(6) C48 0.058(7) 0.041(6) 0.054(7) 0.015(5) -0.021(6) -0.001(5) C49 0.058(7) 0.050(7) 0.063(7) 0.014(5) -0.010(7) 0.002(6) C50 0.055(7) 0.052(7) 0.053(8) 0.002(6) -0.011(6) 0.008(5) C51 0.032(6) 0.047(6) 0.077(8) -0.008(6) 0.003(6) 0.000(5) C52 0.052(8) 0.073(8) 0.071(8) -0.005(6) 0.008(6) -0.005(6) C53 0.029(6) 0.074(8) 0.087(9) -0.008(7) 0.014(6) -0.005(5) C54 0.060(8) 0.070(8) 0.081(8) -0.010(6) 0.004(7) -0.014(6) C55 0.039(7) 0.075(8) 0.054(8) -0.012(6) 0.003(6) -0.010(6) C56 0.036(6) 0.040(6) 0.079(8) -0.006(6) -0.004(6) 0.000(5) C57 0.068(8) 0.096(9) 0.080(8) 0.040(7) 0.023(7) 0.000(7) C58 0.093(9) 0.068(8) 0.053(7) 0.019(6) -0.005(6) 0.005(6) C59 0.037(6) 0.087(9) 0.104(9) -0.008(7) -0.012(6) 0.010(6) C60 0.053(8) 0.126(12) 0.147(13) -0.009(9) 0.046(8) -0.014(7) C61 0.034(6) 0.061(7) 0.034(6) 0.020(5) 0.012(5) 0.013(5) C62 0.047(6) 0.051(7) 0.037(6) 0.004(5) 0.009(5) 0.001(5) C63 0.038(6) 0.060(7) 0.036(6) -0.002(5) 0.000(5) -0.005(5) C64 0.042(6) 0.065(7) 0.042(7) 0.005(5) -0.001(5) -0.016(5) C65 0.091(8) 0.063(7) 0.039(7) -0.002(5) 0.013(6) -0.037(6) C66 0.088(8) 0.081(8) 0.038(7) 0.010(6) 0.027(6) -0.037(7) C67 0.072(7) 0.076(8) 0.035(6) -0.001(6) 0.018(5) -0.037(6) C68 0.081(8) 0.064(7) 0.035(7) 0.001(5) 0.018(5) -0.028(6) C69 0.071(7) 0.073(8) 0.024(6) 0.005(5) 0.006(5) -0.031(6) C70 0.053(7) 0.060(7) 0.056(8) 0.012(6) 0.005(6) -0.014(5) C71 0.040(6) 0.049(6) 0.040(6) 0.006(5) 0.006(5) -0.010(5) C72 0.036(6) 0.061(7) 0.029(6) 0.009(5) 0.010(5) -0.005(5) C73 0.070(7) 0.075(8) 0.052(7) -0.002(6) 0.015(6) -0.007(6) C74 0.070(8) 0.093(9) 0.062(7) -0.004(6) 0.004(6) -0.023(7) C75 0.120(10) 0.100(9) 0.039(7) -0.001(6) 0.023(7) -0.055(8) C76 0.092(9) 0.080(8) 0.045(7) -0.002(6) 0.023(6) -0.023(7) C77 0.053(7) 0.065(7) 0.041(7) 0.000(5) 0.008(5) -0.023(6) C78 0.056(7) 0.057(7) 0.035(6) 0.000(5) 0.000(5) -0.004(6) C79 0.047(6) 0.057(7) 0.049(7) 0.005(5) -0.002(5) -0.016(5) C80 0.052(6) 0.057(7) 0.041(7) 0.005(5) 0.007(5) -0.009(6) C81 0.061(7) 0.069(7) 0.054(7) -0.001(6) 0.019(6) -0.015(6) C82 0.065(7) 0.072(8) 0.039(7) 0.010(6) 0.013(5) -0.017(6) C83 0.054(7) 0.077(8) 0.037(7) 0.014(6) 0.003(5) -0.002(6) C84 0.055(7) 0.121(10) 0.036(7) -0.007(7) 0.006(6) -0.010(7) C85 0.076(9) 0.123(11) 0.048(8) -0.016(7) 0.011(6) -0.029(8) C86 0.074(8) 0.098(9) 0.052(8) -0.009(7) 0.011(6) -0.024(7) C87 0.035(6) 0.052(7) 0.049(7) 0.009(5) -0.001(5) -0.004(5) C88 0.039(6) 0.040(6) 0.041(6) 0.003(5) -0.003(5) -0.005(5) C89 0.062(7) 0.080(8) 0.052(7) -0.001(6) 0.010(5) -0.033(6) C90 0.066(7) 0.071(8) 0.064(7) 0.001(6) 0.017(6) -0.022(6) C91 0.075(8) 0.143(12) 0.043(7) 0.002(7) 0.008(6) -0.027(8) C92 0.145(13) 0.192(17) 0.057(9) -0.037(9) 0.019(9) -0.091(12) C93 0.131(12) 0.055(9) 0.074(9) 0.007(7) 0.009(8) 0.016(8) C94 0.172(16) 0.065(10) 0.094(11) -0.009(8) -0.050(11) 0.026(10) C95 0.147(14) 0.081(11) 0.087(10) 0.009(8) -0.023(10) 0.057(10) C96 0.106(11) 0.076(10) 0.078(9) -0.010(7) -0.025(8) 0.039(9) C97 0.101(11) 0.084(11) 0.096(10) -0.014(8) -0.042(8) 0.039(9) C98 0.092(10) 0.091(11) 0.093(10) -0.025(8) -0.033(8) 0.011(8) C99 0.072(8) 0.062(8) 0.061(7) -0.004(6) -0.010(6) 0.023(7) C100 0.071(8) 0.079(9) 0.055(7) -0.008(6) -0.004(6) -0.005(7) C101 0.065(8) 0.048(7) 0.067(7) -0.003(6) 0.016(6) 0.001(6) C102 0.074(8) 0.043(7) 0.054(7) 0.002(5) 0.022(6) 0.005(6) C103 0.074(8) 0.044(7) 0.051(7) -0.004(5) 0.000(6) 0.011(6) C104 0.080(9) 0.054(8) 0.053(7) -0.003(6) -0.005(6) 0.018(7) C105 0.29(2) 0.040(9) 0.146(14) -0.014(8) -0.069(14) 0.050(11) C106 0.216(19) 0.128(14) 0.144(15) -0.017(11) -0.083(14) 0.104(14) C107 0.108(10) 0.070(9) 0.103(10) -0.027(7) -0.020(8) -0.003(8) C108 0.079(8) 0.051(7) 0.084(8) -0.004(6) 0.011(7) 0.009(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N4 2.029(8) . ? Co1 N7 2.070(10) . ? Co1 N16 2.136(7) . ? Co1 N13 2.139(8) . ? Co1 N14 2.163(8) . ? Co1 N15 2.180(7) . ? Co2 N5 1.915(9) . ? Co2 N8 1.952(9) . ? Co2 N19 1.978(9) . ? Co2 N20 1.983(8) . ? Co2 N17 1.991(7) . ? Co2 N18 1.996(8) . ? Co3 N9 1.937(8) . ? Co3 N6 1.961(9) . ? Co3 N24 1.995(8) . ? Co3 N23 1.999(7) . ? Co3 N21 2.012(7) . ? Co3 N22 2.034(7) . ? Fe1 C4 1.904(10) . ? Fe1 C5 1.908(11) . ? Fe1 C2 1.927(12) . ? Fe1 C6 1.935(12) . ? Fe1 C3 1.934(11) . ? Fe1 C1 1.953(12) . ? Fe2 C9 1.896(10) . ? Fe2 C8 1.896(11) . ? Fe2 C7 1.895(12) . ? Fe2 C12 1.915(13) . ? Fe2 C10 1.918(12) . ? Fe2 C11 1.966(13) . ? N1 C1 1.146(12) . ? N2 C2 1.185(12) . ? N3 C3 1.178(11) . ? N4 C4 1.160(10) . ? N5 C5 1.161(10) . ? N6 C6 1.172(11) . ? N7 C7 1.183(11) . ? N8 C8 1.160(10) . ? N9 C9 1.162(10) . ? N10 C10 1.178(12) . ? N11 C11 1.156(13) . ? N12 C12 1.165(12) . ? N13 C45 1.336(11) . ? N13 C56 1.390(11) . ? N14 C54 1.311(12) . ? N14 C55 1.347(12) . ? N15 C61 1.344(11) . ? N15 C72 1.368(10) . ? N16 C70 1.332(11) . ? N16 C71 1.357(11) . ? N17 C77 1.318(11) . ? N17 C88 1.379(10) . ? N18 C86 1.322(12) . ? N18 C87 1.367(11) . ? N19 C93 1.337(13) . ? N19 C104 1.363(13) . ? N20 C102 1.348(11) . ? N20 C103 1.348(12) . ? N21 C38 1.329(10) . ? N21 C39 1.357(11) . ? N22 C40 1.353(11) . ? N22 C29 1.361(11) . ? N23 C13 1.326(11) . ? N23 C24 1.348(11) . ? N24 C22 1.351(11) . ? N24 C23 1.365(11) . ? C13 C14 1.388(13) . ? C14 C15 1.374(14) . ? C14 C25 1.492(13) . ? C15 C16 1.440(14) . ? C15 C26 1.513(13) . ? C16 C17 1.414(14) . ? C16 C24 1.435(12) . ? C17 C18 1.386(15) . ? C18 C19 1.465(14) . ? C19 C23 1.381(13) . ? C19 C20 1.445(14) . ? C20 C21 1.400(13) . ? C20 C27 1.512(14) . ? C21 C22 1.380(13) . ? C21 C28 1.521(13) . ? C23 C24 1.429(12) . ? C29 C30 1.379(13) . ? C30 C31 1.377(14) . ? C30 C41 1.532(14) . ? C31 C32 1.428(14) . ? C31 C42 1.479(14) . ? C32 C40 1.400(13) . ? C32 C33 1.434(14) . ? C33 C34 1.376(15) . ? C34 C35 1.420(13) . ? C35 C39 1.404(12) . ? C35 C36 1.426(13) . ? C36 C37 1.387(13) . ? C36 C43 1.516(13) . ? C37 C38 1.404(12) . ? C37 C44 1.518(13) . ? C39 C40 1.422(12) . ? C45 C46 1.414(13) . ? C46 C47 1.376(13) . ? C46 C57 1.505(13) . ? C47 C48 1.420(13) . ? C47 C58 1.491(13) . ? C48 C49 1.435(13) . ? C48 C56 1.436(13) . ? C49 C50 1.332(13) . ? C50 C51 1.389(13) . ? C51 C52 1.390(13) . ? C51 C55 1.461(13) . ? C52 C53 1.386(14) . ? C52 C59 1.549(14) . ? C53 C54 1.455(14) . ? C53 C60 1.507(14) . ? C55 C56 1.412(13) . ? C61 C62 1.385(12) . ? C62 C63 1.367(12) . ? C62 C73 1.496(12) . ? C63 C64 1.418(12) . ? C63 C74 1.507(13) . ? C64 C72 1.400(12) . ? C64 C65 1.453(12) . ? C65 C66 1.345(13) . ? C66 C67 1.460(13) . ? C67 C71 1.391(12) . ? C67 C68 1.417(12) . ? C68 C69 1.361(13) . ? C68 C75 1.519(12) . ? C69 C70 1.412(12) . ? C69 C76 1.511(13) . ? C71 C72 1.452(12) . ? C77 C78 1.403(13) . ? C78 C79 1.390(12) . ? C78 C89 1.517(12) . ? C79 C80 1.412(13) . ? C79 C90 1.521(13) . ? C80 C88 1.402(12) . ? C80 C81 1.447(13) . ? C81 C82 1.339(13) . ? C82 C83 1.427(13) . ? C83 C87 1.403(12) . ? C83 C84 1.434(14) . ? C84 C85 1.399(15) . ? C84 C91 1.508(14) . ? C85 C86 1.396(15) . ? C85 C92 1.530(15) . ? C87 C88 1.411(12) . ? C93 C94 1.400(17) . ? C94 C95 1.373(19) . ? C94 C105 1.526(17) . ? C95 C96 1.448(17) . ? C95 C106 1.533(18) . ? C96 C104 1.398(15) . ? C96 C97 1.420(17) . ? C97 C98 1.366(16) . ? C98 C99 1.434(15) . ? C99 C103 1.388(14) . ? C99 C100 1.440(15) . ? C100 C101 1.409(14) . ? C100 C107 1.503(15) . ? C101 C102 1.408(13) . ? C101 C108 1.502(13) . ? C103 C104 1.443(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N7 91.2(3) . . ? N4 Co1 N16 97.3(3) . . ? N7 Co1 N16 90.8(3) . . ? N4 Co1 N13 91.2(3) . . ? N7 Co1 N13 100.9(3) . . ? N16 Co1 N13 165.4(3) . . ? N4 Co1 N14 168.0(3) . . ? N7 Co1 N14 91.7(3) . . ? N16 Co1 N14 94.3(3) . . ? N13 Co1 N14 76.8(3) . . ? N4 Co1 N15 95.1(3) . . ? N7 Co1 N15 165.9(3) . . ? N16 Co1 N15 76.0(3) . . ? N13 Co1 N15 91.6(3) . . ? N14 Co1 N15 84.8(3) . . ? N5 Co2 N8 92.9(3) . . ? N5 Co2 N19 89.8(3) . . ? N8 Co2 N19 174.3(4) . . ? N5 Co2 N20 92.0(3) . . ? N8 Co2 N20 91.7(3) . . ? N19 Co2 N20 83.2(4) . . ? N5 Co2 N17 91.3(3) . . ? N8 Co2 N17 90.8(3) . . ? N19 Co2 N17 94.1(4) . . ? N20 Co2 N17 175.7(3) . . ? N5 Co2 N18 171.4(3) . . ? N8 Co2 N18 92.5(3) . . ? N19 Co2 N18 85.4(3) . . ? N20 Co2 N18 94.6(3) . . ? N17 Co2 N18 81.8(3) . . ? N9 Co3 N6 90.7(3) . . ? N9 Co3 N24 95.3(3) . . ? N6 Co3 N24 95.9(3) . . ? N9 Co3 N23 176.6(3) . . ? N6 Co3 N23 88.3(3) . . ? N24 Co3 N23 81.6(3) . . ? N9 Co3 N21 93.6(3) . . ? N6 Co3 N21 94.6(3) . . ? N24 Co3 N21 166.2(3) . . ? N23 Co3 N21 89.7(3) . . ? N9 Co3 N22 92.2(3) . . ? N6 Co3 N22 174.9(3) . . ? N24 Co3 N22 88.0(3) . . ? N23 Co3 N22 89.0(3) . . ? N21 Co3 N22 81.1(3) . . ? C4 Fe1 C5 88.7(4) . . ? C4 Fe1 C2 88.3(4) . . ? C5 Fe1 C2 89.3(4) . . ? C4 Fe1 C6 93.2(4) . . ? C5 Fe1 C6 86.6(4) . . ? C2 Fe1 C6 175.6(4) . . ? C4 Fe1 C3 177.4(4) . . ? C5 Fe1 C3 93.9(4) . . ? C2 Fe1 C3 91.6(4) . . ? C6 Fe1 C3 87.0(4) . . ? C4 Fe1 C1 87.4(4) . . ? C5 Fe1 C1 175.2(4) . . ? C2 Fe1 C1 87.7(4) . . ? C6 Fe1 C1 96.5(4) . . ? C3 Fe1 C1 90.0(4) . . ? C9 Fe2 C8 89.3(4) . . ? C9 Fe2 C7 91.3(4) . . ? C8 Fe2 C7 86.3(4) . . ? C9 Fe2 C12 91.7(4) . . ? C8 Fe2 C12 90.5(4) . . ? C7 Fe2 C12 175.6(4) . . ? C9 Fe2 C10 86.0(4) . . ? C8 Fe2 C10 175.2(4) . . ? C7 Fe2 C10 94.6(4) . . ? C12 Fe2 C10 88.9(4) . . ? C9 Fe2 C11 176.1(4) . . ? C8 Fe2 C11 93.8(4) . . ? C7 Fe2 C11 86.6(5) . . ? C12 Fe2 C11 90.6(5) . . ? C10 Fe2 C11 90.9(4) . . ? C4 N4 Co1 152.1(7) . . ? C5 N5 Co2 165.6(7) . . ? C6 N6 Co3 158.8(7) . . ? C7 N7 Co1 162.9(8) . . ? C8 N8 Co2 159.4(7) . . ? C9 N9 Co3 162.0(7) . . ? C45 N13 C56 116.1(8) . . ? C45 N13 Co1 129.6(6) . . ? C56 N13 Co1 114.2(6) . . ? C54 N14 C55 118.3(9) . . ? C54 N14 Co1 127.5(8) . . ? C55 N14 Co1 114.1(6) . . ? C61 N15 C72 115.2(8) . . ? C61 N15 Co1 129.8(6) . . ? C72 N15 Co1 115.1(6) . . ? C70 N16 C71 117.1(8) . . ? C70 N16 Co1 126.7(6) . . ? C71 N16 Co1 116.2(6) . . ? C77 N17 C88 117.8(8) . . ? C77 N17 Co2 129.4(6) . . ? C88 N17 Co2 112.8(6) . . ? C86 N18 C87 117.3(9) . . ? C86 N18 Co2 129.1(7) . . ? C87 N18 Co2 113.5(6) . . ? C93 N19 C104 118.5(10) . . ? C93 N19 Co2 129.3(10) . . ? C104 N19 Co2 112.1(7) . . ? C102 N20 C103 118.7(9) . . ? C102 N20 Co2 129.0(7) . . ? C103 N20 Co2 112.3(7) . . ? C38 N21 C39 118.6(8) . . ? C38 N21 Co3 128.7(6) . . ? C39 N21 Co3 112.1(6) . . ? C40 N22 C29 117.4(8) . . ? C40 N22 Co3 112.5(6) . . ? C29 N22 Co3 130.0(6) . . ? C13 N23 C24 118.1(8) . . ? C13 N23 Co3 128.8(7) . . ? C24 N23 Co3 113.0(6) . . ? C22 N24 C23 117.8(8) . . ? C22 N24 Co3 128.2(7) . . ? C23 N24 Co3 113.7(6) . . ? N1 C1 Fe1 175.6(10) . . ? N2 C2 Fe1 175.7(9) . . ? N3 C3 Fe1 176.9(9) . . ? N4 C4 Fe1 176.6(8) . . ? N5 C5 Fe1 173.5(8) . . ? N6 C6 Fe1 170.8(8) . . ? N7 C7 Fe2 174.8(8) . . ? N8 C8 Fe2 175.3(8) . . ? N9 C9 Fe2 177.1(8) . . ? N10 C10 Fe2 176.5(10) . . ? N11 C11 Fe2 176.9(12) . . ? N12 C12 Fe2 178.3(10) . . ? N23 C13 C14 124.6(10) . . ? C15 C14 C13 119.2(9) . . ? C15 C14 C25 119.8(10) . . ? C13 C14 C25 121.0(10) . . ? C14 C15 C16 118.7(9) . . ? C14 C15 C26 122.4(10) . . ? C16 C15 C26 118.8(11) . . ? C17 C16 C24 117.0(10) . . ? C17 C16 C15 126.1(10) . . ? C24 C16 C15 116.9(10) . . ? C18 C17 C16 122.1(10) . . ? C17 C18 C19 121.1(11) . . ? C23 C19 C20 118.7(9) . . ? C23 C19 C18 116.8(10) . . ? C20 C19 C18 124.5(10) . . ? C21 C20 C19 116.6(9) . . ? C21 C20 C27 121.0(10) . . ? C19 C20 C27 122.3(10) . . ? C22 C21 C20 120.6(10) . . ? C22 C21 C28 119.3(9) . . ? C20 C21 C28 120.1(10) . . ? N24 C22 C21 122.9(9) . . ? N24 C23 C19 123.2(9) . . ? N24 C23 C24 114.6(9) . . ? C19 C23 C24 122.2(9) . . ? N23 C24 C23 116.9(8) . . ? N23 C24 C16 122.4(9) . . ? C23 C24 C16 120.7(9) . . ? N22 C29 C30 123.7(9) . . ? C29 C30 C31 120.3(9) . . ? C29 C30 C41 118.1(9) . . ? C31 C30 C41 121.5(9) . . ? C30 C31 C32 116.7(9) . . ? C30 C31 C42 121.3(10) . . ? C32 C31 C42 121.8(10) . . ? C40 C32 C31 120.0(9) . . ? C40 C32 C33 116.5(9) . . ? C31 C32 C33 123.5(10) . . ? C34 C33 C32 121.3(10) . . ? C33 C34 C35 121.9(10) . . ? C39 C35 C34 117.9(9) . . ? C39 C35 C36 117.9(9) . . ? C34 C35 C36 124.2(10) . . ? C37 C36 C35 118.0(9) . . ? C37 C36 C43 119.6(9) . . ? C35 C36 C43 122.5(9) . . ? C36 C37 C38 119.9(9) . . ? C36 C37 C44 123.3(9) . . ? C38 C37 C44 116.7(9) . . ? N21 C38 C37 122.6(9) . . ? N21 C39 C35 123.0(8) . . ? N21 C39 C40 117.3(8) . . ? C35 C39 C40 119.7(9) . . ? N22 C40 C32 121.8(8) . . ? N22 C40 C39 115.7(8) . . ? C32 C40 C39 122.5(9) . . ? N13 C45 C46 125.4(9) . . ? C47 C46 C45 119.8(9) . . ? C47 C46 C57 121.6(9) . . ? C45 C46 C57 118.6(9) . . ? C46 C47 C48 117.2(9) . . ? C46 C47 C58 125.4(10) . . ? C48 C47 C58 117.3(10) . . ? C47 C48 C49 123.6(10) . . ? C47 C48 C56 120.1(9) . . ? C49 C48 C56 116.3(10) . . ? C50 C49 C48 121.4(10) . . ? C49 C50 C51 124.5(10) . . ? C50 C51 C52 126.1(10) . . ? C50 C51 C55 117.3(9) . . ? C52 C51 C55 116.6(10) . . ? C53 C52 C51 120.6(10) . . ? C53 C52 C59 119.7(10) . . ? C51 C52 C59 119.7(10) . . ? C52 C53 C54 117.6(9) . . ? C52 C53 C60 125.3(10) . . ? C54 C53 C60 117.0(11) . . ? N14 C54 C53 123.4(11) . . ? N14 C55 C56 118.3(9) . . ? N14 C55 C51 123.3(9) . . ? C56 C55 C51 118.4(10) . . ? N13 C56 C55 116.6(10) . . ? N13 C56 C48 121.5(9) . . ? C55 C56 C48 121.9(9) . . ? N15 C61 C62 126.1(8) . . ? C63 C62 C61 119.3(8) . . ? C63 C62 C73 121.2(9) . . ? C61 C62 C73 119.5(8) . . ? C62 C63 C64 116.6(9) . . ? C62 C63 C74 121.0(9) . . ? C64 C63 C74 122.4(9) . . ? C72 C64 C63 120.7(8) . . ? C72 C64 C65 116.3(8) . . ? C63 C64 C65 123.0(9) . . ? C66 C65 C64 121.9(9) . . ? C65 C66 C67 122.2(8) . . ? C71 C67 C68 117.9(9) . . ? C71 C67 C66 117.6(9) . . ? C68 C67 C66 124.5(8) . . ? C69 C68 C67 119.1(8) . . ? C69 C68 C75 121.5(9) . . ? C67 C68 C75 119.3(9) . . ? C68 C69 C70 118.8(9) . . ? C68 C69 C76 123.7(8) . . ? C70 C69 C76 117.6(9) . . ? N16 C70 C69 123.6(9) . . ? N16 C71 C67 123.5(8) . . ? N16 C71 C72 116.9(8) . . ? C67 C71 C72 119.7(9) . . ? N15 C72 C64 122.0(8) . . ? N15 C72 C71 115.6(8) . . ? C64 C72 C71 122.3(8) . . ? N17 C77 C78 123.8(8) . . ? C79 C78 C77 119.4(8) . . ? C79 C78 C89 123.0(9) . . ? C77 C78 C89 117.6(8) . . ? C78 C79 C80 117.8(8) . . ? C78 C79 C90 120.9(9) . . ? C80 C79 C90 121.2(9) . . ? C88 C80 C79 119.1(8) . . ? C88 C80 C81 116.1(9) . . ? C79 C80 C81 124.8(9) . . ? C82 C81 C80 121.4(9) . . ? C81 C82 C83 123.5(9) . . ? C87 C83 C82 115.9(9) . . ? C87 C83 C84 118.2(10) . . ? C82 C83 C84 125.9(9) . . ? C85 C84 C83 117.9(9) . . ? C85 C84 C91 123.4(10) . . ? C83 C84 C91 118.6(10) . . ? C86 C85 C84 118.5(10) . . ? C86 C85 C92 120.1(11) . . ? C84 C85 C92 121.4(10) . . ? N18 C86 C85 125.1(11) . . ? N18 C87 C83 123.0(9) . . ? N18 C87 C88 115.6(8) . . ? C83 C87 C88 121.4(9) . . ? N17 C88 C80 122.1(8) . . ? N17 C88 C87 116.2(8) . . ? C80 C88 C87 121.7(9) . . ? N19 C93 C94 123.4(13) . . ? C95 C94 C93 119.3(12) . . ? C95 C94 C105 122.1(14) . . ? C93 C94 C105 118.5(14) . . ? C94 C95 C96 118.5(12) . . ? C94 C95 C106 123.2(14) . . ? C96 C95 C106 118.3(15) . . ? C104 C96 C97 115.9(11) . . ? C104 C96 C95 117.9(13) . . ? C97 C96 C95 126.2(12) . . ? C98 C97 C96 122.8(11) . . ? C97 C98 C99 121.8(12) . . ? C103 C99 C98 116.9(11) . . ? C103 C99 C100 118.4(10) . . ? C98 C99 C100 124.7(11) . . ? C101 C100 C99 118.3(10) . . ? C101 C100 C107 118.8(11) . . ? C99 C100 C107 122.9(11) . . ? C102 C101 C100 118.1(10) . . ? C102 C101 C108 118.7(10) . . ? C100 C101 C108 123.2(10) . . ? N20 C102 C101 123.2(10) . . ? N20 C103 C99 123.1(9) . . ? N20 C103 C104 116.2(10) . . ? C99 C103 C104 120.6(10) . . ? N19 C104 C96 122.4(10) . . ? N19 C104 C103 115.6(10) . . ? C96 C104 C103 121.9(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.710 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.098 #end============================== data_{[Co(tmphen)2]3[Fe(CN)6]2}_130K #=================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; '{(Co(tmphen)2)3(Fe(CN)6)2}.11H2O' ; _chemical_name_common '{(Co(tmphen)2)3(Fe(CN)6)2}.11H2O' _chemical_melting_point ? _chemical_formula_moiety 'C108 H118 Co3 Fe2 N24 O11' _chemical_formula_sum 'C108 H118 Co3 Fe2 N24 O11' _chemical_formula_weight 2216.7 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.054(14) _cell_length_b 24.95(2) _cell_length_c 24.782(18) _cell_angle_alpha 90.00 _cell_angle_beta 97.688(19) _cell_angle_gamma 90.00 _cell_volume 11676(15) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 12224 _cell_measurement_theta_min 2.1615 _cell_measurement_theta_max 17.4395 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4532 _exptl_absorpt_coefficient_mu 0.724 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.7271 _exptl_absorpt_correction_T_max 0.8013 _exptl_absorpt_process_details 'SADABS: Bruker,2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER APEX' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57830 _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 20.82 _reflns_number_total 12224 _reflns_number_gt 8976 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER, 2000)' _computing_cell_refinement 'SAINT (BRUKER, 2001)' _computing_data_reduction 'SAINT (BRUKER, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1796P)^2^+20.0561P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0122(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12224 _refine_ls_number_parameters 1395 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1289 _refine_ls_R_factor_gt 0.0971 _refine_ls_wR_factor_ref 0.2881 _refine_ls_wR_factor_gt 0.2587 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.136 _refine_ls_shift/su_max 0.702 _refine_ls_shift/su_mean 0.025 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.06086(3) 0.37107(3) 0.61580(3) 0.0435(2) Uani 1 1 d . A -1 Co2 Co 0.29200(4) 0.36585(3) 0.82980(3) 0.0471(2) Uani 1 1 d . A -1 Co3 Co 0.35555(4) 0.54586(3) 0.66479(3) 0.0429(2) Uani 1 1 d . A -1 Fe1 Fe 0.32240(4) 0.35148(3) 0.63590(3) 0.0492(2) Uani 1 1 d . A -1 Fe2 Fe 0.13936(4) 0.51344(3) 0.75316(3) 0.0568(3) Uani 1 1 d . A -1 O1S O -0.0871(13) 0.0523(10) 0.4221(10) 0.132(8) Uiso 0.25 1 d P B -1 O2S O -0.2794(11) 0.1668(9) 0.5598(9) 0.110(7) Uiso 0.25 1 d P C -2 O3S O 0.0847(7) 0.0568(5) 0.4615(5) 0.137(4) Uiso 0.50 1 d P D -3 O4S O 0.0712(8) 0.0845(6) 0.4964(6) 0.165(5) Uiso 0.50 1 d P E -4 O5S O -0.237(2) 0.2201(19) 0.7168(19) 0.256(19) Uiso 0.25 1 d P F -5 O6S O 0.1367(12) 0.0677(10) 0.6495(10) 0.121(8) Uiso 0.25 1 d P G -6 O7S O -0.2193(10) 0.2328(8) 0.8048(8) 0.096(6) Uiso 0.25 1 d P H -7 O8S O 0.2825(14) 0.1157(10) 0.8067(10) 0.132(8) Uiso 0.25 1 d P I -8 O9S O 0.3058(7) 0.1785(6) 0.7634(6) 0.150(5) Uiso 0.50 1 d P J -9 O10S O -0.1379(11) 0.4519(9) 0.7643(9) 0.106(7) Uiso 0.25 1 d P K -10 O11S O -0.2210(19) 0.5539(14) 0.7582(14) 0.187(13) Uiso 0.25 1 d P L -11 O12S O 0.4200(14) 0.2142(11) 0.5476(11) 0.136(9) Uiso 0.25 1 d P M -12 O13S O 0.3161(6) 0.1906(4) 0.9111(4) 0.107(3) Uiso 0.50 1 d P N -13 O14S O 0.1141(7) 0.4803(6) 0.9219(6) 0.145(5) Uiso 0.50 1 d P O -14 O15S O -0.0670(8) 0.5810(6) 0.8647(6) 0.167(5) Uiso 0.50 1 d P P -15 O16S O 0.5079(13) 0.2917(10) 1.0813(10) 0.128(8) Uiso 0.25 1 d P Q -16 O17S O 0.7173(14) 0.4628(11) 1.0007(11) 0.139(9) Uiso 0.25 1 d P R -17 O18S O 0.7165(8) 0.3836(6) 0.7600(6) 0.167(6) Uiso 0.50 1 d P S -18 O19S O 0.6319(8) 0.3558(6) 0.6660(6) 0.156(5) Uiso 0.50 1 d P T -19 O20S O 0.6126(13) 0.4116(10) 0.6720(10) 0.125(8) Uiso 0.25 1 d P U -20 O21S O 0.2276(11) 0.7026(8) 0.7282(8) 0.098(6) Uiso 0.25 1 d P V -13 O22S O 0.2243(10) 0.8198(8) 0.5974(8) 0.098(6) Uiso 0.25 1 d P W -22 O27S O 0.3722(16) 0.7026(13) 0.3547(12) 0.165(11) Uiso 0.25 1 d P X -27 O28S O 0.2510(12) 0.7092(9) 0.3385(9) 0.110(7) Uiso 0.25 1 d P Y -28 O29S O -0.2417(6) 0.1700(5) 0.7263(5) 0.128(4) Uiso 0.50 1 d P Z -29 N1 N 0.3073(3) 0.3273(2) 0.5129(2) 0.086(2) Uani 1 1 d . A -1 N2 N 0.3236(3) 0.2292(2) 0.6543(2) 0.0772(19) Uani 1 1 d . A -1 N3 N 0.4851(3) 0.3570(2) 0.6395(3) 0.089(2) Uani 1 1 d . A -1 N4 N 0.1604(2) 0.34368(17) 0.62678(16) 0.0440(13) Uani 1 1 d . A -1 N5 N 0.3230(2) 0.36716(17) 0.75859(19) 0.0517(14) Uani 1 1 d . A -1 N6 N 0.3292(2) 0.47431(18) 0.63196(18) 0.0521(14) Uani 1 1 d . A -1 N7 N 0.0926(2) 0.44065(19) 0.65570(16) 0.0537(14) Uani 1 1 d . A -1 N8 N 0.2141(2) 0.41602(17) 0.80839(17) 0.0477(13) Uani 1 1 d . A -1 N9 N 0.2796(2) 0.54144(16) 0.71186(16) 0.0450(13) Uani 1 1 d . A -1 N10 N 0.0846(3) 0.6169(2) 0.6961(2) 0.0788(18) Uani 1 1 d . A -1 N11 N -0.0067(3) 0.4894(3) 0.7868(3) 0.136(3) Uani 1 1 d . A -1 N12 N 0.1813(4) 0.5773(2) 0.8589(2) 0.106(2) Uani 1 1 d . A -1 N13 N 0.0716(2) 0.39622(18) 0.53610(18) 0.0531(14) Uani 1 1 d . A -1 N14 N -0.0405(2) 0.4042(2) 0.5884(2) 0.0638(15) Uani 1 1 d . A -1 N15 N 0.01554(19) 0.29716(17) 0.58750(15) 0.0401(12) Uani 1 1 d . A -1 N16 N 0.0316(2) 0.33750(17) 0.68739(16) 0.0449(13) Uani 1 1 d . A -1 N17 N 0.2268(2) 0.30361(17) 0.80919(17) 0.0485(13) Uani 1 1 d . A -1 N18 N 0.2602(3) 0.3521(2) 0.90256(19) 0.0634(16) Uani 1 1 d . A -1 N19 N 0.3742(3) 0.32031(19) 0.8573(2) 0.0801(19) Uani 1 1 d . A -1 N20 N 0.3583(3) 0.42460(18) 0.85666(19) 0.0599(15) Uani 1 1 d . A -1 N21 N 0.4338(2) 0.51744(15) 0.72266(17) 0.0404(12) Uani 1 1 d . A -1 N22 N 0.3958(2) 0.61712(17) 0.70056(19) 0.0539(15) Uani 1 1 d . A -1 N23 N 0.4278(2) 0.55341(17) 0.6119(2) 0.0582(15) Uani 1 1 d . A -1 N24 N 0.2979(2) 0.59167(17) 0.60605(17) 0.0490(13) Uani 1 1 d . A -1 C1 C 0.3130(3) 0.3375(2) 0.5587(3) 0.064(2) Uani 1 1 d . A -1 C2 C 0.3244(3) 0.2747(3) 0.6479(2) 0.0593(19) Uani 1 1 d . A -1 C3 C 0.4243(3) 0.3543(2) 0.6389(3) 0.063(2) Uani 1 1 d . A -1 C4 C 0.2210(3) 0.3477(2) 0.6303(2) 0.0425(16) Uani 1 1 d . A -1 C5 C 0.3253(3) 0.36213(19) 0.7124(2) 0.0456(16) Uani 1 1 d . A -1 C6 C 0.3230(3) 0.4284(2) 0.6293(2) 0.0502(17) Uani 1 1 d . A -1 C7 C 0.1119(3) 0.4702(2) 0.6915(2) 0.0503(17) Uani 1 1 d . A -1 C8 C 0.1826(3) 0.4523(2) 0.7878(2) 0.0465(16) Uani 1 1 d . A -1 C9 C 0.2278(3) 0.5295(2) 0.7276(2) 0.0479(17) Uani 1 1 d . A -1 C10 C 0.1039(3) 0.5772(3) 0.7173(2) 0.067(2) Uani 1 1 d . A -1 C11 C 0.0481(4) 0.4987(3) 0.7746(3) 0.092(2) Uani 1 1 d . A -1 C12 C 0.1644(4) 0.5532(3) 0.8193(2) 0.079(2) Uani 1 1 d . A -1 C13 C 0.4924(3) 0.5333(2) 0.6120(3) 0.071(2) Uani 1 1 d . A -1 H13 H 0.5092 0.5118 0.6426 0.085 Uiso 1 1 calc R . . C14 C 0.5368(3) 0.5392(3) 0.5754(3) 0.082(2) Uani 1 1 d . A -1 C15 C 0.5140(3) 0.5663(3) 0.5279(3) 0.099(2) Uani 1 1 d . A -1 C16 C 0.4450(4) 0.5917(2) 0.5227(3) 0.084(2) Uani 1 1 d . A -1 C17 C 0.4157(4) 0.6242(3) 0.4797(3) 0.087(2) Uani 1 1 d . A -1 H17 H 0.4420 0.6308 0.4504 0.105 Uiso 1 1 calc R . . C18 C 0.3505(4) 0.6466(3) 0.4786(3) 0.097(3) Uani 1 1 d . A -1 H18 H 0.3328 0.6679 0.4480 0.117 Uiso 1 1 calc R . . C19 C 0.3058(3) 0.6396(3) 0.5223(2) 0.069(2) Uani 1 1 d . A -1 C20 C 0.2375(3) 0.6627(3) 0.5245(2) 0.069(2) Uani 1 1 d . A -1 C21 C 0.2019(3) 0.6483(2) 0.5676(2) 0.0616(19) Uani 1 1 d . A -1 C22 C 0.2333(3) 0.6124(2) 0.6073(2) 0.0534(18) Uani 1 1 d . A -1 H22 H 0.2077 0.6025 0.6361 0.064 Uiso 1 1 calc R . . C23 C 0.3348(3) 0.6057(2) 0.5638(2) 0.0601(18) Uani 1 1 d . A -1 C24 C 0.4048(3) 0.5826(2) 0.5672(2) 0.0634(18) Uani 1 1 d . A -1 C25 C 0.6101(3) 0.5173(3) 0.5816(4) 0.117(3) Uani 1 1 d . A -1 H25A H 0.6158 0.4946 0.5502 0.176 Uiso 1 1 calc R . . H25B H 0.6186 0.4959 0.6150 0.176 Uiso 1 1 calc R . . H25C H 0.6441 0.5469 0.5836 0.176 Uiso 1 1 calc R . . C26 C 0.5592(4) 0.5769(3) 0.4832(4) 0.154(3) Uani 1 1 d . A -1 H26A H 0.5891 0.6084 0.4927 0.230 Uiso 1 1 calc R . . H26B H 0.5286 0.5836 0.4488 0.230 Uiso 1 1 calc R . . H26C H 0.5892 0.5457 0.4791 0.230 Uiso 1 1 calc R . . C27 C 0.2024(5) 0.6993(3) 0.4802(3) 0.103(3) Uani 1 1 d . A -1 H27A H 0.1559 0.6849 0.4658 0.155 Uiso 1 1 calc R . . H27B H 0.2320 0.7017 0.4508 0.155 Uiso 1 1 calc R . . H27C H 0.1967 0.7351 0.4953 0.155 Uiso 1 1 calc R . . C28 C 0.1297(3) 0.6716(3) 0.5743(3) 0.071(2) Uani 1 1 d . A -1 H28A H 0.1115 0.6541 0.6049 0.106 Uiso 1 1 calc R . . H28B H 0.0969 0.6657 0.5409 0.106 Uiso 1 1 calc R . . H28C H 0.1344 0.7102 0.5814 0.106 Uiso 1 1 calc R . . C29 C 0.3739(3) 0.6676(2) 0.6894(3) 0.073(2) Uani 1 1 d . A -1 H29 H 0.3318 0.6729 0.6648 0.087 Uiso 1 1 calc R . . C30 C 0.4090(4) 0.7116(3) 0.7114(4) 0.103(3) Uani 1 1 d . A -1 C31 C 0.4707(4) 0.7052(2) 0.7489(3) 0.099(3) Uani 1 1 d . A -1 C32 C 0.4950(3) 0.6536(2) 0.7613(3) 0.067(2) Uani 1 1 d . A -1 C33 C 0.5568(4) 0.6409(2) 0.7957(3) 0.087(3) Uani 1 1 d . A -1 H33 H 0.5846 0.6693 0.8127 0.105 Uiso 1 1 calc R . . C34 C 0.5789(3) 0.5897(2) 0.8061(3) 0.087(2) Uani 1 1 d . A -1 H34 H 0.6219 0.5834 0.8294 0.105 Uiso 1 1 calc R . . C35 C 0.5388(3) 0.5456(2) 0.7827(3) 0.064(2) Uani 1 1 d . A -1 C36 C 0.5581(4) 0.4910(2) 0.7914(3) 0.076(2) Uani 1 1 d . A -1 C37 C 0.5117(3) 0.4520(2) 0.7689(3) 0.064(2) Uani 1 1 d . A -1 C38 C 0.4504(3) 0.4667(2) 0.7339(2) 0.0480(16) Uani 1 1 d . A -1 H38 H 0.4198 0.4394 0.7178 0.058 Uiso 1 1 calc R . . C39 C 0.4769(3) 0.5560(2) 0.7468(2) 0.0461(16) Uani 1 1 d . A -1 C40 C 0.4554(3) 0.61088(19) 0.7363(2) 0.0488(17) Uani 1 1 d . A -1 C41 C 0.3777(4) 0.7675(3) 0.6956(4) 0.148(4) Uani 1 1 d . A -1 H41A H 0.3736 0.7881 0.7287 0.222 Uiso 1 1 calc R . . H41B H 0.3308 0.7634 0.6745 0.222 Uiso 1 1 calc R . . H41C H 0.4090 0.7864 0.6737 0.222 Uiso 1 1 calc R . . C42 C 0.5117(5) 0.7526(3) 0.7720(4) 0.167(4) Uani 1 1 d . A -1 H42A H 0.4899 0.7854 0.7556 0.250 Uiso 1 1 calc R . . H42B H 0.5606 0.7501 0.7639 0.250 Uiso 1 1 calc R . . H42C H 0.5116 0.7537 0.8115 0.250 Uiso 1 1 calc R . . C43 C 0.6246(4) 0.4758(3) 0.8296(4) 0.125(3) Uani 1 1 d . A -1 H43A H 0.6189 0.4862 0.8669 0.187 Uiso 1 1 calc R . . H43B H 0.6655 0.4945 0.8184 0.187 Uiso 1 1 calc R . . H43C H 0.6321 0.4371 0.8280 0.187 Uiso 1 1 calc R . . C44 C 0.5269(4) 0.3931(2) 0.7751(3) 0.087(3) Uani 1 1 d . A -1 H44A H 0.5655 0.3836 0.7544 0.130 Uiso 1 1 calc R . . H44B H 0.4844 0.3727 0.7612 0.130 Uiso 1 1 calc R . . H44C H 0.5409 0.3847 0.8136 0.130 Uiso 1 1 calc R . . C45 C 0.1253(3) 0.3917(2) 0.5077(3) 0.064(2) Uani 1 1 d . A -1 H45 H 0.1671 0.3753 0.5254 0.076 Uiso 1 1 calc R . . C46 C 0.1267(3) 0.4090(2) 0.4531(2) 0.067(2) Uani 1 1 d . A -1 C47 C 0.0692(4) 0.4314(2) 0.4258(3) 0.071(2) Uani 1 1 d . A -1 C48 C 0.0094(3) 0.4377(2) 0.4524(2) 0.0601(19) Uani 1 1 d . A -1 C49 C -0.0546(3) 0.4624(2) 0.4283(3) 0.069(2) Uani 1 1 d . A -1 H49 H -0.0580 0.4752 0.3919 0.083 Uiso 1 1 calc R . . C50 C -0.1092(4) 0.4677(2) 0.4554(2) 0.067(2) Uani 1 1 d . A -1 H50 H -0.1501 0.4852 0.4374 0.081 Uiso 1 1 calc R . . C51 C -0.1117(3) 0.4498(2) 0.5084(3) 0.064(2) Uani 1 1 d . A -1 C52 C -0.1659(4) 0.4531(3) 0.5386(3) 0.081(2) Uani 1 1 d . A -1 C53 C -0.1632(3) 0.4332(2) 0.5904(3) 0.067(2) Uani 1 1 d . A -1 C54 C -0.0955(3) 0.4089(3) 0.6155(3) 0.086(2) Uani 1 1 d . A -1 H54 H -0.0916 0.3963 0.6519 0.103 Uiso 1 1 calc R . . C55 C -0.0467(3) 0.4239(2) 0.5371(3) 0.0621(19) Uani 1 1 d . A -1 C56 C 0.0112(3) 0.4196(2) 0.5078(3) 0.0586(19) Uani 1 1 d . A -1 C57 C 0.1935(4) 0.4001(3) 0.4279(3) 0.086(2) Uani 1 1 d . A -1 H57A H 0.2305 0.3859 0.4554 0.128 Uiso 1 1 calc R . . H57B H 0.2092 0.4342 0.4140 0.128 Uiso 1 1 calc R . . H57C H 0.1842 0.3745 0.3978 0.128 Uiso 1 1 calc R . . C58 C 0.0643(4) 0.4523(3) 0.3684(3) 0.091(3) Uani 1 1 d . A -1 H58A H 0.1095 0.4464 0.3545 0.137 Uiso 1 1 calc R . . H58B H 0.0538 0.4908 0.3681 0.137 Uiso 1 1 calc R . . H58C H 0.0266 0.4334 0.3452 0.137 Uiso 1 1 calc R . . C59 C -0.2363(3) 0.4800(3) 0.5147(3) 0.099(3) Uani 1 1 d . A -1 H59A H -0.2312 0.5190 0.5172 0.148 Uiso 1 1 calc R . . H59B H -0.2741 0.4685 0.5353 0.148 Uiso 1 1 calc R . . H59C H -0.2483 0.4696 0.4765 0.148 Uiso 1 1 calc R . . C60 C -0.2185(3) 0.4361(4) 0.6277(3) 0.113(3) Uani 1 1 d . A -1 H60A H -0.2230 0.4732 0.6398 0.170 Uiso 1 1 calc R . . H60B H -0.2048 0.4131 0.6595 0.170 Uiso 1 1 calc R . . H60C H -0.2640 0.4240 0.6084 0.170 Uiso 1 1 calc R . . C61 C 0.0088(3) 0.2764(2) 0.5380(2) 0.0459(16) Uani 1 1 d . A -1 H61 H 0.0269 0.2968 0.5106 0.055 Uiso 1 1 calc R . . C62 C -0.0222(3) 0.2276(2) 0.5227(2) 0.0489(17) Uani 1 1 d . A -1 C63 C -0.0515(3) 0.1973(2) 0.5612(2) 0.0540(18) Uani 1 1 d . A -1 C64 C -0.0462(3) 0.2189(2) 0.6148(2) 0.0484(17) Uani 1 1 d . A -1 C65 C -0.0729(3) 0.1916(3) 0.6587(2) 0.0654(19) Uani 1 1 d . A -1 H65 H -0.0954 0.1578 0.6523 0.078 Uiso 1 1 calc R . . C66 C -0.0666(3) 0.2128(3) 0.7086(2) 0.075(2) Uani 1 1 d . A -1 H66 H -0.0861 0.1938 0.7363 0.090 Uiso 1 1 calc R . . C67 C -0.0310(3) 0.2640(3) 0.7225(2) 0.0611(19) Uani 1 1 d . A -1 C68 C -0.0208(3) 0.2863(2) 0.7745(2) 0.0626(19) Uani 1 1 d . A -1 C69 C 0.0171(3) 0.3331(2) 0.7821(2) 0.0551(18) Uani 1 1 d . A -1 C70 C 0.0421(3) 0.3564(2) 0.7369(2) 0.0515(17) Uani 1 1 d . A -1 H70 H 0.0689 0.3885 0.7427 0.062 Uiso 1 1 calc R . . C71 C -0.0036(3) 0.2904(2) 0.6804(2) 0.0487(17) Uani 1 1 d . A -1 C72 C -0.0124(2) 0.2682(2) 0.62635(19) 0.0389(15) Uani 1 1 d . A -1 C73 C -0.0251(4) 0.2075(3) 0.4655(2) 0.071(2) Uani 1 1 d . A -1 H73A H 0.0030 0.1746 0.4653 0.106 Uiso 1 1 calc R . . H73B H -0.0057 0.2348 0.4432 0.106 Uiso 1 1 calc R . . H73C H -0.0743 0.2000 0.4506 0.106 Uiso 1 1 calc R . . C74 C -0.0872(3) 0.1451(2) 0.5458(2) 0.068(2) Uani 1 1 d . A -1 H74A H -0.1212 0.1500 0.5128 0.103 Uiso 1 1 calc R . . H74B H -0.1121 0.1327 0.5756 0.103 Uiso 1 1 calc R . . H74C H -0.0516 0.1185 0.5388 0.103 Uiso 1 1 calc R . . C75 C -0.0514(4) 0.2596(3) 0.8207(2) 0.087(2) Uani 1 1 d . A -1 H75A H -0.0129 0.2484 0.8486 0.130 Uiso 1 1 calc R . . H75B H -0.0790 0.2282 0.8069 0.130 Uiso 1 1 calc R . . H75C H -0.0823 0.2849 0.8365 0.130 Uiso 1 1 calc R . . C76 C 0.0321(3) 0.3604(3) 0.8366(2) 0.066(2) Uani 1 1 d . A -1 H76A H -0.0127 0.3693 0.8498 0.099 Uiso 1 1 calc R . . H76B H 0.0590 0.3933 0.8329 0.099 Uiso 1 1 calc R . . H76C H 0.0597 0.3363 0.8625 0.099 Uiso 1 1 calc R . . C77 C 0.2091(3) 0.2816(2) 0.7599(2) 0.0539(18) Uani 1 1 d . A -1 H77 H 0.2277 0.2968 0.7297 0.065 Uiso 1 1 calc R . . C78 C 0.1653(3) 0.2380(2) 0.7515(2) 0.0555(18) Uani 1 1 d . A -1 C79 C 0.1360(3) 0.2152(2) 0.7942(2) 0.0588(19) Uani 1 1 d . A -1 C80 C 0.1521(3) 0.2398(2) 0.8462(2) 0.0554(18) Uani 1 1 d . A -1 C81 C 0.1256(3) 0.2223(3) 0.8952(2) 0.073(2) Uani 1 1 d . A -1 H81 H 0.0923 0.1938 0.8928 0.088 Uiso 1 1 calc R . . C82 C 0.1461(3) 0.2448(3) 0.9439(2) 0.067(2) Uani 1 1 d . A -1 H82 H 0.1298 0.2301 0.9753 0.080 Uiso 1 1 calc R . . C83 C 0.1917(3) 0.2901(2) 0.9497(2) 0.0574(19) Uani 1 1 d . A -1 C84 C 0.2143(4) 0.3164(3) 1.0002(3) 0.083(2) Uani 1 1 d . A -1 C85 C 0.2585(4) 0.3596(3) 0.9994(3) 0.088(3) Uani 1 1 d . A -1 C86 C 0.2800(4) 0.3766(3) 0.9498(3) 0.087(3) Uani 1 1 d . A -1 H86 H 0.3101 0.4069 0.9502 0.105 Uiso 1 1 calc R . . C87 C 0.2173(3) 0.3090(2) 0.9030(2) 0.0538(18) Uani 1 1 d . A -1 C88 C 0.1974(3) 0.2835(2) 0.8519(2) 0.0462(16) Uani 1 1 d . A -1 C89 C 0.1539(3) 0.2142(3) 0.6951(2) 0.070(2) Uani 1 1 d . A -1 H89A H 0.1796 0.1801 0.6950 0.105 Uiso 1 1 calc R . . H89B H 0.1715 0.2390 0.6694 0.105 Uiso 1 1 calc R . . H89C H 0.1032 0.2078 0.6842 0.105 Uiso 1 1 calc R . . C90 C 0.0911(3) 0.1654(3) 0.7869(3) 0.083(2) Uani 1 1 d . A -1 H90A H 0.0590 0.1678 0.7527 0.125 Uiso 1 1 calc R . . H90B H 0.0634 0.1621 0.8173 0.125 Uiso 1 1 calc R . . H90C H 0.1218 0.1340 0.7861 0.125 Uiso 1 1 calc R . . C91 C 0.1884(4) 0.2969(3) 1.0520(3) 0.097(3) Uani 1 1 d . A -1 H91A H 0.2277 0.2802 1.0756 0.146 Uiso 1 1 calc R . . H91B H 0.1506 0.2705 1.0428 0.146 Uiso 1 1 calc R . . H91C H 0.1701 0.3272 1.0709 0.146 Uiso 1 1 calc R . . C92 C 0.2861(5) 0.3911(4) 1.0521(3) 0.131(4) Uani 1 1 d . A -1 H92A H 0.2949 0.3661 1.0827 0.196 Uiso 1 1 calc R . . H92B H 0.2506 0.4175 1.0595 0.196 Uiso 1 1 calc R . . H92C H 0.3302 0.4095 1.0472 0.196 Uiso 1 1 calc R . . C93 C 0.3800(5) 0.2683(3) 0.8545(3) 0.107(3) Uani 1 1 d . A -1 H93 H 0.3422 0.2483 0.8352 0.128 Uiso 1 1 calc R . . C94 C 0.4399(6) 0.2411(3) 0.8789(4) 0.145(4) Uani 1 1 d . A -1 C95 C 0.4975(6) 0.2698(3) 0.9052(4) 0.140(4) Uani 1 1 d . A -1 C96 C 0.4903(5) 0.3256(3) 0.9104(3) 0.117(3) Uani 1 1 d . A -1 C97 C 0.5446(5) 0.3614(3) 0.9367(4) 0.132(4) Uani 1 1 d . A -1 H97 H 0.5875 0.3466 0.9543 0.159 Uiso 1 1 calc R . . C98 C 0.5357(4) 0.4155(4) 0.9367(4) 0.127(3) Uani 1 1 d . A -1 H98 H 0.5714 0.4372 0.9561 0.152 Uiso 1 1 calc R . . C99 C 0.4731(4) 0.4407(3) 0.9080(3) 0.084(2) Uani 1 1 d . A -1 C100 C 0.4607(4) 0.4961(3) 0.9051(3) 0.078(2) Uani 1 1 d . A -1 C101 C 0.3989(4) 0.5145(2) 0.8742(3) 0.069(2) Uani 1 1 d . A -1 C102 C 0.3485(3) 0.4773(2) 0.8518(2) 0.064(2) Uani 1 1 d . A -1 H102 H 0.3055 0.4902 0.8323 0.077 Uiso 1 1 calc R . . C103 C 0.4203(4) 0.4065(3) 0.8829(3) 0.076(2) Uani 1 1 d . A -1 C104 C 0.4283(4) 0.3489(3) 0.8831(3) 0.081(2) Uani 1 1 d . A -1 C105 C 0.4432(7) 0.1791(3) 0.8779(5) 0.218(7) Uani 1 1 d . A -1 H10G H 0.4833 0.1667 0.9039 0.327 Uiso 1 1 calc R . . H10H H 0.4493 0.1669 0.8413 0.327 Uiso 1 1 calc R . . H10I H 0.3991 0.1643 0.8881 0.327 Uiso 1 1 calc R . . C106 C 0.5662(6) 0.2427(4) 0.9374(5) 0.212(5) Uani 1 1 d . A -1 H10J H 0.6001 0.2706 0.9512 0.319 Uiso 1 1 calc R . . H10K H 0.5879 0.2189 0.9129 0.319 Uiso 1 1 calc R . . H10L H 0.5529 0.2219 0.9681 0.319 Uiso 1 1 calc R . . C107 C 0.5137(5) 0.5349(3) 0.9337(4) 0.121(4) Uani 1 1 d . A -1 H10D H 0.5524 0.5150 0.9547 0.181 Uiso 1 1 calc R . . H10E H 0.4904 0.5576 0.9582 0.181 Uiso 1 1 calc R . . H10F H 0.5327 0.5574 0.9066 0.181 Uiso 1 1 calc R . . C108 C 0.3812(4) 0.5733(2) 0.8669(3) 0.084(2) Uani 1 1 d . A -1 H10A H 0.3756 0.5892 0.9023 0.127 Uiso 1 1 calc R . . H10B H 0.3369 0.5773 0.8421 0.127 Uiso 1 1 calc R . . H10C H 0.4195 0.5917 0.8516 0.127 Uiso 1 1 calc R . . O30S O 0.5547(13) 0.2967(10) 1.0818(9) 0.117(8) Uiso 0.25 1 d P A -30 O31S O 0.4799(11) 0.2914(8) 1.0527(8) 0.086(6) Uiso 0.25 1 d P B -31 O37S O 0.6744(7) 0.4847(5) 1.0058(5) 0.136(4) Uiso 0.50 1 d P C -37 O35S O 0.2729(13) 0.0767(11) 0.7952(10) 0.130(8) Uiso 0.25 1 d P D -35 O32S O 0.5185(14) 0.3219(11) 1.0485(11) 0.133(8) Uiso 0.25 1 d P E -32 O36S O 0.7182(15) 0.4778(11) 1.0273(11) 0.131(9) Uiso 0.25 1 d P F -36 O33S O 0.0238(15) 0.0302(11) 0.4249(11) 0.145(9) Uiso 0.25 1 d P G -33 O38S O 0.4332(9) 0.2491(7) 0.5408(7) 0.073(5) Uiso 0.25 1 d P H -38 O34S O 0.2013(13) 0.0651(10) 0.6699(10) 0.128(8) Uiso 0.25 1 d P I -34 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0286(3) 0.0667(5) 0.0347(4) 0.0056(4) 0.0024(3) 0.0025(3) Co2 0.0568(4) 0.0402(4) 0.0424(4) 0.0083(3) -0.0007(4) -0.0039(4) Co3 0.0447(4) 0.0331(4) 0.0529(4) 0.0050(3) 0.0137(3) 0.0029(3) Fe1 0.0403(4) 0.0513(5) 0.0555(5) 0.0125(4) 0.0051(4) 0.0057(4) Fe2 0.0670(5) 0.0654(5) 0.0410(4) 0.0102(4) 0.0183(4) 0.0277(4) N1 0.093(4) 0.101(4) 0.064(3) 0.018(3) 0.010(3) -0.001(3) N2 0.060(3) 0.051(3) 0.115(4) 0.024(3) -0.008(3) 0.010(3) N3 0.048(3) 0.092(4) 0.130(5) -0.014(4) 0.018(3) 0.004(3) N4 0.042(2) 0.053(3) 0.035(2) 0.010(2) -0.002(2) 0.001(2) N5 0.049(3) 0.045(3) 0.056(3) 0.006(2) -0.009(2) -0.010(2) N6 0.050(2) 0.054(3) 0.056(3) 0.012(2) 0.023(2) 0.003(2) N7 0.036(2) 0.089(3) 0.038(2) 0.030(2) 0.010(2) 0.013(2) N8 0.045(2) 0.052(3) 0.044(3) 0.006(2) 0.001(2) -0.009(2) N9 0.064(3) 0.031(2) 0.038(2) -0.003(2) 0.001(2) 0.006(2) N10 0.108(4) 0.076(3) 0.054(3) -0.004(3) 0.017(3) 0.044(3) N11 0.108(4) 0.187(7) 0.132(5) 0.043(5) 0.081(4) 0.061(4) N12 0.191(6) 0.077(4) 0.054(3) -0.001(3) 0.030(4) 0.039(4) N13 0.028(2) 0.061(3) 0.066(3) 0.008(2) -0.010(2) 0.006(2) N14 0.034(2) 0.078(3) 0.083(3) -0.035(3) 0.021(2) -0.009(2) N15 0.032(2) 0.061(3) 0.030(2) 0.006(2) 0.0144(18) 0.003(2) N16 0.040(2) 0.064(3) 0.030(2) -0.001(2) 0.0029(19) -0.020(2) N17 0.050(2) 0.053(3) 0.041(3) -0.001(2) 0.001(2) -0.009(2) N18 0.072(3) 0.068(3) 0.048(3) -0.005(3) 0.001(3) -0.016(3) N19 0.123(4) 0.041(3) 0.071(3) 0.009(3) -0.005(3) 0.016(3) N20 0.075(3) 0.040(3) 0.066(3) 0.006(2) 0.015(3) 0.010(2) N21 0.040(2) 0.027(2) 0.055(3) -0.006(2) 0.010(2) -0.0052(19) N22 0.042(2) 0.046(3) 0.072(3) 0.005(2) -0.001(2) -0.002(2) N23 0.050(2) 0.040(3) 0.091(3) 0.005(2) 0.034(2) -0.001(2) N24 0.047(2) 0.051(3) 0.050(3) -0.007(2) 0.010(2) -0.009(2) C1 0.057(3) 0.068(4) 0.067(4) 0.024(3) 0.004(3) 0.008(3) C2 0.031(3) 0.081(4) 0.064(4) 0.011(3) 0.000(3) 0.014(3) C3 0.054(4) 0.059(4) 0.076(4) 0.002(3) 0.005(3) 0.004(3) C4 0.044(3) 0.046(3) 0.036(3) 0.011(2) -0.001(2) -0.002(3) C5 0.033(3) 0.034(3) 0.067(4) 0.014(3) -0.004(3) -0.003(2) C6 0.040(3) 0.063(4) 0.051(3) 0.021(3) 0.018(3) 0.009(3) C7 0.033(3) 0.079(4) 0.040(3) 0.023(3) 0.013(2) 0.023(3) C8 0.048(3) 0.055(3) 0.038(3) 0.000(3) 0.010(3) 0.001(3) C9 0.066(3) 0.039(3) 0.037(3) 0.003(3) 0.000(3) 0.010(3) C10 0.087(4) 0.069(4) 0.048(3) 0.009(3) 0.020(3) 0.035(3) C11 0.088(4) 0.123(6) 0.071(4) 0.027(4) 0.037(4) 0.056(4) C12 0.123(5) 0.072(4) 0.047(4) 0.010(3) 0.027(4) 0.050(4) C13 0.052(3) 0.051(4) 0.115(5) -0.014(4) 0.036(3) -0.011(3) C14 0.075(4) 0.062(4) 0.120(5) -0.004(4) 0.056(4) -0.012(3) C15 0.076(3) 0.091(4) 0.151(5) -0.063(4) 0.091(3) -0.045(3) C16 0.123(5) 0.057(4) 0.084(4) -0.016(3) 0.052(4) -0.047(4) C17 0.100(5) 0.083(5) 0.090(5) -0.025(4) 0.054(4) -0.023(4) C18 0.154(6) 0.090(5) 0.049(4) 0.005(4) 0.016(4) -0.057(5) C19 0.089(4) 0.074(4) 0.047(4) -0.001(3) 0.019(3) -0.032(3) C20 0.080(4) 0.070(4) 0.055(4) 0.001(3) 0.006(3) -0.013(4) C21 0.065(4) 0.072(4) 0.045(3) -0.011(3) -0.002(3) -0.020(3) C22 0.049(3) 0.065(4) 0.045(3) -0.012(3) 0.001(3) -0.013(3) C23 0.071(4) 0.055(3) 0.059(4) -0.009(3) 0.027(3) -0.025(3) C24 0.056(3) 0.063(4) 0.081(4) -0.029(3) 0.046(3) -0.023(3) C25 0.069(4) 0.090(5) 0.211(8) -0.044(5) 0.084(4) -0.004(4) C26 0.174(5) 0.116(6) 0.208(6) -0.067(5) 0.163(5) -0.058(5) C27 0.145(7) 0.103(6) 0.060(4) 0.016(4) 0.005(5) 0.002(5) C28 0.066(4) 0.077(4) 0.067(4) 0.004(4) -0.002(3) 0.007(4) C29 0.057(4) 0.038(3) 0.113(5) 0.005(4) -0.029(4) 0.005(3) C30 0.082(5) 0.038(4) 0.172(7) -0.002(4) -0.045(5) -0.008(3) C31 0.081(4) 0.038(4) 0.157(7) 0.008(4) -0.056(5) -0.021(3) C32 0.061(4) 0.026(3) 0.104(5) 0.002(3) -0.024(4) -0.003(3) C33 0.079(4) 0.034(3) 0.132(6) 0.003(4) -0.044(4) -0.012(3) C34 0.074(4) 0.040(4) 0.129(6) 0.004(4) -0.054(4) -0.012(3) C35 0.056(4) 0.053(4) 0.078(4) 0.003(3) -0.009(3) 0.000(3) C36 0.079(4) 0.038(3) 0.102(5) 0.009(3) -0.023(4) 0.010(3) C37 0.061(4) 0.040(3) 0.083(4) -0.005(3) -0.016(3) 0.006(3) C38 0.046(3) 0.037(3) 0.060(3) 0.002(3) 0.007(3) -0.003(3) C39 0.040(3) 0.045(3) 0.053(3) -0.001(3) 0.008(3) 0.001(3) C40 0.048(3) 0.027(3) 0.067(4) 0.005(3) -0.003(3) -0.002(3) C41 0.114(6) 0.040(4) 0.258(10) 0.016(5) -0.097(6) 0.009(4) C42 0.166(7) 0.032(4) 0.257(10) 0.007(5) -0.138(6) -0.020(4) C43 0.087(5) 0.056(4) 0.201(8) 0.007(5) -0.090(5) 0.005(4) C44 0.095(5) 0.028(3) 0.125(6) 0.015(4) -0.029(4) 0.003(3) C45 0.044(3) 0.065(4) 0.078(4) 0.005(3) -0.005(3) 0.006(3) C46 0.085(4) 0.050(3) 0.058(4) 0.018(3) -0.018(3) -0.007(3) C47 0.082(4) 0.051(4) 0.075(4) 0.010(3) -0.005(4) 0.001(3) C48 0.071(4) 0.045(3) 0.052(3) 0.010(3) -0.037(3) -0.006(3) C49 0.075(4) 0.051(4) 0.073(4) -0.006(3) -0.021(4) 0.004(3) C50 0.081(4) 0.054(4) 0.060(4) -0.003(3) -0.017(3) -0.011(3) C51 0.035(3) 0.054(4) 0.104(5) -0.033(3) 0.007(3) -0.001(3) C52 0.078(4) 0.091(5) 0.074(4) -0.019(4) 0.014(4) -0.006(4) C53 0.031(3) 0.062(4) 0.114(5) -0.025(4) 0.031(3) 0.001(3) C54 0.058(4) 0.102(5) 0.101(5) -0.030(4) 0.021(4) -0.021(4) C55 0.046(3) 0.066(4) 0.070(4) -0.022(3) -0.009(3) -0.004(3) C56 0.040(3) 0.043(3) 0.091(4) -0.011(3) -0.002(3) 0.000(3) C57 0.098(5) 0.089(5) 0.073(4) 0.023(4) 0.028(4) -0.011(4) C58 0.142(6) 0.064(4) 0.059(4) 0.019(4) -0.020(4) 0.014(4) C59 0.052(4) 0.099(5) 0.134(6) -0.031(5) -0.027(4) 0.024(4) C60 0.048(4) 0.144(7) 0.153(7) -0.032(6) 0.028(4) 0.011(4) C61 0.047(3) 0.054(3) 0.038(3) 0.012(3) 0.013(2) 0.014(3) C62 0.050(3) 0.065(4) 0.031(3) 0.005(3) 0.003(3) 0.006(3) C63 0.048(3) 0.070(4) 0.043(3) -0.002(3) 0.004(3) -0.003(3) C64 0.048(3) 0.067(4) 0.030(3) -0.005(3) 0.002(2) -0.013(3) C65 0.083(4) 0.078(4) 0.034(3) -0.005(3) 0.004(3) -0.043(3) C66 0.088(4) 0.097(5) 0.043(3) -0.002(3) 0.018(3) -0.055(4) C67 0.069(3) 0.090(4) 0.026(3) 0.000(3) 0.015(3) -0.040(3) C68 0.070(4) 0.078(4) 0.039(3) 0.005(3) 0.004(3) -0.029(3) C69 0.064(3) 0.076(4) 0.025(3) -0.001(3) 0.006(3) -0.025(3) C70 0.057(3) 0.068(4) 0.027(3) 0.002(3) -0.002(3) -0.024(3) C71 0.050(3) 0.060(4) 0.036(3) -0.001(3) 0.006(3) -0.011(3) C72 0.033(3) 0.055(3) 0.028(3) 0.002(3) 0.004(2) -0.003(3) C73 0.095(4) 0.074(4) 0.046(4) -0.008(3) 0.017(3) -0.005(4) C74 0.076(4) 0.073(4) 0.055(4) -0.008(3) 0.006(3) -0.023(3) C75 0.110(5) 0.118(5) 0.036(3) -0.003(3) 0.022(3) -0.064(4) C76 0.073(4) 0.082(4) 0.044(3) -0.007(3) 0.009(3) -0.027(3) C77 0.049(3) 0.071(4) 0.039(3) 0.005(3) -0.005(3) -0.022(3) C78 0.061(3) 0.060(4) 0.044(3) 0.001(3) -0.002(3) -0.017(3) C79 0.060(3) 0.064(4) 0.050(3) 0.005(3) -0.001(3) -0.014(3) C80 0.052(3) 0.068(4) 0.048(3) 0.015(3) 0.014(3) -0.007(3) C81 0.066(4) 0.090(5) 0.063(4) 0.010(4) 0.007(3) -0.020(4) C82 0.066(4) 0.090(4) 0.044(3) 0.011(3) 0.010(3) -0.027(3) C83 0.059(3) 0.075(4) 0.036(3) 0.008(3) -0.004(3) -0.009(3) C84 0.078(4) 0.119(6) 0.050(4) 0.001(4) 0.006(3) -0.027(4) C85 0.091(5) 0.128(6) 0.045(4) -0.017(4) 0.004(4) -0.039(4) C86 0.087(5) 0.100(5) 0.073(5) -0.018(4) 0.001(4) -0.028(4) C87 0.053(3) 0.069(4) 0.037(3) 0.006(3) -0.001(3) -0.011(3) C88 0.048(3) 0.055(3) 0.034(3) 0.008(3) 0.002(3) -0.011(3) C89 0.055(3) 0.091(5) 0.061(4) -0.004(4) -0.001(3) -0.027(3) C90 0.083(4) 0.092(5) 0.075(4) -0.002(4) 0.011(4) -0.043(4) C91 0.090(5) 0.150(7) 0.053(4) 0.000(4) 0.015(4) -0.028(5) C92 0.135(7) 0.185(8) 0.074(5) -0.045(5) 0.022(5) -0.070(6) C93 0.139(7) 0.042(4) 0.128(6) 0.021(4) -0.018(6) 0.014(4) C94 0.193(9) 0.069(5) 0.152(8) -0.013(6) -0.052(7) 0.011(6) C95 0.208(9) 0.073(5) 0.123(7) 0.011(5) -0.040(7) 0.073(5) C96 0.166(7) 0.070(5) 0.100(6) -0.002(4) -0.032(6) 0.048(5) C97 0.127(7) 0.091(6) 0.160(8) -0.017(6) -0.050(6) 0.042(5) C98 0.109(6) 0.109(6) 0.139(7) -0.024(6) -0.069(5) 0.013(5) C99 0.100(5) 0.056(4) 0.091(5) -0.014(4) -0.008(4) 0.009(4) C100 0.079(4) 0.073(4) 0.079(5) -0.011(4) 0.000(4) 0.006(4) C101 0.092(4) 0.044(3) 0.075(4) -0.003(3) 0.028(4) 0.002(3) C102 0.084(4) 0.043(3) 0.072(4) 0.005(3) 0.029(3) 0.004(3) C103 0.098(5) 0.062(4) 0.067(4) 0.005(3) 0.007(4) 0.013(4) C104 0.094(5) 0.059(4) 0.086(5) 0.010(4) -0.004(4) 0.031(4) C105 0.315(14) 0.031(4) 0.273(14) 0.010(6) -0.091(12) 0.051(7) C106 0.267(10) 0.111(6) 0.219(11) 0.003(7) -0.113(9) 0.111(7) C107 0.115(6) 0.084(5) 0.155(8) -0.029(6) -0.017(6) -0.015(5) C108 0.092(5) 0.046(4) 0.119(6) -0.003(4) 0.032(4) -0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N4 2.001(4) . ? Co1 N7 2.048(5) . ? Co1 N16 2.103(4) . ? Co1 N13 2.108(5) . ? Co1 N15 2.116(4) . ? Co1 N14 2.127(4) . ? Co2 N5 1.935(5) . ? Co2 N8 1.960(4) . ? Co2 N19 1.981(5) . ? Co2 N20 1.990(5) . ? Co2 N18 2.007(5) . ? Co2 N17 2.012(4) . ? Co3 N9 1.980(5) . ? Co3 N6 1.998(5) . ? Co3 N23 2.033(5) . ? Co3 N21 2.052(4) . ? Co3 N24 2.051(4) . ? Co3 N22 2.086(5) . ? Fe1 C5 1.907(6) . ? Fe1 C4 1.920(5) . ? Fe1 C1 1.929(7) . ? Fe1 C6 1.927(6) . ? Fe1 C2 1.937(7) . ? Fe1 C3 1.934(6) . ? Fe2 C8 1.886(5) . ? Fe2 C7 1.885(6) . ? Fe2 C10 1.902(6) . ? Fe2 C12 1.921(6) . ? Fe2 C11 1.921(7) . ? Fe2 C9 1.920(6) . ? N1 C1 1.155(8) . ? N2 C2 1.149(8) . ? N3 C3 1.159(8) . ? N4 C4 1.150(6) . ? N5 C5 1.159(7) . ? N6 C6 1.152(7) . ? N7 C7 1.176(7) . ? N8 C8 1.164(7) . ? N9 C9 1.148(7) . ? N10 C10 1.159(8) . ? N11 C11 1.149(9) . ? N12 C12 1.160(8) . ? N13 C45 1.323(8) . ? N13 C56 1.394(7) . ? N14 C54 1.323(8) . ? N14 C55 1.355(8) . ? N15 C61 1.320(6) . ? N15 C72 1.368(6) . ? N16 C70 1.304(6) . ? N16 C71 1.354(7) . ? N17 C77 1.340(7) . ? N17 C88 1.358(7) . ? N18 C86 1.329(8) . ? N18 C87 1.352(7) . ? N19 C93 1.306(8) . ? N19 C104 1.343(9) . ? N20 C102 1.332(7) . ? N20 C103 1.348(8) . ? N21 C38 1.325(6) . ? N21 C39 1.352(6) . ? N22 C29 1.344(7) . ? N22 C40 1.354(7) . ? N23 C13 1.327(7) . ? N23 C24 1.348(7) . ? N24 C22 1.339(7) . ? N24 C23 1.382(7) . ? C13 C14 1.330(9) . ? C14 C15 1.378(10) . ? C14 C25 1.487(9) . ? C15 C16 1.449(9) . ? C15 C26 1.516(11) . ? C16 C17 1.397(10) . ? C16 C24 1.441(9) . ? C17 C18 1.358(11) . ? C18 C19 1.476(10) . ? C19 C23 1.387(8) . ? C19 C20 1.430(9) . ? C20 C21 1.387(9) . ? C20 C27 1.513(9) . ? C21 C22 1.403(8) . ? C21 C28 1.523(9) . ? C23 C24 1.447(8) . ? C29 C30 1.361(9) . ? C30 C31 1.408(10) . ? C30 C41 1.545(9) . ? C31 C32 1.388(8) . ? C31 C42 1.489(9) . ? C32 C33 1.395(9) . ? C32 C40 1.400(7) . ? C33 C34 1.358(8) . ? C34 C35 1.419(8) . ? C35 C39 1.403(8) . ? C35 C36 1.421(8) . ? C36 C37 1.381(8) . ? C36 C43 1.523(9) . ? C37 C38 1.408(8) . ? C37 C44 1.500(8) . ? C39 C40 1.442(7) . ? C45 C46 1.422(9) . ? C46 C47 1.331(9) . ? C46 C57 1.508(10) . ? C47 C48 1.401(9) . ? C47 C58 1.505(9) . ? C48 C49 1.425(8) . ? C48 C56 1.440(8) . ? C49 C50 1.319(9) . ? C50 C51 1.393(9) . ? C51 C52 1.355(9) . ? C51 C55 1.491(8) . ? C52 C53 1.372(10) . ? C52 C59 1.545(9) . ? C53 C54 1.483(9) . ? C53 C60 1.494(10) . ? C55 C56 1.403(9) . ? C61 C62 1.387(8) . ? C62 C63 1.391(8) . ? C62 C73 1.496(8) . ? C63 C64 1.424(7) . ? C63 C74 1.494(8) . ? C64 C72 1.399(7) . ? C64 C65 1.435(8) . ? C65 C66 1.334(8) . ? C66 C67 1.466(9) . ? C67 C68 1.393(8) . ? C67 C71 1.394(8) . ? C68 C69 1.373(8) . ? C68 C75 1.506(8) . ? C69 C70 1.401(8) . ? C69 C76 1.506(8) . ? C71 C72 1.438(7) . ? C77 C78 1.371(8) . ? C78 C79 1.384(8) . ? C78 C89 1.507(8) . ? C79 C80 1.422(8) . ? C79 C90 1.505(9) . ? C80 C88 1.386(8) . ? C80 C81 1.443(8) . ? C81 C82 1.341(8) . ? C82 C83 1.422(8) . ? C83 C87 1.395(8) . ? C83 C84 1.429(8) . ? C84 C85 1.370(10) . ? C84 C91 1.515(9) . ? C85 C86 1.410(10) . ? C85 C92 1.555(10) . ? C87 C88 1.423(7) . ? C93 C94 1.394(12) . ? C94 C95 1.396(13) . ? C94 C105 1.551(11) . ? C95 C96 1.406(11) . ? C95 C106 1.590(13) . ? C96 C104 1.407(10) . ? C96 C97 1.453(12) . ? C97 C98 1.360(12) . ? C98 C99 1.449(10) . ? C99 C103 1.401(10) . ? C99 C100 1.400(9) . ? C100 C101 1.394(9) . ? C100 C107 1.506(10) . ? C101 C102 1.395(8) . ? C101 C108 1.512(9) . ? C103 C104 1.444(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N7 90.62(17) . . ? N4 Co1 N16 95.88(16) . . ? N7 Co1 N16 91.42(17) . . ? N4 Co1 N13 91.13(16) . . ? N7 Co1 N13 98.08(18) . . ? N16 Co1 N13 168.14(16) . . ? N4 Co1 N15 94.87(16) . . ? N7 Co1 N15 168.41(16) . . ? N16 Co1 N15 77.89(16) . . ? N13 Co1 N15 92.02(16) . . ? N4 Co1 N14 168.62(18) . . ? N7 Co1 N14 91.21(18) . . ? N16 Co1 N14 95.30(18) . . ? N13 Co1 N14 77.49(18) . . ? N15 Co1 N14 85.42(17) . . ? N5 Co2 N8 93.14(18) . . ? N5 Co2 N19 90.0(2) . . ? N8 Co2 N19 174.2(2) . . ? N5 Co2 N20 92.01(19) . . ? N8 Co2 N20 92.51(19) . . ? N19 Co2 N20 82.5(2) . . ? N5 Co2 N18 171.15(19) . . ? N8 Co2 N18 92.48(19) . . ? N19 Co2 N18 85.0(2) . . ? N20 Co2 N18 94.6(2) . . ? N5 Co2 N17 92.02(18) . . ? N8 Co2 N17 90.26(18) . . ? N19 Co2 N17 94.5(2) . . ? N20 Co2 N17 174.98(18) . . ? N18 Co2 N17 81.13(19) . . ? N9 Co3 N6 91.52(17) . . ? N9 Co3 N23 175.34(17) . . ? N6 Co3 N23 88.57(18) . . ? N9 Co3 N21 95.11(17) . . ? N6 Co3 N21 95.47(17) . . ? N23 Co3 N21 89.52(18) . . ? N9 Co3 N24 94.85(18) . . ? N6 Co3 N24 97.32(18) . . ? N23 Co3 N24 80.52(18) . . ? N21 Co3 N24 163.55(16) . . ? N9 Co3 N22 93.04(18) . . ? N6 Co3 N22 173.00(17) . . ? N23 Co3 N22 87.32(18) . . ? N21 Co3 N22 78.84(17) . . ? N24 Co3 N22 87.59(18) . . ? C5 Fe1 C4 88.5(2) . . ? C5 Fe1 C1 175.6(2) . . ? C4 Fe1 C1 87.7(2) . . ? C5 Fe1 C6 86.9(2) . . ? C4 Fe1 C6 93.4(2) . . ? C1 Fe1 C6 95.6(2) . . ? C5 Fe1 C2 89.3(2) . . ? C4 Fe1 C2 87.8(2) . . ? C1 Fe1 C2 88.4(3) . . ? C6 Fe1 C2 175.9(2) . . ? C5 Fe1 C3 93.5(2) . . ? C4 Fe1 C3 177.9(2) . . ? C1 Fe1 C3 90.2(3) . . ? C6 Fe1 C3 87.1(2) . . ? C2 Fe1 C3 91.8(2) . . ? C8 Fe2 C7 87.9(2) . . ? C8 Fe2 C10 174.9(3) . . ? C7 Fe2 C10 93.2(3) . . ? C8 Fe2 C12 89.1(2) . . ? C7 Fe2 C12 175.5(3) . . ? C10 Fe2 C12 90.0(3) . . ? C8 Fe2 C11 94.4(3) . . ? C7 Fe2 C11 87.3(3) . . ? C10 Fe2 C11 90.6(3) . . ? C12 Fe2 C11 89.6(3) . . ? C8 Fe2 C9 88.3(2) . . ? C7 Fe2 C9 90.7(2) . . ? C10 Fe2 C9 86.8(3) . . ? C12 Fe2 C9 92.6(3) . . ? C11 Fe2 C9 176.6(3) . . ? C4 N4 Co1 154.7(4) . . ? C5 N5 Co2 163.0(4) . . ? C6 N6 Co3 158.4(4) . . ? C7 N7 Co1 159.9(4) . . ? C8 N8 Co2 160.4(4) . . ? C9 N9 Co3 160.7(4) . . ? C45 N13 C56 114.4(5) . . ? C45 N13 Co1 130.8(4) . . ? C56 N13 Co1 114.8(4) . . ? C54 N14 C55 117.9(5) . . ? C54 N14 Co1 128.4(5) . . ? C55 N14 Co1 113.7(4) . . ? C61 N15 C72 116.6(4) . . ? C61 N15 Co1 129.3(3) . . ? C72 N15 Co1 114.1(3) . . ? C70 N16 C71 116.5(4) . . ? C70 N16 Co1 128.6(4) . . ? C71 N16 Co1 114.9(3) . . ? C77 N17 C88 118.6(5) . . ? C77 N17 Co2 128.3(4) . . ? C88 N17 Co2 113.1(3) . . ? C86 N18 C87 117.3(5) . . ? C86 N18 Co2 129.0(5) . . ? C87 N18 Co2 113.5(4) . . ? C93 N19 C104 119.3(6) . . ? C93 N19 Co2 128.3(5) . . ? C104 N19 Co2 112.3(4) . . ? C102 N20 C103 118.5(5) . . ? C102 N20 Co2 128.5(4) . . ? C103 N20 Co2 112.9(4) . . ? C38 N21 C39 118.3(4) . . ? C38 N21 Co3 127.4(3) . . ? C39 N21 Co3 113.9(3) . . ? C29 N22 C40 116.9(5) . . ? C29 N22 Co3 128.7(4) . . ? C40 N22 Co3 114.1(3) . . ? C13 N23 C24 113.9(5) . . ? C13 N23 Co3 132.1(4) . . ? C24 N23 Co3 114.0(4) . . ? C22 N24 C23 118.8(5) . . ? C22 N24 Co3 127.3(4) . . ? C23 N24 Co3 113.6(3) . . ? N1 C1 Fe1 177.6(6) . . ? N2 C2 Fe1 178.0(5) . . ? N3 C3 Fe1 178.2(6) . . ? N4 C4 Fe1 177.8(5) . . ? N5 C5 Fe1 175.8(5) . . ? N6 C6 Fe1 170.8(5) . . ? N7 C7 Fe2 174.9(5) . . ? N8 C8 Fe2 174.9(5) . . ? N9 C9 Fe2 176.9(5) . . ? N10 C10 Fe2 177.4(6) . . ? N11 C11 Fe2 178.9(8) . . ? N12 C12 Fe2 178.2(7) . . ? N23 C13 C14 129.1(6) . . ? C13 C14 C15 118.7(6) . . ? C13 C14 C25 124.4(7) . . ? C15 C14 C25 117.0(7) . . ? C14 C15 C16 118.0(6) . . ? C14 C15 C26 124.4(6) . . ? C16 C15 C26 117.2(7) . . ? C17 C16 C24 118.4(6) . . ? C17 C16 C15 125.9(7) . . ? C24 C16 C15 115.6(6) . . ? C18 C17 C16 121.7(7) . . ? C17 C18 C19 123.5(6) . . ? C23 C19 C20 119.4(6) . . ? C23 C19 C18 113.9(6) . . ? C20 C19 C18 126.7(6) . . ? C21 C20 C19 117.8(6) . . ? C21 C20 C27 120.0(6) . . ? C19 C20 C27 122.1(6) . . ? C20 C21 C22 119.9(6) . . ? C20 C21 C28 121.8(5) . . ? C22 C21 C28 118.3(5) . . ? N24 C22 C21 122.5(5) . . ? N24 C23 C19 121.6(5) . . ? N24 C23 C24 114.4(5) . . ? C19 C23 C24 124.0(6) . . ? N23 C24 C16 124.4(5) . . ? N23 C24 C23 117.3(5) . . ? C16 C24 C23 118.2(6) . . ? N22 C29 C30 123.5(6) . . ? C29 C30 C31 119.6(6) . . ? C29 C30 C41 118.3(6) . . ? C31 C30 C41 122.0(6) . . ? C32 C31 C30 118.4(6) . . ? C32 C31 C42 120.8(6) . . ? C30 C31 C42 120.7(6) . . ? C31 C32 C33 125.0(5) . . ? C31 C32 C40 117.7(5) . . ? C33 C32 C40 117.3(5) . . ? C34 C33 C32 122.9(6) . . ? C33 C34 C35 121.0(6) . . ? C39 C35 C36 116.9(5) . . ? C39 C35 C34 118.5(5) . . ? C36 C35 C34 124.6(5) . . ? C37 C36 C35 118.4(6) . . ? C37 C36 C43 120.7(5) . . ? C35 C36 C43 120.6(6) . . ? C36 C37 C38 119.9(5) . . ? C36 C37 C44 122.9(5) . . ? C38 C37 C44 116.9(5) . . ? N21 C38 C37 122.3(5) . . ? N21 C39 C35 123.9(5) . . ? N21 C39 C40 117.1(4) . . ? C35 C39 C40 118.9(5) . . ? N22 C40 C32 123.8(5) . . ? N22 C40 C39 114.8(4) . . ? C32 C40 C39 121.3(5) . . ? N13 C45 C46 126.5(5) . . ? C47 C46 C45 119.6(6) . . ? C47 C46 C57 122.2(6) . . ? C45 C46 C57 118.3(5) . . ? C46 C47 C48 118.2(6) . . ? C46 C47 C58 124.8(7) . . ? C48 C47 C58 117.1(6) . . ? C47 C48 C49 123.7(6) . . ? C47 C48 C56 119.8(5) . . ? C49 C48 C56 116.4(6) . . ? C50 C49 C48 121.2(6) . . ? C49 C50 C51 125.3(6) . . ? C52 C51 C50 128.7(6) . . ? C52 C51 C55 114.1(6) . . ? C50 C51 C55 117.1(6) . . ? C51 C52 C53 124.0(6) . . ? C51 C52 C59 120.1(6) . . ? C53 C52 C59 115.9(6) . . ? C52 C53 C54 117.5(6) . . ? C52 C53 C60 128.4(6) . . ? C54 C53 C60 114.0(6) . . ? N14 C54 C53 121.9(7) . . ? N14 C55 C56 118.9(5) . . ? N14 C55 C51 124.5(5) . . ? C56 C55 C51 116.6(6) . . ? N13 C56 C55 115.1(5) . . ? N13 C56 C48 121.6(5) . . ? C55 C56 C48 123.3(5) . . ? N15 C61 C62 125.7(5) . . ? C61 C62 C63 119.0(5) . . ? C61 C62 C73 120.9(5) . . ? C63 C62 C73 120.1(5) . . ? C62 C63 C64 116.7(5) . . ? C62 C63 C74 120.5(5) . . ? C64 C63 C74 122.8(5) . . ? C72 C64 C63 119.8(5) . . ? C72 C64 C65 117.5(5) . . ? C63 C64 C65 122.6(5) . . ? C66 C65 C64 121.1(6) . . ? C65 C66 C67 123.0(6) . . ? C68 C67 C71 119.0(5) . . ? C68 C67 C66 124.7(5) . . ? C71 C67 C66 116.3(5) . . ? C69 C68 C67 118.1(5) . . ? C69 C68 C75 121.5(5) . . ? C67 C68 C75 120.3(5) . . ? C68 C69 C70 118.2(5) . . ? C68 C69 C76 122.7(5) . . ? C70 C69 C76 119.1(5) . . ? N16 C70 C69 125.2(5) . . ? N16 C71 C67 122.9(5) . . ? N16 C71 C72 116.6(5) . . ? C67 C71 C72 120.5(5) . . ? N15 C72 C64 122.2(4) . . ? N15 C72 C71 116.3(4) . . ? C64 C72 C71 121.5(5) . . ? N17 C77 C78 122.6(5) . . ? C77 C78 C79 120.6(5) . . ? C77 C78 C89 117.6(5) . . ? C79 C78 C89 121.7(5) . . ? C78 C79 C80 117.1(5) . . ? C78 C79 C90 121.8(5) . . ? C80 C79 C90 121.0(5) . . ? C88 C80 C79 119.2(5) . . ? C88 C80 C81 115.8(5) . . ? C79 C80 C81 125.0(5) . . ? C82 C81 C80 122.5(6) . . ? C81 C82 C83 121.6(6) . . ? C87 C83 C82 117.5(5) . . ? C87 C83 C84 118.3(6) . . ? C82 C83 C84 124.2(6) . . ? C85 C84 C83 117.4(6) . . ? C85 C84 C91 122.5(6) . . ? C83 C84 C91 120.1(6) . . ? C84 C85 C86 120.0(6) . . ? C84 C85 C92 121.6(6) . . ? C86 C85 C92 118.4(7) . . ? N18 C86 C85 123.2(7) . . ? N18 C87 C83 123.6(5) . . ? N18 C87 C88 116.0(5) . . ? C83 C87 C88 120.4(5) . . ? N17 C88 C80 121.9(5) . . ? N17 C88 C87 116.1(5) . . ? C80 C88 C87 122.0(5) . . ? N19 C93 C94 122.0(8) . . ? C95 C94 C93 120.1(8) . . ? C95 C94 C105 119.2(9) . . ? C93 C94 C105 120.7(9) . . ? C94 C95 C96 118.0(8) . . ? C94 C95 C106 124.1(8) . . ? C96 C95 C106 117.3(8) . . ? C95 C96 C104 116.9(8) . . ? C95 C96 C97 125.3(8) . . ? C104 C96 C97 117.5(7) . . ? C98 C97 C96 122.0(8) . . ? C97 C98 C99 121.7(8) . . ? C103 C99 C100 118.2(6) . . ? C103 C99 C98 116.6(6) . . ? C100 C99 C98 125.1(7) . . ? C101 C100 C99 118.5(6) . . ? C101 C100 C107 120.6(6) . . ? C99 C100 C107 120.9(6) . . ? C100 C101 C102 119.0(6) . . ? C100 C101 C108 123.1(6) . . ? C102 C101 C108 117.8(6) . . ? N20 C102 C101 122.7(6) . . ? N20 C103 C99 122.7(6) . . ? N20 C103 C104 114.9(6) . . ? C99 C103 C104 122.4(6) . . ? N19 C104 C96 123.4(6) . . ? N19 C104 C103 116.9(6) . . ? C96 C104 C103 119.7(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.147 _refine_diff_density_min -1.146 _refine_diff_density_rms 0.292 #end======================== data_{[Co(tmphen)2]3[Fe(CN)6]2}_150K #======================================================================= _audit_creation_method SHELXL-97 _chemical_name_systematic ; '{[Co(tmphen)2]3[Fe(CN)6]2}.8H2O' ; _chemical_name_common '{[Co(tmphen)2]3[Fe(CN)6]2}.8H2O' _chemical_melting_point ? _chemical_formula_moiety 'C108 H112 Co3 Fe2 N24 O8' _chemical_formula_sum 'C108 H112 Co3 Fe2 N24 O8' _chemical_formula_weight 2162.7 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.05(5) _cell_length_b 25.16(7) _cell_length_c 24.45(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.62(6) _cell_angle_gamma 90.00 _cell_volume 11617(54) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12002 _cell_measurement_theta_min 2.063 _cell_measurement_theta_max 17.2425 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4436 _exptl_absorpt_coefficient_mu 0.725 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8511 _exptl_absorpt_correction_T_max 0.9181 _exptl_absorpt_process_details 'SADABS: Bruker,2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER APEX' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37304 _diffrn_reflns_av_R_equivalents 0.2171 _diffrn_reflns_av_sigmaI/netI 0.1954 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 20.81 _reflns_number_total 12002 _reflns_number_gt 5828 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER, 2000)' _computing_cell_refinement 'SAINT (BRUKER, 2001)' _computing_data_reduction 'SAINT (BRUKER, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0153(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12002 _refine_ls_number_parameters 1326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1901 _refine_ls_R_factor_gt 0.1210 _refine_ls_wR_factor_ref 0.3452 _refine_ls_wR_factor_gt 0.2919 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.437 _refine_ls_shift/su_mean 0.007 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.06142(9) 0.37142(8) 0.61561(8) 0.0498(7) Uani 1 1 d . . . Co3 Co 0.35596(9) 0.54639(7) 0.66436(8) 0.0499(7) Uani 1 1 d . . . Co2 Co 0.29370(10) 0.36747(7) 0.83122(8) 0.0517(7) Uani 1 1 d . . . Fe1 Fe 0.32467(10) 0.35118(8) 0.63448(9) 0.0553(7) Uani 1 1 d . . . Fe2 Fe 0.13897(11) 0.51590(8) 0.75379(9) 0.0574(7) Uani 1 1 d . . . N15 N 0.0135(5) 0.2964(4) 0.5872(5) 0.045(3) Uani 1 1 d . . . N13 N 0.0719(6) 0.3956(4) 0.5350(4) 0.048(3) Uani 1 1 d . . . N21 N 0.4344(5) 0.5181(5) 0.7228(5) 0.050(3) Uani 1 1 d . . . N4 N 0.1630(6) 0.3435(4) 0.6265(4) 0.049(3) Uani 1 1 d . . . C4 C 0.2228(8) 0.3469(5) 0.6295(5) 0.047(4) Uani 1 1 d . . . N6 N 0.3293(5) 0.4741(5) 0.6304(5) 0.054(3) Uani 1 1 d . . . N22 N 0.3959(7) 0.6173(4) 0.7024(5) 0.059(3) Uani 1 1 d . . . N9 N 0.2781(7) 0.5419(4) 0.7109(5) 0.056(3) Uani 1 1 d . . . N7 N 0.0930(5) 0.4411(5) 0.6579(5) 0.046(3) Uani 1 1 d . . . C5 C 0.3282(7) 0.3628(5) 0.7126(7) 0.053(4) Uani 1 1 d . . . N8 N 0.2134(6) 0.4195(5) 0.8103(5) 0.056(3) Uani 1 1 d . . . N20 N 0.3621(7) 0.4267(5) 0.8589(5) 0.062(3) Uani 1 1 d . . . N16 N 0.0292(6) 0.3367(5) 0.6873(5) 0.052(3) Uani 1 1 d . . . N14 N -0.0407(6) 0.4040(5) 0.5882(5) 0.056(3) Uiso 1 1 d . . . N24 N 0.3016(6) 0.5930(5) 0.6035(5) 0.061(3) Uani 1 1 d . . . C8 C 0.1825(7) 0.4554(6) 0.7893(5) 0.040(3) Uani 1 1 d . . . N5 N 0.3253(6) 0.3672(4) 0.7586(5) 0.056(3) Uani 1 1 d . . . C7 C 0.1112(7) 0.4718(6) 0.6928(6) 0.050(4) Uani 1 1 d . . . N23 N 0.4298(6) 0.5531(5) 0.6112(5) 0.054(3) Uani 1 1 d . . . C108 C 0.4090(8) 0.5819(6) 0.5676(8) 0.059(4) Uani 1 1 d . . . N17 N 0.2265(6) 0.3037(4) 0.8094(6) 0.056(3) Uani 1 1 d . . . N18 N 0.2601(7) 0.3518(5) 0.9041(5) 0.062(4) Uani 1 1 d . . . C6 C 0.3253(6) 0.4263(7) 0.6278(5) 0.049(4) Uani 1 1 d . . . C47 C -0.0465(7) 0.4232(5) 0.5386(7) 0.057(4) Uani 1 1 d . . . C59 C -0.0075(7) 0.2916(6) 0.6809(7) 0.058(4) Uani 1 1 d . . . C58 C 0.0399(7) 0.3551(6) 0.7377(7) 0.059(4) Uani 1 1 d . . . H58 H 0.0686 0.3860 0.7437 0.071 Uiso 1 1 calc R . . C10 C 0.1036(9) 0.5809(7) 0.7160(7) 0.069(5) Uani 1 1 d . . . C60 C -0.0149(6) 0.2680(6) 0.6263(6) 0.050(4) Uani 1 1 d . . . C96 C 0.4770(8) 0.5575(6) 0.7479(6) 0.055(4) Uani 1 1 d . . . C95 C 0.4557(7) 0.6112(6) 0.7368(6) 0.052(4) Uani 1 1 d . . . C103 C 0.3124(9) 0.6378(7) 0.5202(8) 0.074(5) Uani 1 1 d . . . C39 C 0.0689(8) 0.4308(6) 0.4247(6) 0.059(4) Uani 1 1 d . . . C85 C 0.4530(8) 0.4689(6) 0.7344(6) 0.060(4) Uani 1 1 d . . . H85 H 0.4223 0.4412 0.7194 0.072 Uiso 1 1 calc R . . N3 N 0.4868(7) 0.3595(5) 0.6389(6) 0.079(4) Uani 1 1 d . . . N19 N 0.3830(10) 0.3243(6) 0.8624(6) 0.092(5) Uani 1 1 d . . . C48 C 0.0124(8) 0.4190(5) 0.5068(7) 0.055(4) Uani 1 1 d . . . C3 C 0.4262(9) 0.3543(6) 0.6383(6) 0.064(4) Uani 1 1 d . . . C50 C -0.0252(7) 0.2262(6) 0.5248(6) 0.056(4) Uani 1 1 d . . . C37 C 0.1254(7) 0.3918(5) 0.5055(6) 0.053(4) Uani 1 1 d . . . H37 H 0.1676 0.3763 0.5238 0.064 Uiso 1 1 calc R . . C49 C 0.0062(7) 0.2751(6) 0.5372(7) 0.052(4) Uani 1 1 d . . . H49 H 0.0235 0.2944 0.5084 0.063 Uiso 1 1 calc R . . C105 C 0.2076(8) 0.6515(7) 0.5626(8) 0.077(5) Uani 1 1 d . . . C51 C -0.0541(7) 0.1978(6) 0.5621(7) 0.060(4) Uani 1 1 d . . . C97 C 0.4938(8) 0.5326(6) 0.6129(7) 0.065(4) Uani 1 1 d . . . H97 H 0.5105 0.5123 0.6448 0.078 Uiso 1 1 calc R . . C9 C 0.2265(8) 0.5313(6) 0.7279(6) 0.055(4) Uani 1 1 d . . . C64 C 0.1509(7) 0.2410(6) 0.8465(7) 0.060(4) Uani 1 1 d . . . C100 C 0.4509(9) 0.5888(6) 0.5237(7) 0.064(4) Uani 1 1 d . . . C43 C -0.1106(8) 0.4494(6) 0.5100(7) 0.062(4) Uani 1 1 d . . . C56 C -0.0260(8) 0.2873(7) 0.7739(7) 0.075(5) Uani 1 1 d . . . C40 C 0.0102(8) 0.4369(6) 0.4515(7) 0.056(4) Uani 1 1 d . . . C72 C 0.1971(7) 0.2837(6) 0.8522(7) 0.051(4) Uani 1 1 d . . . C71 C 0.2175(7) 0.3078(6) 0.9041(7) 0.057(4) Uani 1 1 d . . . C1 C 0.3166(9) 0.3373(6) 0.5597(7) 0.069(5) Uani 1 1 d . . . C45 C -0.1615(8) 0.4318(6) 0.5932(8) 0.070(5) Uani 1 1 d . . . C107 C 0.3378(8) 0.6057(7) 0.5617(7) 0.064(4) Uani 1 1 d . . . C38S C 0.1277(7) 0.4074(6) 0.4512(6) 0.052(4) Uani 1 1 d . . . C46 C -0.0960(8) 0.4087(7) 0.6157(8) 0.081(5) Uani 1 1 d . . . H46 H -0.0914 0.3960 0.6526 0.097 Uiso 1 1 calc R . . C98 C 0.5382(9) 0.5369(7) 0.5747(9) 0.073(5) Uani 1 1 d . . . C83 C 0.4248(10) 0.4096(7) 0.8863(7) 0.072(5) Uani 1 1 d . . . C52 C -0.0499(7) 0.2198(6) 0.6146(7) 0.061(4) Uani 1 1 d . . . C2 C 0.3254(7) 0.2761(7) 0.6468(6) 0.059(4) Uani 1 1 d . . . C91 C 0.4935(9) 0.6543(6) 0.7613(7) 0.072(5) Uani 1 1 d . . . C42 C -0.1116(8) 0.4680(6) 0.4549(7) 0.060(4) Uani 1 1 d . . . H42 H -0.1528 0.4852 0.4370 0.072 Uiso 1 1 calc R . . C102 C 0.3542(10) 0.6462(7) 0.4760(7) 0.079(5) Uani 1 1 d . . . H102 H 0.3362 0.6667 0.4446 0.095 Uiso 1 1 calc R . . C88 C 0.5409(8) 0.5470(6) 0.7814(6) 0.065(4) Uani 1 1 d . . . C99 C 0.5164(9) 0.5657(7) 0.5287(9) 0.074(5) Uani 1 1 d . . . C61 C 0.2077(8) 0.2807(6) 0.7620(7) 0.065(4) Uani 1 1 d . . . H61 H 0.2263 0.2949 0.7309 0.078 Uiso 1 1 calc R . . C79 C 0.4769(11) 0.4431(8) 0.9106(7) 0.082(5) Uani 1 1 d . . . C94 C 0.3739(8) 0.6671(7) 0.6940(7) 0.073(5) Uani 1 1 d . . . H94 H 0.3302 0.6715 0.6707 0.088 Uiso 1 1 calc R . . C55 C -0.0361(8) 0.2633(6) 0.7233(7) 0.063(4) Uani 1 1 d . . . C53 C -0.0808(9) 0.1946(7) 0.6595(9) 0.092(6) Uani 1 1 d . . . H53 H -0.1073 0.1628 0.6524 0.111 Uiso 1 1 calc R . . C82 C 0.3532(8) 0.4771(7) 0.8563(6) 0.064(4) Uani 1 1 d . . . H82 H 0.3087 0.4895 0.8387 0.077 Uiso 1 1 calc R . . C87 C 0.5603(8) 0.4937(7) 0.7891(6) 0.069(5) Uani 1 1 d . . . C86 C 0.5163(8) 0.4546(6) 0.7679(6) 0.068(5) Uani 1 1 d . . . N2 N 0.3237(6) 0.2298(6) 0.6545(6) 0.081(4) Uani 1 1 d . . . N10 N 0.0877(8) 0.6215(6) 0.6933(6) 0.083(4) Uani 1 1 d . . . C67 C 0.1912(7) 0.2892(7) 0.9514(8) 0.072(5) Uani 1 1 d . . . C106 C 0.2351(8) 0.6151(6) 0.6017(7) 0.069(5) Uani 1 1 d . . . H106 H 0.2067 0.6047 0.6290 0.083 Uiso 1 1 calc R . . N1 N 0.3114(6) 0.3266(6) 0.5144(7) 0.076(4) Uani 1 1 d . . . C13 C 0.1951(8) 0.3980(6) 0.4253(7) 0.078(5) Uani 1 1 d . . . H13A H 0.2319 0.3837 0.4533 0.117 Uiso 1 1 calc R . . H13B H 0.2112 0.4316 0.4112 0.117 Uiso 1 1 calc R . . H13C H 0.1854 0.3725 0.3950 0.117 Uiso 1 1 calc R . . C81 C 0.4043(10) 0.5172(7) 0.8774(7) 0.073(5) Uani 1 1 d . . . C57 C 0.0136(8) 0.3342(6) 0.7834(7) 0.065(4) Uani 1 1 d . . . C14 C 0.0643(9) 0.4527(7) 0.3659(6) 0.077(5) Uani 1 1 d . . . H14A H 0.0281 0.4330 0.3417 0.116 Uiso 1 1 calc R . . H14B H 0.1102 0.4487 0.3525 0.116 Uiso 1 1 calc R . . H14C H 0.0515 0.4904 0.3659 0.116 Uiso 1 1 calc R . . C65 C 0.1230(8) 0.2235(6) 0.8969(8) 0.073(5) Uani 1 1 d . . . H65 H 0.0885 0.1960 0.8945 0.087 Uiso 1 1 calc R . . C12 C 0.1684(9) 0.5566(7) 0.8194(7) 0.067(5) Uani 1 1 d . . . C41 C -0.0563(8) 0.4618(5) 0.4284(7) 0.063(4) Uani 1 1 d . . . H41 H -0.0600 0.4745 0.3915 0.075 Uiso 1 1 calc R . . C21 C 0.1515(8) 0.2159(6) 0.6948(6) 0.064(4) Uani 1 1 d . . . H21A H 0.1694 0.1793 0.6949 0.096 Uiso 1 1 calc R . . H21B H 0.1762 0.2377 0.6702 0.096 Uiso 1 1 calc R . . H21C H 0.1006 0.2160 0.6817 0.096 Uiso 1 1 calc R . . C15 C -0.2336(7) 0.4792(7) 0.5151(7) 0.086(5) Uani 1 1 d . . . H15A H -0.2717 0.4694 0.5365 0.129 Uiso 1 1 calc R . . H15B H -0.2457 0.4672 0.4769 0.129 Uiso 1 1 calc R . . H15C H -0.2276 0.5179 0.5158 0.129 Uiso 1 1 calc R . . C31 C 0.5078(12) 0.7551(7) 0.7761(9) 0.135(9) Uani 1 1 d . . . H31A H 0.5425 0.7660 0.7520 0.203 Uiso 1 1 calc R . . H31B H 0.5326 0.7456 0.8125 0.203 Uiso 1 1 calc R . . H31C H 0.4752 0.7846 0.7800 0.203 Uiso 1 1 calc R . . C62 C 0.1644(7) 0.2385(6) 0.7534(7) 0.058(4) Uani 1 1 d . . . C54 C -0.0723(9) 0.2160(7) 0.7121(7) 0.081(5) Uani 1 1 d . . . H54 H -0.0915 0.1980 0.7409 0.097 Uiso 1 1 calc R . . C77 C 0.5493(13) 0.3656(12) 0.9381(9) 0.131(10) Uani 1 1 d . . . H77 H 0.5913 0.3514 0.9580 0.157 Uiso 1 1 calc R . . C104 C 0.2440(10) 0.6622(7) 0.5188(8) 0.081(5) Uani 1 1 d . . . C17 C -0.0259(8) 0.2052(6) 0.4664(6) 0.075(5) Uani 1 1 d . . . H17A H -0.0020 0.1707 0.4676 0.112 Uiso 1 1 calc R . . H17B H -0.0012 0.2303 0.4450 0.112 Uiso 1 1 calc R . . H17C H -0.0750 0.2012 0.4489 0.112 Uiso 1 1 calc R . . N11 N -0.0064(9) 0.4906(7) 0.7909(7) 0.109(6) Uani 1 1 d . . . C63 C 0.1337(7) 0.2167(6) 0.7938(8) 0.061(4) Uani 1 1 d . . . C44 C -0.1661(8) 0.4534(7) 0.5398(9) 0.072(5) Uani 1 1 d . . . C90 C 0.5585(10) 0.6419(8) 0.7968(7) 0.095(6) Uani 1 1 d . . . H90 H 0.5853 0.6698 0.8157 0.114 Uiso 1 1 calc R . . C70 C 0.2781(9) 0.3721(8) 0.9491(9) 0.089(6) Uani 1 1 d . . . H70 H 0.3093 0.4016 0.9494 0.107 Uiso 1 1 calc R . . C84 C 0.4352(11) 0.3540(9) 0.8853(7) 0.087(6) Uani 1 1 d . . . C23 C 0.1869(9) 0.2959(8) 1.0550(6) 0.097(6) Uani 1 1 d . . . H23A H 0.2142 0.3122 1.0875 0.146 Uiso 1 1 calc R . . H23B H 0.1926 0.2572 1.0569 0.146 Uiso 1 1 calc R . . H23C H 0.1367 0.3049 1.0541 0.146 Uiso 1 1 calc R . . C30 C 0.6290(10) 0.4792(8) 0.8249(8) 0.117(7) Uani 1 1 d . . . H30A H 0.6245 0.4863 0.8636 0.175 Uiso 1 1 calc R . . H30B H 0.6678 0.5005 0.8138 0.175 Uiso 1 1 calc R . . H30C H 0.6391 0.4414 0.8202 0.175 Uiso 1 1 calc R . . C33 C 0.6113(8) 0.5122(7) 0.5854(8) 0.098(6) Uani 1 1 d . . . H33A H 0.6172 0.4866 0.5561 0.147 Uiso 1 1 calc R . . H33B H 0.6168 0.4939 0.6211 0.147 Uiso 1 1 calc R . . H33C H 0.6473 0.5401 0.5860 0.147 Uiso 1 1 calc R . . C80 C 0.4673(10) 0.4993(9) 0.9066(7) 0.091(6) Uani 1 1 d . . . C101 C 0.4213(11) 0.6239(8) 0.4801(8) 0.090(6) Uani 1 1 d . . . H101 H 0.4497 0.6323 0.4521 0.108 Uiso 1 1 calc R . . C74 C 0.453(2) 0.2450(11) 0.8844(13) 0.167(14) Uani 1 1 d . . . C93 C 0.4052(9) 0.7118(7) 0.7141(9) 0.092(6) Uani 1 1 d . . . C18 C -0.0904(9) 0.1449(7) 0.5455(7) 0.091(6) Uani 1 1 d . . . H18A H -0.1105 0.1462 0.5065 0.137 Uiso 1 1 calc R . . H18B H -0.1284 0.1385 0.5681 0.137 Uiso 1 1 calc R . . H18C H -0.0557 0.1160 0.5512 0.137 Uiso 1 1 calc R . . C78 C 0.5422(11) 0.4198(11) 0.9380(8) 0.123(8) Uani 1 1 d . . . H78 H 0.5791 0.4417 0.9556 0.147 Uiso 1 1 calc R . . C11 C 0.0488(9) 0.5013(7) 0.7774(7) 0.078(5) Uani 1 1 d . . . C68 C 0.2130(9) 0.3163(8) 1.0040(7) 0.085(5) Uani 1 1 d . . . C89 C 0.5810(9) 0.5918(7) 0.8032(7) 0.086(6) Uani 1 1 d . . . H89 H 0.6264 0.5857 0.8235 0.103 Uiso 1 1 calc R . . C34 C 0.5631(9) 0.5740(7) 0.4838(8) 0.109(7) Uani 1 1 d . . . H34A H 0.5870 0.6085 0.4890 0.163 Uiso 1 1 calc R . . H34B H 0.5340 0.5733 0.4476 0.163 Uiso 1 1 calc R . . H34C H 0.5987 0.5457 0.4856 0.163 Uiso 1 1 calc R . . C27 C 0.5191(10) 0.5401(8) 0.9342(7) 0.106(7) Uani 1 1 d . . . H27A H 0.5638 0.5225 0.9483 0.158 Uiso 1 1 calc R . . H27B H 0.4991 0.5568 0.9649 0.158 Uiso 1 1 calc R . . H27C H 0.5280 0.5673 0.9073 0.158 Uiso 1 1 calc R . . C92 C 0.4659(10) 0.7068(6) 0.7508(8) 0.087(5) Uani 1 1 d . . . C29 C 0.5335(9) 0.3942(6) 0.7740(8) 0.096(6) Uani 1 1 d . . . H29A H 0.5738 0.3857 0.7544 0.143 Uiso 1 1 calc R . . H29B H 0.4921 0.3735 0.7582 0.143 Uiso 1 1 calc R . . H29C H 0.5454 0.3853 0.8131 0.143 Uiso 1 1 calc R . . C36 C 0.1362(9) 0.6737(7) 0.5695(6) 0.080(5) Uani 1 1 d . . . H36A H 0.1390 0.7125 0.5718 0.121 Uiso 1 1 calc R . . H36B H 0.1211 0.6595 0.6035 0.121 Uiso 1 1 calc R . . H36C H 0.1018 0.6634 0.5379 0.121 Uiso 1 1 calc R . . C69 C 0.2581(10) 0.3570(8) 1.0020(7) 0.092(6) Uani 1 1 d . . . C73 C 0.3876(16) 0.2688(7) 0.8589(9) 0.130(9) Uani 1 1 d . . . H73 H 0.3498 0.2479 0.8409 0.157 Uiso 1 1 calc R . . C22 C 0.0884(9) 0.1685(6) 0.7861(7) 0.083(5) Uani 1 1 d . . . H22A H 0.0483 0.1752 0.7575 0.124 Uiso 1 1 calc R . . H22B H 0.0706 0.1598 0.8209 0.124 Uiso 1 1 calc R . . H22C H 0.1163 0.1386 0.7749 0.124 Uiso 1 1 calc R . . N12 N 0.1857(8) 0.5808(6) 0.8570(6) 0.084(5) Uani 1 1 d . . . C75 C 0.509(2) 0.2739(13) 0.9102(12) 0.157(13) Uani 1 1 d . . . C35 C 0.2120(11) 0.6976(9) 0.4747(8) 0.116(7) Uani 1 1 d . . . H35A H 0.2152 0.6811 0.4388 0.174 Uiso 1 1 calc R . . H35B H 0.2373 0.7316 0.4771 0.174 Uiso 1 1 calc R . . H35C H 0.1621 0.7037 0.4787 0.174 Uiso 1 1 calc R . . C24 C 0.2849(11) 0.3860(9) 1.0567(8) 0.134(9) Uani 1 1 d . . . H24A H 0.2744 0.4240 1.0527 0.201 Uiso 1 1 calc R . . H24B H 0.3362 0.3810 1.0654 0.201 Uiso 1 1 calc R . . H24C H 0.2612 0.3713 1.0865 0.201 Uiso 1 1 calc R . . C66 C 0.1452(8) 0.2454(7) 0.9455(7) 0.068(5) Uani 1 1 d . . . H66 H 0.1294 0.2309 0.9775 0.081 Uiso 1 1 calc R . . C28 C 0.3844(8) 0.5752(6) 0.8699(7) 0.080(5) Uani 1 1 d . . . H28A H 0.3871 0.5924 0.9061 0.120 Uiso 1 1 calc R . . H28B H 0.3361 0.5781 0.8507 0.120 Uiso 1 1 calc R . . H28C H 0.4173 0.5928 0.8481 0.120 Uiso 1 1 calc R . . C16 C -0.2174(9) 0.4330(8) 0.6287(7) 0.102(6) Uani 1 1 d . . . H16A H -0.2224 0.4692 0.6424 0.154 Uiso 1 1 calc R . . H16B H -0.2051 0.4088 0.6600 0.154 Uiso 1 1 calc R . . H16C H -0.2622 0.4217 0.6076 0.154 Uiso 1 1 calc R . . C76 C 0.5019(15) 0.3301(11) 0.9122(8) 0.124(8) Uani 1 1 d . . . C25 C 0.452(2) 0.1827(9) 0.8822(11) 0.235(19) Uani 1 1 d . . . H25A H 0.4790 0.1704 0.8532 0.353 Uiso 1 1 calc R . . H25B H 0.4028 0.1705 0.8739 0.353 Uiso 1 1 calc R . . H25C H 0.4729 0.1684 0.9179 0.353 Uiso 1 1 calc R . . C20 C 0.0300(9) 0.3610(6) 0.8391(6) 0.074(5) Uani 1 1 d . . . H20A H -0.0128 0.3783 0.8487 0.111 Uiso 1 1 calc R . . H20B H 0.0671 0.3878 0.8374 0.111 Uiso 1 1 calc R . . H20C H 0.0464 0.3344 0.8672 0.111 Uiso 1 1 calc R . . C19 C -0.0602(10) 0.2612(7) 0.8207(6) 0.095(6) Uani 1 1 d . . . H19A H -0.0843 0.2884 0.8402 0.143 Uiso 1 1 calc R . . H19B H -0.0235 0.2440 0.8467 0.143 Uiso 1 1 calc R . . H19C H -0.0947 0.2345 0.8052 0.143 Uiso 1 1 calc R . . C32 C 0.3767(11) 0.7688(7) 0.7005(9) 0.132(9) Uani 1 1 d . . . H32A H 0.3281 0.7668 0.6818 0.198 Uiso 1 1 calc R . . H32B H 0.4067 0.7865 0.6765 0.198 Uiso 1 1 calc R . . H32C H 0.3775 0.7891 0.7348 0.198 Uiso 1 1 calc R . . C26 C 0.5699(16) 0.2468(11) 0.9410(11) 0.204(15) Uani 1 1 d . . . H26A H 0.5604 0.2396 0.9787 0.305 Uiso 1 1 calc R . . H26B H 0.6119 0.2695 0.9421 0.305 Uiso 1 1 calc R . . H26C H 0.5783 0.2132 0.9227 0.305 Uiso 1 1 calc R . . O17S O 0.6973(15) 0.4805(11) 1.0092(10) 0.119(9) Uiso 0.50 1 d P A -17 O12S O 0.239(2) 0.0607(18) 0.7630(17) 0.215(17) Uiso 0.50 1 d P B -12 O3S O 0.219(2) 0.8323(18) 0.6064(18) 0.218(17) Uiso 0.50 1 d P C -3 O18S O 0.6342(15) 0.3846(11) 0.6820(11) 0.125(9) Uiso 0.50 1 d P D -18 O16S O 0.5223(17) 0.2890(12) 1.0708(12) 0.139(10) Uiso 0.50 1 d P E -16 O8S O -0.146(3) 0.4608(19) 0.7704(18) 0.229(19) Uiso 0.50 1 d P F -8 O15S O 0.440(2) 0.2689(14) 1.0464(14) 0.169(13) Uiso 0.50 1 d P G -15 O10S O 0.068(2) 0.0857(16) 0.4979(15) 0.174(13) Uiso 0.50 1 d P H -10 O2S O 0.370(3) 0.681(2) 0.3404(18) 0.232(19) Uiso 0.50 1 d P I -2 O14S O 0.3080(17) 0.1753(13) 0.7681(13) 0.149(11) Uiso 0.50 1 d P J -14 O5S O 0.264(3) 0.690(2) 0.7995(19) 0.24(2) Uiso 0.50 1 d P K -5 O9S O -0.085(2) 0.5785(17) 0.8589(16) 0.209(16) Uiso 0.50 1 d P L -9 O4S O 0.262(4) 0.751(3) 0.826(3) 0.16(3) Uiso 0.25 1 d P . -4 O11S O 0.086(2) 0.0569(15) 0.4603(15) 0.162(13) Uiso 0.50 1 d P M -11 O1S O 0.250(4) 0.709(3) 0.327(3) 0.17(3) Uiso 0.25 1 d P . . O7S O 0.1181(19) 0.4814(14) 0.9199(14) 0.164(12) Uiso 0.50 1 d P N -7 O13S O 0.289(4) 0.111(3) 0.794(3) 0.16(2) Uiso 0.25 1 d P O -13 O6S O 0.284(3) 0.664(2) 0.942(2) 0.109(16) Uiso 0.25 1 d P P -6 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0182(11) 0.0696(14) 0.0628(14) 0.0091(10) 0.0101(9) -0.0005(9) Co3 0.0271(12) 0.0462(13) 0.0793(15) 0.0022(9) 0.0180(10) -0.0013(8) Co2 0.0416(13) 0.0473(13) 0.0670(14) 0.0043(9) 0.0106(10) -0.0003(9) Fe1 0.0250(13) 0.0593(15) 0.0819(17) 0.0145(11) 0.0088(11) -0.0004(10) Fe2 0.0510(15) 0.0559(14) 0.0699(16) 0.0058(11) 0.0254(12) 0.0157(10) N15 0.016(6) 0.066(8) 0.056(8) 0.005(7) 0.015(6) 0.011(5) N13 0.023(7) 0.061(8) 0.063(8) 0.008(6) 0.012(7) -0.001(6) N21 0.033(7) 0.043(8) 0.076(9) 0.006(6) 0.020(6) 0.002(6) N4 0.009(6) 0.073(8) 0.066(8) 0.016(6) 0.007(6) -0.007(6) C4 0.039(10) 0.045(9) 0.059(10) 0.003(7) 0.010(8) -0.008(7) N6 0.025(7) 0.072(9) 0.072(9) 0.008(7) 0.027(6) -0.001(6) N22 0.052(9) 0.041(8) 0.089(10) 0.008(6) 0.031(8) 0.006(6) N9 0.049(9) 0.056(8) 0.063(8) -0.001(6) 0.011(7) 0.013(6) N7 0.024(7) 0.062(8) 0.056(8) 0.028(6) 0.016(6) 0.003(6) C5 0.029(9) 0.058(10) 0.067(11) 0.019(9) -0.007(8) -0.010(7) N8 0.034(8) 0.048(8) 0.087(10) 0.012(7) 0.017(7) 0.001(6) N20 0.067(10) 0.038(9) 0.079(9) 0.010(6) 0.009(8) 0.017(7) N16 0.024(7) 0.075(10) 0.059(9) -0.012(7) 0.008(6) 0.002(6) N24 0.037(8) 0.075(9) 0.074(9) 0.001(7) 0.021(7) -0.004(7) C8 0.026(8) 0.058(10) 0.040(8) 0.000(7) 0.021(7) 0.000(7) N5 0.055(9) 0.060(8) 0.049(8) 0.013(7) -0.003(7) -0.009(6) C7 0.029(9) 0.066(11) 0.057(10) -0.010(8) 0.008(8) 0.005(7) N23 0.026(8) 0.057(8) 0.082(10) 0.001(7) 0.013(7) -0.004(6) C108 0.031(10) 0.056(10) 0.096(14) -0.020(9) 0.037(10) -0.009(8) N17 0.038(8) 0.047(8) 0.082(10) 0.014(7) 0.008(7) -0.017(6) N18 0.062(9) 0.088(10) 0.034(8) -0.024(7) 0.002(6) -0.005(8) C6 0.005(7) 0.077(12) 0.063(10) 0.014(8) 0.000(6) -0.003(7) C47 0.012(8) 0.050(9) 0.111(14) -0.008(9) 0.013(9) -0.001(7) C59 0.027(9) 0.065(11) 0.083(13) -0.017(10) 0.011(8) -0.015(8) C58 0.040(10) 0.049(10) 0.088(14) 0.006(9) 0.002(9) -0.017(7) C10 0.076(12) 0.061(12) 0.080(12) -0.009(9) 0.044(10) 0.008(9) C60 0.015(8) 0.055(10) 0.076(12) 0.005(9) -0.007(8) -0.017(7) C96 0.040(10) 0.050(11) 0.072(10) 0.005(8) -0.002(8) 0.007(8) C95 0.025(9) 0.054(11) 0.073(11) 0.009(8) -0.010(8) -0.002(8) C103 0.053(12) 0.087(13) 0.090(14) -0.002(11) 0.035(11) 0.000(10) C39 0.054(11) 0.056(10) 0.069(11) 0.010(8) 0.020(10) -0.001(8) C85 0.045(10) 0.058(12) 0.082(12) -0.003(8) 0.026(9) -0.001(8) N3 0.030(9) 0.097(11) 0.113(12) 0.010(8) 0.015(8) 0.001(7) N19 0.121(15) 0.061(11) 0.098(12) 0.013(8) 0.034(11) 0.039(10) C48 0.037(11) 0.048(9) 0.078(12) 0.001(8) 0.001(9) -0.003(7) C3 0.034(10) 0.070(11) 0.088(12) -0.002(8) 0.010(9) 0.001(8) C50 0.035(9) 0.063(11) 0.069(12) -0.003(9) 0.006(8) 0.011(8) C37 0.026(9) 0.053(10) 0.078(12) 0.022(8) 0.000(8) -0.002(7) C49 0.036(9) 0.058(11) 0.070(12) -0.003(8) 0.030(8) 0.009(8) C105 0.026(10) 0.083(13) 0.115(16) -0.010(11) -0.020(11) 0.016(9) C51 0.035(9) 0.075(12) 0.072(12) 0.004(10) 0.015(9) -0.009(8) C97 0.025(10) 0.065(11) 0.109(14) -0.013(9) 0.022(10) -0.001(8) C9 0.042(10) 0.057(10) 0.069(11) 0.007(8) 0.023(9) 0.010(8) C64 0.029(9) 0.066(11) 0.091(13) 0.027(10) 0.023(9) 0.010(8) C100 0.054(12) 0.062(11) 0.076(12) -0.003(9) 0.013(10) -0.009(9) C43 0.029(10) 0.063(11) 0.096(14) -0.023(9) 0.009(10) -0.016(8) C56 0.057(11) 0.088(13) 0.082(14) 0.004(11) 0.015(10) -0.026(10) C40 0.039(11) 0.056(10) 0.071(12) -0.007(8) -0.004(9) -0.008(8) C72 0.014(8) 0.053(10) 0.083(12) -0.001(9) -0.004(8) -0.011(7) C71 0.029(9) 0.066(11) 0.078(13) 0.002(9) 0.017(9) -0.027(8) C1 0.084(14) 0.069(12) 0.049(11) 0.004(9) -0.005(10) -0.013(9) C45 0.032(11) 0.072(12) 0.113(16) -0.025(11) 0.030(11) -0.004(8) C107 0.045(11) 0.084(12) 0.065(12) -0.007(10) 0.012(10) -0.014(9) C38S 0.025(9) 0.063(10) 0.063(11) 0.024(8) -0.013(8) 0.002(7) C46 0.033(11) 0.098(14) 0.118(15) -0.004(11) 0.039(10) 0.008(9) C98 0.043(12) 0.088(13) 0.098(15) -0.022(11) 0.041(11) -0.009(10) C83 0.077(14) 0.056(13) 0.081(12) 0.001(9) -0.002(10) 0.022(11) C52 0.035(9) 0.085(12) 0.063(11) -0.002(10) 0.011(8) -0.007(9) C2 0.016(8) 0.075(12) 0.086(12) 0.010(9) 0.009(7) -0.003(8) C91 0.057(12) 0.044(11) 0.110(14) 0.015(9) -0.012(10) -0.001(9) C42 0.045(11) 0.066(11) 0.067(12) 0.006(9) 0.006(9) 0.010(8) C102 0.075(14) 0.091(14) 0.071(12) -0.005(9) 0.006(11) -0.021(11) C88 0.047(11) 0.061(12) 0.084(12) -0.002(9) -0.001(9) -0.002(9) C99 0.041(12) 0.078(13) 0.113(16) -0.038(11) 0.047(12) -0.019(10) C61 0.052(11) 0.062(11) 0.084(14) -0.003(9) 0.014(10) -0.001(9) C79 0.085(15) 0.077(14) 0.083(13) -0.013(10) 0.002(11) 0.023(12) C94 0.034(10) 0.068(13) 0.109(14) 0.004(10) -0.021(9) 0.004(9) C55 0.048(10) 0.082(12) 0.062(11) -0.009(10) 0.021(9) -0.036(9) C53 0.068(13) 0.091(14) 0.122(17) -0.003(12) 0.028(12) -0.044(10) C82 0.038(10) 0.091(15) 0.063(11) -0.006(9) 0.006(8) 0.002(10) C87 0.053(11) 0.064(12) 0.081(12) -0.009(9) -0.018(9) 0.006(9) C86 0.047(11) 0.071(12) 0.079(12) -0.007(9) -0.019(9) 0.018(9) N2 0.041(9) 0.070(11) 0.129(13) 0.011(9) 0.003(8) 0.010(7) N10 0.094(12) 0.072(11) 0.086(11) 0.005(8) 0.023(8) 0.032(9) C67 0.021(9) 0.094(13) 0.100(14) 0.017(11) 0.006(9) -0.017(9) C106 0.024(10) 0.081(12) 0.103(14) -0.014(10) 0.007(9) -0.007(9) N1 0.034(8) 0.088(11) 0.106(12) 0.021(9) 0.005(8) -0.008(7) C13 0.064(12) 0.076(12) 0.100(13) 0.014(9) 0.035(10) -0.005(9) C81 0.068(13) 0.071(12) 0.084(12) -0.001(9) 0.030(10) 0.004(10) C57 0.044(10) 0.084(12) 0.068(12) 0.010(10) 0.013(9) -0.023(9) C14 0.065(12) 0.098(13) 0.071(12) 0.010(9) 0.016(9) -0.001(9) C65 0.048(11) 0.068(11) 0.112(15) 0.019(11) 0.043(11) -0.007(8) C12 0.068(12) 0.069(12) 0.066(12) -0.015(9) 0.014(10) 0.013(9) C41 0.043(10) 0.057(10) 0.083(12) 0.008(8) -0.009(10) 0.009(8) C21 0.046(10) 0.070(11) 0.077(12) -0.007(9) 0.013(8) -0.019(8) C15 0.029(10) 0.101(14) 0.126(15) -0.027(11) 0.002(10) 0.004(9) C31 0.14(2) 0.054(13) 0.18(2) -0.007(12) -0.080(16) -0.011(12) C62 0.036(9) 0.063(11) 0.079(12) -0.002(9) 0.023(9) -0.027(8) C54 0.085(13) 0.098(14) 0.065(12) -0.019(10) 0.028(10) -0.051(11) C77 0.12(2) 0.15(2) 0.111(18) -0.038(17) -0.042(15) 0.074(19) C104 0.068(14) 0.109(15) 0.070(13) 0.007(11) 0.024(11) -0.023(11) C17 0.055(11) 0.090(13) 0.081(13) -0.007(10) 0.016(9) -0.010(9) N11 0.073(12) 0.137(15) 0.126(14) 0.020(10) 0.045(11) 0.041(10) C63 0.032(9) 0.055(10) 0.093(13) -0.002(10) 0.003(9) -0.012(8) C44 0.025(11) 0.078(12) 0.110(15) -0.027(11) -0.004(10) -0.001(8) C90 0.082(15) 0.080(15) 0.113(15) -0.001(11) -0.026(12) -0.025(11) C70 0.076(14) 0.114(16) 0.087(15) 0.012(13) 0.047(12) -0.041(11) C84 0.086(16) 0.101(18) 0.072(13) 0.014(12) 0.003(11) 0.021(14) C23 0.063(12) 0.17(2) 0.063(12) 0.014(12) 0.022(10) -0.021(12) C30 0.077(15) 0.091(15) 0.17(2) -0.010(13) -0.047(13) 0.012(11) C33 0.038(11) 0.111(15) 0.156(18) -0.028(12) 0.052(11) 0.000(10) C80 0.062(14) 0.127(19) 0.081(14) -0.011(12) -0.001(11) 0.014(13) C101 0.083(16) 0.094(15) 0.104(16) -0.028(13) 0.053(13) -0.028(12) C74 0.28(5) 0.07(2) 0.15(3) 0.017(17) 0.02(3) 0.08(2) C93 0.053(12) 0.046(12) 0.165(18) 0.012(11) -0.031(12) -0.004(9) C18 0.089(14) 0.093(14) 0.095(14) -0.006(10) 0.020(11) -0.025(11) C78 0.080(16) 0.15(2) 0.128(19) -0.002(15) -0.025(13) 0.044(15) C11 0.049(11) 0.097(14) 0.091(13) 0.022(10) 0.025(10) 0.039(10) C68 0.066(13) 0.113(15) 0.075(14) -0.025(11) 0.010(10) -0.027(12) C89 0.076(13) 0.052(12) 0.117(15) 0.005(10) -0.036(11) 0.003(10) C34 0.078(14) 0.110(16) 0.152(18) -0.053(13) 0.061(14) -0.037(11) C27 0.083(14) 0.132(18) 0.094(14) -0.023(12) -0.016(11) -0.030(13) C92 0.078(14) 0.046(12) 0.130(16) -0.011(10) -0.006(12) -0.019(10) C29 0.085(14) 0.035(10) 0.155(17) 0.015(10) -0.027(12) 0.009(9) C36 0.070(13) 0.090(13) 0.082(12) -0.002(9) 0.012(10) -0.003(10) C69 0.070(13) 0.126(17) 0.079(14) -0.026(12) 0.002(11) -0.038(12) C73 0.23(3) 0.033(13) 0.132(18) 0.010(11) 0.048(19) 0.037(14) C22 0.073(13) 0.072(12) 0.107(14) 0.000(10) 0.025(10) -0.017(10) N12 0.113(13) 0.066(10) 0.077(11) 0.003(8) 0.026(10) 0.023(9) C75 0.21(4) 0.10(2) 0.16(3) 0.004(18) 0.00(2) 0.11(2) C35 0.099(17) 0.15(2) 0.100(16) 0.021(14) 0.002(13) 0.003(14) C24 0.094(17) 0.19(2) 0.121(18) -0.049(16) 0.012(14) -0.052(16) C66 0.048(11) 0.085(13) 0.070(12) -0.001(10) 0.006(9) -0.015(9) C28 0.061(11) 0.064(12) 0.117(14) -0.008(10) 0.019(10) 0.001(9) C16 0.050(12) 0.149(18) 0.115(15) -0.031(13) 0.039(11) -0.002(11) C76 0.16(2) 0.14(2) 0.070(15) -0.004(14) -0.016(14) 0.06(2) C25 0.43(6) 0.09(2) 0.17(2) 0.027(16) -0.02(3) 0.12(3) C20 0.092(14) 0.065(11) 0.068(12) -0.001(9) 0.016(10) -0.027(9) C19 0.117(16) 0.107(15) 0.066(12) 0.009(10) 0.026(11) -0.065(12) C32 0.105(17) 0.071(14) 0.20(2) 0.030(13) -0.064(15) -0.001(12) C26 0.23(3) 0.18(3) 0.18(3) 0.02(2) -0.04(2) 0.14(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N4 2.042(12) . ? Co1 N7 2.082(14) . ? Co1 N13 2.097(12) . ? Co1 N16 2.121(13) . ? Co1 N14 2.134(13) . ? Co1 N15 2.171(13) . ? Co3 N9 1.990(13) . ? Co3 N6 2.036(15) . ? Co3 N23 2.045(12) . ? Co3 N21 2.053(12) . ? Co3 N24 2.063(13) . ? Co3 N22 2.108(13) . ? Co2 N5 1.948(14) . ? Co2 N18 2.012(13) . ? Co2 N8 2.027(13) . ? Co2 N20 2.036(13) . ? Co2 N19 2.077(16) . ? Co2 N17 2.078(12) . ? Fe1 C1 1.848(18) . ? Fe1 C6 1.896(18) . ? Fe1 C2 1.912(19) . ? Fe1 C3 1.925(17) . ? Fe1 C5 1.924(18) . ? Fe1 C4 1.932(16) . ? Fe2 C7 1.877(16) . ? Fe2 C8 1.890(16) . ? Fe2 C9 1.902(16) . ? Fe2 C11 1.919(19) . ? Fe2 C12 1.923(18) . ? Fe2 C10 1.955(19) . ? N15 C49 1.326(16) . ? N15 C60 1.360(16) . ? N13 C37 1.329(16) . ? N13 C48 1.378(17) . ? N21 C85 1.309(17) . ? N21 C96 1.374(17) . ? N4 C4 1.135(15) . ? N6 C6 1.206(17) . ? N22 C94 1.329(18) . ? N22 C95 1.331(17) . ? N9 C9 1.146(16) . ? N7 C7 1.170(15) . ? C5 N5 1.140(16) . ? N8 C8 1.159(15) . ? N20 C82 1.281(18) . ? N20 C83 1.359(19) . ? N16 C58 1.307(17) . ? N16 C59 1.332(17) . ? N14 C47 1.298(17) . ? N14 C46 1.328(16) . ? N24 C107 1.346(18) . ? N24 C106 1.379(18) . ? N23 C108 1.306(18) . ? N23 C97 1.320(17) . ? C108 C100 1.43(2) . ? C108 C107 1.47(2) . ? N17 C61 1.302(17) . ? N17 C72 1.349(17) . ? N18 C70 1.22(2) . ? N18 C71 1.371(18) . ? C47 C48 1.450(19) . ? C47 C43 1.48(2) . ? C59 C55 1.423(19) . ? C59 C60 1.452(19) . ? C58 C57 1.388(19) . ? C10 N10 1.182(18) . ? C60 C52 1.394(19) . ? C96 C88 1.400(19) . ? C96 C95 1.426(19) . ? C95 C91 1.39(2) . ? C103 C107 1.34(2) . ? C103 C104 1.44(2) . ? C103 C102 1.44(2) . ? C39 C38S 1.351(19) . ? C39 C40 1.380(19) . ? C39 C14 1.530(19) . ? C85 C86 1.41(2) . ? N3 C3 1.160(17) . ? N19 C84 1.31(2) . ? N19 C73 1.40(2) . ? C48 C40 1.420(19) . ? C50 C51 1.333(19) . ? C50 C49 1.386(19) . ? C50 C17 1.522(19) . ? C37 C38S 1.390(18) . ? C105 C104 1.38(2) . ? C105 C106 1.38(2) . ? C105 C36 1.50(2) . ? C51 C52 1.39(2) . ? C51 C18 1.53(2) . ? C97 C98 1.35(2) . ? C64 C72 1.38(2) . ? C64 C63 1.42(2) . ? C64 C65 1.47(2) . ? C100 C99 1.37(2) . ? C100 C101 1.44(2) . ? C43 C44 1.37(2) . ? C43 C42 1.42(2) . ? C56 C55 1.37(2) . ? C56 C57 1.40(2) . ? C56 C19 1.538(19) . ? C40 C41 1.46(2) . ? C72 C71 1.412(19) . ? C71 C67 1.402(19) . ? C1 N1 1.130(17) . ? C45 C44 1.40(2) . ? C45 C46 1.42(2) . ? C45 C16 1.46(2) . ? C38S C13 1.524(19) . ? C98 C99 1.36(2) . ? C98 C33 1.52(2) . ? C83 C79 1.38(2) . ? C83 C84 1.41(2) . ? C52 C53 1.46(2) . ? C2 N2 1.182(18) . ? C91 C92 1.43(2) . ? C91 C90 1.45(2) . ? C42 C41 1.318(19) . ? C102 C101 1.39(2) . ? C88 C87 1.40(2) . ? C88 C89 1.43(2) . ? C99 C34 1.52(2) . ? C61 C62 1.34(2) . ? C79 C80 1.43(2) . ? C79 C78 1.45(2) . ? C94 C93 1.34(2) . ? C55 C54 1.39(2) . ? C53 C54 1.39(2) . ? C82 C81 1.45(2) . ? C87 C86 1.35(2) . ? C87 C30 1.52(2) . ? C86 C29 1.56(2) . ? C67 C66 1.40(2) . ? C67 C68 1.46(2) . ? C81 C80 1.39(2) . ? C81 C28 1.51(2) . ? C57 C20 1.51(2) . ? C65 C66 1.33(2) . ? C12 N12 1.116(17) . ? C21 C62 1.53(2) . ? C15 C44 1.49(2) . ? C31 C92 1.54(2) . ? C62 C63 1.332(19) . ? C77 C76 1.36(3) . ? C77 C78 1.37(3) . ? C104 C35 1.47(2) . ? N11 C11 1.175(19) . ? C63 C22 1.49(2) . ? C90 C89 1.33(2) . ? C70 C69 1.45(2) . ? C84 C76 1.48(3) . ? C23 C68 1.50(2) . ? C80 C27 1.52(2) . ? C74 C75 1.36(4) . ? C74 C73 1.45(4) . ? C74 C25 1.57(4) . ? C93 C92 1.37(2) . ? C93 C32 1.55(2) . ? C68 C69 1.34(2) . ? C69 C24 1.55(2) . ? C75 C76 1.42(3) . ? C75 C26 1.47(3) . ? O4S O1S 1.05(9) 4_576 ? O1S O4S 1.05(9) 4_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N7 91.1(4) . . ? N4 Co1 N13 90.9(4) . . ? N7 Co1 N13 99.5(4) . . ? N4 Co1 N16 97.1(4) . . ? N7 Co1 N16 91.8(5) . . ? N13 Co1 N16 166.0(5) . . ? N4 Co1 N14 168.8(5) . . ? N7 Co1 N14 91.4(4) . . ? N13 Co1 N14 77.9(5) . . ? N16 Co1 N14 93.7(5) . . ? N4 Co1 N15 95.3(4) . . ? N7 Co1 N15 166.4(4) . . ? N13 Co1 N15 92.3(4) . . ? N16 Co1 N15 75.5(5) . . ? N14 Co1 N15 84.6(4) . . ? N9 Co3 N6 91.0(4) . . ? N9 Co3 N23 175.2(5) . . ? N6 Co3 N23 88.3(4) . . ? N9 Co3 N21 96.3(5) . . ? N6 Co3 N21 95.4(5) . . ? N23 Co3 N21 88.4(5) . . ? N9 Co3 N24 96.0(5) . . ? N6 Co3 N24 98.0(5) . . ? N23 Co3 N24 79.4(5) . . ? N21 Co3 N24 161.6(5) . . ? N9 Co3 N22 92.8(5) . . ? N6 Co3 N22 173.0(5) . . ? N23 Co3 N22 88.4(4) . . ? N21 Co3 N22 78.4(5) . . ? N24 Co3 N22 87.4(5) . . ? N5 Co2 N18 168.5(5) . . ? N5 Co2 N8 94.9(5) . . ? N18 Co2 N8 91.9(5) . . ? N5 Co2 N20 92.5(5) . . ? N18 Co2 N20 96.5(5) . . ? N8 Co2 N20 92.3(5) . . ? N5 Co2 N19 89.8(5) . . ? N18 Co2 N19 85.0(5) . . ? N8 Co2 N19 170.0(6) . . ? N20 Co2 N19 78.6(7) . . ? N5 Co2 N17 91.0(5) . . ? N18 Co2 N17 79.5(6) . . ? N8 Co2 N17 90.9(5) . . ? N20 Co2 N17 175.0(5) . . ? N19 Co2 N17 97.9(7) . . ? C1 Fe1 C6 96.0(6) . . ? C1 Fe1 C2 88.1(7) . . ? C6 Fe1 C2 175.9(6) . . ? C1 Fe1 C3 90.4(7) . . ? C6 Fe1 C3 86.9(6) . . ? C2 Fe1 C3 92.7(6) . . ? C1 Fe1 C5 176.5(7) . . ? C6 Fe1 C5 86.2(6) . . ? C2 Fe1 C5 89.7(6) . . ? C3 Fe1 C5 92.4(6) . . ? C1 Fe1 C4 88.6(7) . . ? C6 Fe1 C4 93.9(5) . . ? C2 Fe1 C4 86.6(5) . . ? C3 Fe1 C4 178.8(6) . . ? C5 Fe1 C4 88.5(6) . . ? C7 Fe2 C8 87.1(6) . . ? C7 Fe2 C9 91.4(6) . . ? C8 Fe2 C9 88.1(6) . . ? C7 Fe2 C11 87.5(7) . . ? C8 Fe2 C11 93.7(6) . . ? C9 Fe2 C11 177.8(7) . . ? C7 Fe2 C12 175.9(7) . . ? C8 Fe2 C12 89.1(6) . . ? C9 Fe2 C12 89.9(7) . . ? C11 Fe2 C12 91.4(7) . . ? C7 Fe2 C10 94.3(7) . . ? C8 Fe2 C10 174.2(6) . . ? C9 Fe2 C10 86.2(6) . . ? C11 Fe2 C10 92.0(6) . . ? C12 Fe2 C10 89.6(7) . . ? C49 N15 C60 115.7(13) . . ? C49 N15 Co1 129.3(10) . . ? C60 N15 Co1 115.0(10) . . ? C37 N13 C48 113.5(12) . . ? C37 N13 Co1 131.7(10) . . ? C48 N13 Co1 114.8(9) . . ? C85 N21 C96 117.4(13) . . ? C85 N21 Co3 129.0(11) . . ? C96 N21 Co3 113.2(9) . . ? C4 N4 Co1 155.1(11) . . ? N4 C4 Fe1 178.8(12) . . ? C6 N6 Co3 157.4(11) . . ? C94 N22 C95 115.7(13) . . ? C94 N22 Co3 129.9(11) . . ? C95 N22 Co3 114.2(9) . . ? C9 N9 Co3 163.7(13) . . ? C7 N7 Co1 163.1(11) . . ? N5 C5 Fe1 174.3(12) . . ? C8 N8 Co2 159.6(10) . . ? C82 N20 C83 116.2(14) . . ? C82 N20 Co2 129.3(11) . . ? C83 N20 Co2 114.4(11) . . ? C58 N16 C59 115.3(13) . . ? C58 N16 Co1 127.4(11) . . ? C59 N16 Co1 117.3(10) . . ? C47 N14 C46 117.7(14) . . ? C47 N14 Co1 113.4(10) . . ? C46 N14 Co1 128.8(12) . . ? C107 N24 C106 116.2(14) . . ? C107 N24 Co3 115.1(11) . . ? C106 N24 Co3 128.6(11) . . ? N8 C8 Fe2 175.4(11) . . ? C5 N5 Co2 164.0(12) . . ? N7 C7 Fe2 174.4(13) . . ? C108 N23 C97 114.9(13) . . ? C108 N23 Co3 113.9(10) . . ? C97 N23 Co3 131.2(12) . . ? N23 C108 C100 122.7(14) . . ? N23 C108 C107 118.8(14) . . ? C100 C108 C107 118.4(17) . . ? C61 N17 C72 115.7(13) . . ? C61 N17 Co2 131.2(11) . . ? C72 N17 Co2 113.1(10) . . ? C70 N18 C71 115.8(14) . . ? C70 N18 Co2 129.2(12) . . ? C71 N18 Co2 114.6(10) . . ? N6 C6 Fe1 171.8(12) . . ? N14 C47 C48 119.8(14) . . ? N14 C47 C43 124.8(13) . . ? C48 C47 C43 115.4(14) . . ? N16 C59 C55 125.8(14) . . ? N16 C59 C60 116.2(14) . . ? C55 C59 C60 117.8(14) . . ? N16 C58 C57 126.7(14) . . ? N10 C10 Fe2 174.6(15) . . ? N15 C60 C52 122.4(14) . . ? N15 C60 C59 115.6(13) . . ? C52 C60 C59 122.0(14) . . ? N21 C96 C88 122.8(13) . . ? N21 C96 C95 117.5(13) . . ? C88 C96 C95 119.6(14) . . ? N22 C95 C91 122.2(13) . . ? N22 C95 C96 115.3(13) . . ? C91 C95 C96 122.5(14) . . ? C107 C103 C104 120.9(16) . . ? C107 C103 C102 118.4(17) . . ? C104 C103 C102 120.7(19) . . ? C38S C39 C40 119.5(14) . . ? C38S C39 C14 123.3(14) . . ? C40 C39 C14 117.1(15) . . ? N21 C85 C86 123.4(14) . . ? C84 N19 C73 123(2) . . ? C84 N19 Co2 113.4(13) . . ? C73 N19 Co2 123.5(19) . . ? N13 C48 C40 122.0(13) . . ? N13 C48 C47 114.0(14) . . ? C40 C48 C47 124.0(14) . . ? N3 C3 Fe1 175.3(14) . . ? C51 C50 C49 122.1(15) . . ? C51 C50 C17 120.3(16) . . ? C49 C50 C17 117.6(14) . . ? N13 C37 C38S 128.4(13) . . ? N15 C49 C50 123.3(14) . . ? C104 C105 C106 119.0(15) . . ? C104 C105 C36 125.0(17) . . ? C106 C105 C36 115.8(17) . . ? C50 C51 C52 116.1(15) . . ? C50 C51 C18 119.8(15) . . ? C52 C51 C18 124.1(14) . . ? N23 C97 C98 127.6(17) . . ? N9 C9 Fe2 177.6(14) . . ? C72 C64 C63 119.5(14) . . ? C72 C64 C65 116.3(16) . . ? C63 C64 C65 124.2(16) . . ? C99 C100 C108 118.4(17) . . ? C99 C100 C101 126.1(18) . . ? C108 C100 C101 115.3(16) . . ? C44 C43 C42 124.5(16) . . ? C44 C43 C47 115.4(16) . . ? C42 C43 C47 120.0(14) . . ? C55 C56 C57 121.9(14) . . ? C55 C56 C19 117.5(15) . . ? C57 C56 C19 120.5(15) . . ? C39 C40 C48 119.6(14) . . ? C39 C40 C41 125.6(16) . . ? C48 C40 C41 114.9(14) . . ? N17 C72 C64 122.2(14) . . ? N17 C72 C71 116.5(13) . . ? C64 C72 C71 121.3(15) . . ? N18 C71 C67 123.0(15) . . ? N18 C71 C72 116.0(13) . . ? C67 C71 C72 120.8(14) . . ? N1 C1 Fe1 177.2(16) . . ? C44 C45 C46 117.6(14) . . ? C44 C45 C16 125.7(17) . . ? C46 C45 C16 116.7(18) . . ? C103 C107 N24 123.3(15) . . ? C103 C107 C108 123.9(16) . . ? N24 C107 C108 112.7(16) . . ? C39 C38S C37 117.0(13) . . ? C39 C38S C13 123.9(14) . . ? C37 C38S C13 119.1(13) . . ? N14 C46 C45 123.7(17) . . ? C97 C98 C99 117.9(16) . . ? C97 C98 C33 119.6(19) . . ? C99 C98 C33 122.4(16) . . ? N20 C83 C79 123.7(16) . . ? N20 C83 C84 115.0(18) . . ? C79 C83 C84 121.2(19) . . ? C51 C52 C60 120.2(14) . . ? C51 C52 C53 122.8(16) . . ? C60 C52 C53 117.0(15) . . ? N2 C2 Fe1 178.1(12) . . ? C95 C91 C92 118.9(15) . . ? C95 C91 C90 116.4(14) . . ? C92 C91 C90 124.7(16) . . ? C41 C42 C43 121.0(15) . . ? C101 C102 C103 118.9(17) . . ? C87 C88 C96 117.0(14) . . ? C87 C88 C89 126.1(15) . . ? C96 C88 C89 116.8(15) . . ? C98 C99 C100 118.4(16) . . ? C98 C99 C34 122.0(18) . . ? C100 C99 C34 120(2) . . ? N17 C61 C62 125.5(15) . . ? C83 C79 C80 119.9(17) . . ? C83 C79 C78 118(2) . . ? C80 C79 C78 122(2) . . ? N22 C94 C93 128.2(15) . . ? C56 C55 C54 124.4(15) . . ? C56 C55 C59 114.7(14) . . ? C54 C55 C59 120.9(15) . . ? C54 C53 C52 121.4(16) . . ? N20 C82 C81 126.4(15) . . ? C86 C87 C88 120.5(14) . . ? C86 C87 C30 119.3(15) . . ? C88 C87 C30 120.0(15) . . ? C87 C86 C85 118.5(15) . . ? C87 C86 C29 124.2(14) . . ? C85 C86 C29 117.1(14) . . ? C71 C67 C66 117.6(16) . . ? C71 C67 C68 118.5(15) . . ? C66 C67 C68 123.9(16) . . ? N24 C106 C105 123.7(15) . . ? C80 C81 C82 116.9(16) . . ? C80 C81 C28 124.1(17) . . ? C82 C81 C28 118.9(16) . . ? C58 C57 C56 115.4(15) . . ? C58 C57 C20 120.1(14) . . ? C56 C57 C20 124.5(14) . . ? C66 C65 C64 121.1(16) . . ? N12 C12 Fe2 179.0(18) . . ? C42 C41 C40 124.8(16) . . ? C63 C62 C61 122.0(15) . . ? C63 C62 C21 120.6(14) . . ? C61 C62 C21 117.4(14) . . ? C53 C54 C55 120.8(15) . . ? C76 C77 C78 126(2) . . ? C105 C104 C103 116.6(16) . . ? C105 C104 C35 119.2(18) . . ? C103 C104 C35 124.2(17) . . ? C62 C63 C64 115.0(14) . . ? C62 C63 C22 123.2(16) . . ? C64 C63 C22 121.7(15) . . ? C43 C44 C45 120.6(16) . . ? C43 C44 C15 120.1(18) . . ? C45 C44 C15 119.2(16) . . ? C89 C90 C91 120.6(16) . . ? N18 C70 C69 128.2(17) . . ? N19 C84 C83 118.2(18) . . ? N19 C84 C76 121(2) . . ? C83 C84 C76 121(2) . . ? C81 C80 C79 116.8(17) . . ? C81 C80 C27 118.4(19) . . ? C79 C80 C27 124.7(18) . . ? C102 C101 C100 124.6(16) . . ? C75 C74 C73 123(3) . . ? C75 C74 C25 124(3) . . ? C73 C74 C25 113(3) . . ? C94 C93 C92 117.4(15) . . ? C94 C93 C32 124.9(16) . . ? C92 C93 C32 117.7(16) . . ? C77 C78 C79 119(2) . . ? N11 C11 Fe2 177.5(17) . . ? C69 C68 C67 115.6(16) . . ? C69 C68 C23 125.3(16) . . ? C67 C68 C23 119.0(16) . . ? C90 C89 C88 123.7(16) . . ? C93 C92 C91 117.4(14) . . ? C93 C92 C31 122.6(16) . . ? C91 C92 C31 119.8(17) . . ? C68 C69 C70 118.6(16) . . ? C68 C69 C24 117.9(18) . . ? C70 C69 C24 123.5(18) . . ? N19 C73 C74 116(2) . . ? C74 C75 C76 119(3) . . ? C74 C75 C26 120(3) . . ? C76 C75 C26 121(3) . . ? C65 C66 C67 122.7(16) . . ? C77 C76 C75 128(3) . . ? C77 C76 C84 115(2) . . ? C75 C76 C84 118(3) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.007 _refine_diff_density_min -1.090 _refine_diff_density_rms 0.261 #end=========================== data_{[Co(tmphen)2]3[Fe(CN)6]2}_170K #=========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; '((Co(tmphen)2)3(Fe(CN)6)2).7H2O' ; _chemical_name_common '((Co(tmphen)2)3(Fe(CN)6)2).7H2O' _chemical_melting_point ? _chemical_formula_moiety 'C108 H110 Co3 Fe2 N24 O7' _chemical_formula_sum 'C108 H110 Co3 Fe2 N24 O7' _chemical_formula_weight 2144.7 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.090(19) _cell_length_b 25.21(3) _cell_length_c 24.69(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.67(4) _cell_angle_gamma 90.00 _cell_volume 11779(21) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12281 _cell_measurement_theta_min '2.2575' _cell_measurement_theta_max '17.3805' _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4404 _exptl_absorpt_coefficient_mu 0.713 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8764 _exptl_absorpt_correction_T_max 0.9193 _exptl_absorpt_process_details 'SADABS: Bruker,2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER APEX' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56523 _diffrn_reflns_av_R_equivalents 0.1651 _diffrn_reflns_av_sigmaI/netI 0.1124 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 20.81 _reflns_number_total 12281 _reflns_number_gt 7666 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER, 2000)' _computing_cell_refinement 'SAINT (BRUKER, 2001)' _computing_data_reduction 'SAINT (BRUKER, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1976P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0037(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12281 _refine_ls_number_parameters 1335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1344 _refine_ls_R_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.2941 _refine_ls_wR_factor_gt 0.2664 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.06086(7) 0.37140(5) 0.61565(5) 0.0424(5) Uani 1 1 d . A -1 Co2 Co 0.29261(7) 0.36719(5) 0.83115(5) 0.0441(5) Uani 1 1 d . A -1 Co3 Co 0.35634(7) 0.54553(5) 0.66388(6) 0.0416(5) Uani 1 1 d . A -1 Fe1 Fe 0.32359(7) 0.34984(6) 0.63439(6) 0.0466(5) Uani 1 1 d . A -1 Fe2 Fe 0.13813(8) 0.51603(6) 0.75289(6) 0.0492(5) Uani 1 1 d . A -1 O1S O 0.233(4) 0.714(3) 0.324(3) 0.22(3) Uiso 0.25 1 d P B -1 O2S O 0.230(2) 0.8195(14) 0.5926(15) 0.095(11) Uiso 0.25 1 d P C -2 O4S O 0.636(2) 0.3787(14) 0.6783(15) 0.092(11) Uiso 0.25 1 d P D -4 O5S O 0.631(2) 0.3237(17) 0.6610(17) 0.113(13) Uiso 0.25 1 d P E -5 O6S O -0.280(2) 0.1618(16) 0.5570(17) 0.115(14) Uiso 0.25 1 d P F -6 O7S O -0.247(2) 0.1730(16) 0.7273(17) 0.097(12) Uiso 0.25 1 d P G -7 O8S O 0.3096(18) 0.1777(13) 0.7647(14) 0.083(10) Uiso 0.25 1 d P H -8 O9S O -0.145(2) 0.4603(14) 0.7666(14) 0.218(14) Uiso 0.50 1 d P I -9 O10S O -0.285(3) 0.590(2) 0.704(2) 0.140(17) Uiso 0.25 1 d P J -10 O11S O -0.240(3) 0.558(2) 0.729(2) 0.143(17) Uiso 0.25 1 d P K -11 O12S O -0.0781(18) 0.5785(13) 0.8650(13) 0.201(13) Uiso 0.50 1 d P L -12 O13S O 0.6973(12) 0.4793(8) 1.0104(9) 0.120(7) Uiso 0.50 1 d P M -13 O14S O 0.1178(13) 0.4816(10) 0.9224(10) 0.137(8) Uiso 0.50 1 d P N -14 O15S O 0.0865(15) 0.4457(11) 0.9579(12) 0.150(9) Uiso 0.50 1 d P O -15 O16S O 0.5550(19) 0.2968(12) 1.0799(13) 0.181(12) Uiso 0.50 1 d P P -16 O17S O 0.265(3) 0.806(2) 0.305(3) 0.17(2) Uiso 0.25 1 d P Q -17 O18S O 0.4286(18) 0.2716(12) 1.0452(13) 0.183(11) Uiso 0.50 1 d P R -18 O19S O 0.493(2) 0.2946(12) 1.0680(13) 0.177(11) Uiso 0.50 1 d P S -19 O30S O 0.0697(15) 0.0869(11) 0.4926(12) 0.160(10) Uiso 0.50 1 d P T -30 N1 N 0.3103(5) 0.3253(4) 0.5122(5) 0.078(3) Uani 1 1 d . A -1 N2 N 0.3217(5) 0.2291(4) 0.6552(4) 0.071(3) Uani 1 1 d . A -1 N3 N 0.4868(6) 0.3553(4) 0.6392(5) 0.080(3) Uani 1 1 d . A -1 N4 N 0.1623(5) 0.3441(3) 0.6266(3) 0.046(2) Uani 1 1 d . A -1 N5 N 0.3247(4) 0.3667(3) 0.7572(4) 0.047(2) Uani 1 1 d . A -1 N6 N 0.3299(4) 0.4727(4) 0.6312(4) 0.053(2) Uani 1 1 d . A -1 N7 N 0.0924(4) 0.4411(4) 0.6579(4) 0.046(2) Uani 1 1 d . A -1 N8 N 0.2139(4) 0.4198(4) 0.8098(3) 0.046(2) Uani 1 1 d . A -1 N9 N 0.2770(5) 0.5413(3) 0.7098(3) 0.047(2) Uani 1 1 d . A -1 N10 N 0.0839(6) 0.6191(4) 0.6933(4) 0.073(3) Uani 1 1 d . A -1 N11 N -0.0051(7) 0.4916(5) 0.7897(5) 0.102(4) Uani 1 1 d . A -1 N12 N 0.1826(7) 0.5805(4) 0.8560(5) 0.087(4) Uani 1 1 d . A -1 N13 N 0.0722(4) 0.3959(3) 0.5349(3) 0.047(2) Uani 1 1 d . A -1 N14 N -0.0397(4) 0.4050(3) 0.5877(4) 0.051(2) Uani 1 1 d . A -1 N15 N 0.0147(4) 0.2970(3) 0.5882(3) 0.042(2) Uani 1 1 d . A -1 N16 N 0.0290(4) 0.3370(3) 0.6875(3) 0.043(2) Uani 1 1 d . A -1 N17 N 0.2253(4) 0.3036(3) 0.8107(3) 0.042(2) Uani 1 1 d . A -1 N18 N 0.2577(5) 0.3514(4) 0.9061(4) 0.055(2) Uani 1 1 d . A -1 N19 N 0.3812(6) 0.3237(4) 0.8623(4) 0.072(3) Uani 1 1 d . A -1 N20 N 0.3619(5) 0.4272(4) 0.8594(4) 0.053(2) Uani 1 1 d . A -1 N21 N 0.4357(4) 0.5172(3) 0.7228(3) 0.041(2) Uani 1 1 d . A -1 N22 N 0.3973(5) 0.6173(3) 0.7011(4) 0.050(2) Uani 1 1 d . A -1 N23 N 0.4297(5) 0.5534(3) 0.6094(4) 0.049(2) Uani 1 1 d . A -1 N24 N 0.3012(5) 0.5928(3) 0.6032(4) 0.055(2) Uani 1 1 d . A -1 C1 C 0.3165(6) 0.3360(4) 0.5578(6) 0.056(3) Uani 1 1 d . A -1 C2 C 0.3232(5) 0.2748(5) 0.6463(5) 0.057(3) Uani 1 1 d . A -1 C3 C 0.4251(7) 0.3520(4) 0.6376(5) 0.056(3) Uani 1 1 d . A -1 C4 C 0.2222(7) 0.3469(4) 0.6305(4) 0.045(3) Uani 1 1 d . A -1 C5 C 0.3270(5) 0.3605(4) 0.7108(5) 0.041(3) Uani 1 1 d . A -1 C6 C 0.3255(5) 0.4266(5) 0.6282(4) 0.040(3) Uani 1 1 d . A -1 C7 C 0.1111(5) 0.4713(4) 0.6916(5) 0.044(3) Uani 1 1 d . A -1 C8 C 0.1821(6) 0.4549(4) 0.7888(4) 0.046(3) Uani 1 1 d . A -1 C9 C 0.2245(6) 0.5311(4) 0.7270(4) 0.046(3) Uani 1 1 d . A -1 C10 C 0.1021(6) 0.5794(5) 0.7155(5) 0.054(3) Uani 1 1 d . A -1 C11 C 0.0482(7) 0.5017(5) 0.7767(5) 0.068(4) Uani 1 1 d . A -1 C12 C 0.1652(7) 0.5564(5) 0.8164(5) 0.069(4) Uani 1 1 d . A -1 C13 C 0.4928(6) 0.5336(4) 0.6118(5) 0.058(3) Uani 1 1 d . A -1 H13 H 0.5098 0.5142 0.6439 0.070 Uiso 1 1 calc R . . C14 C 0.5376(7) 0.5376(5) 0.5727(7) 0.074(4) Uani 1 1 d . A -1 C15 C 0.5169(7) 0.5666(6) 0.5260(6) 0.072(4) Uani 1 1 d . A -1 C16 C 0.4506(8) 0.5905(5) 0.5221(5) 0.066(4) Uani 1 1 d . A -1 C17 C 0.4200(9) 0.6242(6) 0.4778(6) 0.083(4) Uani 1 1 d . A -1 H17 H 0.4460 0.6310 0.4483 0.099 Uiso 1 1 calc R . . C18 C 0.3522(9) 0.6474(5) 0.4771(5) 0.083(4) Uani 1 1 d . A -1 H18 H 0.3337 0.6687 0.4469 0.099 Uiso 1 1 calc R . . C19 C 0.3117(7) 0.6397(5) 0.5197(5) 0.065(3) Uani 1 1 d . A -1 C20 C 0.2424(8) 0.6624(5) 0.5206(5) 0.072(4) Uani 1 1 d . A -1 C21 C 0.2060(6) 0.6490(5) 0.5637(6) 0.065(3) Uani 1 1 d . A -1 C22 C 0.2365(6) 0.6142(4) 0.6027(5) 0.058(3) Uani 1 1 d . A -1 H22 H 0.2101 0.6044 0.6311 0.070 Uiso 1 1 calc R . . C23 C 0.3382(6) 0.6059(5) 0.5617(5) 0.057(3) Uani 1 1 d . A -1 C24 C 0.4070(6) 0.5822(5) 0.5656(5) 0.057(3) Uani 1 1 d . A -1 C25 C 0.6093(7) 0.5132(6) 0.5810(7) 0.108(5) Uani 1 1 d . A -1 H25A H 0.6233 0.5036 0.5455 0.163 Uiso 1 1 calc R . . H25B H 0.6085 0.4813 0.6036 0.163 Uiso 1 1 calc R . . H25C H 0.6433 0.5387 0.5994 0.163 Uiso 1 1 calc R . . C26 C 0.5627(8) 0.5745(6) 0.4827(6) 0.112(6) Uani 1 1 d . A -1 H26A H 0.5890 0.6077 0.4892 0.168 Uiso 1 1 calc R . . H26B H 0.5333 0.5760 0.4470 0.168 Uiso 1 1 calc R . . H26C H 0.5960 0.5448 0.4831 0.168 Uiso 1 1 calc R . . C27 C 0.2118(8) 0.6995(6) 0.4763(6) 0.105(5) Uani 1 1 d . A -1 H27A H 0.1702 0.6832 0.4553 0.157 Uiso 1 1 calc R . . H27B H 0.2473 0.7070 0.4520 0.157 Uiso 1 1 calc R . . H27C H 0.1980 0.7327 0.4927 0.157 Uiso 1 1 calc R . . C28 C 0.1348(6) 0.6732(5) 0.5709(5) 0.077(4) Uani 1 1 d . A -1 H28A H 0.1193 0.6595 0.6044 0.116 Uiso 1 1 calc R . . H28B H 0.1000 0.6637 0.5395 0.116 Uiso 1 1 calc R . . H28C H 0.1392 0.7118 0.5733 0.116 Uiso 1 1 calc R . . C29 C 0.3752(6) 0.6678(4) 0.6907(5) 0.067(3) Uani 1 1 d . A -1 H29 H 0.3332 0.6734 0.6661 0.081 Uiso 1 1 calc R . . C30 C 0.4102(7) 0.7109(4) 0.7139(6) 0.080(4) Uani 1 1 d . A -1 C31 C 0.4726(7) 0.7057(5) 0.7466(6) 0.088(5) Uani 1 1 d . A -1 C32 C 0.4967(7) 0.6527(5) 0.7591(5) 0.071(4) Uani 1 1 d . A -1 C33 C 0.5614(7) 0.6413(5) 0.7940(6) 0.091(5) Uani 1 1 d . A -1 H33 H 0.5894 0.6695 0.8107 0.109 Uiso 1 1 calc R . . C34 C 0.5823(7) 0.5912(5) 0.8029(5) 0.080(4) Uani 1 1 d . A -1 H34 H 0.6261 0.5850 0.8252 0.096 Uiso 1 1 calc R . . C35 C 0.5418(6) 0.5453(4) 0.7803(5) 0.059(3) Uani 1 1 d . A -1 C36 C 0.5610(6) 0.4917(5) 0.7906(5) 0.067(3) Uani 1 1 d . A -1 C37 C 0.5159(6) 0.4536(4) 0.7679(5) 0.057(3) Uani 1 1 d . A -1 C38 C 0.4534(6) 0.4684(4) 0.7349(4) 0.047(3) Uani 1 1 d . A -1 H38 H 0.4220 0.4410 0.7206 0.057 Uiso 1 1 calc R . . C39 C 0.4791(5) 0.5568(4) 0.7465(4) 0.048(3) Uani 1 1 d . A -1 C40 C 0.4576(6) 0.6108(4) 0.7352(4) 0.048(3) Uani 1 1 d . A -1 C41 C 0.3809(9) 0.7665(5) 0.6963(7) 0.125(7) Uani 1 1 d . A -1 H41A H 0.3670 0.7851 0.7280 0.187 Uiso 1 1 calc R . . H41B H 0.3397 0.7626 0.6683 0.187 Uiso 1 1 calc R . . H41C H 0.4175 0.7869 0.6813 0.187 Uiso 1 1 calc R . . C42 C 0.5128(9) 0.7524(5) 0.7714(7) 0.138(8) Uani 1 1 d . A -1 H42A H 0.5276 0.7746 0.7423 0.206 Uiso 1 1 calc R . . H42B H 0.5546 0.7402 0.7955 0.206 Uiso 1 1 calc R . . H42C H 0.4826 0.7732 0.7926 0.206 Uiso 1 1 calc R . . C43 C 0.6295(7) 0.4773(6) 0.8249(7) 0.112(6) Uani 1 1 d . A -1 H43A H 0.6198 0.4549 0.8555 0.168 Uiso 1 1 calc R . . H43B H 0.6538 0.5097 0.8391 0.168 Uiso 1 1 calc R . . H43C H 0.6595 0.4579 0.8025 0.168 Uiso 1 1 calc R . . C44 C 0.5302(7) 0.3939(4) 0.7761(5) 0.085(4) Uani 1 1 d . A -1 H44A H 0.5668 0.3828 0.7541 0.127 Uiso 1 1 calc R . . H44B H 0.4867 0.3740 0.7645 0.127 Uiso 1 1 calc R . . H44C H 0.5463 0.3868 0.8148 0.127 Uiso 1 1 calc R . . C45 C 0.1271(5) 0.3911(4) 0.5060(4) 0.045(3) Uani 1 1 d . A -1 H45 H 0.1689 0.3749 0.5239 0.054 Uiso 1 1 calc R . . C46 C 0.1282(6) 0.4075(4) 0.4525(4) 0.051(3) Uani 1 1 d . A -1 C47 C 0.0691(7) 0.4312(4) 0.4257(5) 0.059(3) Uani 1 1 d . A -1 C48 C 0.0091(6) 0.4373(4) 0.4529(5) 0.051(3) Uani 1 1 d . A -1 C49 C -0.0557(6) 0.4617(4) 0.4294(5) 0.056(3) Uani 1 1 d . A -1 H49 H -0.0595 0.4745 0.3929 0.068 Uiso 1 1 calc R . . C50 C -0.1096(6) 0.4669(4) 0.4563(5) 0.054(3) Uani 1 1 d . A -1 H50 H -0.1510 0.4840 0.4388 0.064 Uiso 1 1 calc R . . C51 C -0.1091(6) 0.4482(4) 0.5102(5) 0.052(3) Uani 1 1 d . A -1 C52 C -0.1657(7) 0.4521(5) 0.5389(6) 0.071(4) Uani 1 1 d . A -1 C53 C -0.1609(6) 0.4318(5) 0.5911(6) 0.072(4) Uani 1 1 d . A -1 C54 C -0.0956(6) 0.4090(5) 0.6142(5) 0.069(4) Uani 1 1 d . A -1 H54 H -0.0916 0.3960 0.6506 0.083 Uiso 1 1 calc R . . C55 C -0.0472(5) 0.4241(4) 0.5372(5) 0.047(3) Uani 1 1 d . A -1 C56 C 0.0128(6) 0.4193(4) 0.5080(5) 0.050(3) Uani 1 1 d . A -1 C57 C 0.1954(6) 0.3993(5) 0.4282(5) 0.074(4) Uani 1 1 d . A -1 H57A H 0.2313 0.3838 0.4557 0.111 Uiso 1 1 calc R . . H57B H 0.2122 0.4335 0.4161 0.111 Uiso 1 1 calc R . . H57C H 0.1865 0.3752 0.3969 0.111 Uiso 1 1 calc R . . C58 C 0.0640(7) 0.4519(4) 0.3675(5) 0.072(4) Uani 1 1 d . A -1 H58A H 0.1065 0.4417 0.3517 0.108 Uiso 1 1 calc R . . H58B H 0.0599 0.4906 0.3676 0.108 Uiso 1 1 calc R . . H58C H 0.0222 0.4367 0.3455 0.108 Uiso 1 1 calc R . . C60 C -0.2181(7) 0.4338(7) 0.6300(6) 0.111(6) Uani 1 1 d . A -1 H60A H -0.2258 0.4707 0.6402 0.167 Uiso 1 1 calc R . . H60B H -0.2024 0.4130 0.6629 0.167 Uiso 1 1 calc R . . H60C H -0.2624 0.4189 0.6114 0.167 Uiso 1 1 calc R . . C61 C 0.0070(5) 0.2758(4) 0.5380(4) 0.049(3) Uani 1 1 d . A -1 H61 H 0.0248 0.2954 0.5099 0.058 Uiso 1 1 calc R . . C62 C -0.0250(6) 0.2271(5) 0.5237(4) 0.050(3) Uani 1 1 d . A -1 C63 C -0.0528(5) 0.1980(4) 0.5629(4) 0.052(3) Uani 1 1 d . A -1 C64 C -0.0478(5) 0.2192(4) 0.6159(4) 0.048(3) Uani 1 1 d . A -1 C65 C -0.0759(6) 0.1933(5) 0.6602(5) 0.068(4) Uani 1 1 d . A -1 H65 H -0.0998 0.1604 0.6540 0.082 Uiso 1 1 calc R . . C66 C -0.0685(7) 0.2155(5) 0.7110(4) 0.066(4) Uani 1 1 d . A -1 H66 H -0.0877 0.1974 0.7394 0.079 Uiso 1 1 calc R . . C67 C -0.0329(5) 0.2650(4) 0.7230(4) 0.046(3) Uani 1 1 d . A -1 C68 C -0.0227(6) 0.2868(4) 0.7744(4) 0.057(3) Uani 1 1 d . A -1 C69 C 0.0149(6) 0.3340(5) 0.7834(4) 0.055(3) Uani 1 1 d . A -1 C70 C 0.0401(5) 0.3569(4) 0.7378(5) 0.051(3) Uani 1 1 d . A -1 H70 H 0.0668 0.3887 0.7433 0.061 Uiso 1 1 calc R . . C71 C -0.0065(5) 0.2903(4) 0.6804(4) 0.043(3) Uani 1 1 d . A -1 C72 C -0.0133(5) 0.2680(4) 0.6264(4) 0.042(3) Uani 1 1 d . A -1 C73 C -0.0267(6) 0.2077(5) 0.4659(4) 0.062(3) Uani 1 1 d . A -1 H73A H -0.0059 0.1721 0.4662 0.093 Uiso 1 1 calc R . . H73B H 0.0004 0.2320 0.4457 0.093 Uiso 1 1 calc R . . H73C H -0.0758 0.2063 0.4482 0.093 Uiso 1 1 calc R . . C74 C -0.0888(7) 0.1469(5) 0.5480(5) 0.078(4) Uani 1 1 d . A -1 H74A H -0.1395 0.1531 0.5375 0.116 Uiso 1 1 calc R . . H74B H -0.0819 0.1228 0.5794 0.116 Uiso 1 1 calc R . . H74C H -0.0688 0.1309 0.5173 0.116 Uiso 1 1 calc R . . C75 C -0.0547(7) 0.2617(5) 0.8224(4) 0.075(4) Uani 1 1 d . A -1 H75A H -0.0286 0.2740 0.8570 0.113 Uiso 1 1 calc R . . H75B H -0.0515 0.2230 0.8202 0.113 Uiso 1 1 calc R . . H75C H -0.1044 0.2722 0.8205 0.113 Uiso 1 1 calc R . . C76 C 0.0310(6) 0.3614(4) 0.8375(4) 0.061(3) Uani 1 1 d . A -1 H76A H -0.0129 0.3753 0.8486 0.092 Uiso 1 1 calc R . . H76B H 0.0639 0.3907 0.8344 0.092 Uiso 1 1 calc R . . H76C H 0.0524 0.3360 0.8650 0.092 Uiso 1 1 calc R . . C77 C 0.2079(5) 0.2814(4) 0.7630(4) 0.052(3) Uani 1 1 d . A -1 H77 H 0.2266 0.2964 0.7327 0.062 Uiso 1 1 calc R . . C78 C 0.1642(6) 0.2375(4) 0.7533(4) 0.050(3) Uani 1 1 d . A -1 C79 C 0.1348(6) 0.2155(4) 0.7959(5) 0.056(3) Uani 1 1 d . A -1 C80 C 0.1507(5) 0.2396(4) 0.8475(5) 0.054(3) Uani 1 1 d . A -1 C81 C 0.1244(6) 0.2219(5) 0.8968(6) 0.065(3) Uani 1 1 d . A -1 H81 H 0.0913 0.1936 0.8942 0.078 Uiso 1 1 calc R . . C82 C 0.1445(7) 0.2436(5) 0.9459(5) 0.067(3) Uani 1 1 d . A -1 H82 H 0.1280 0.2288 0.9773 0.081 Uiso 1 1 calc R . . C83 C 0.1902(6) 0.2886(5) 0.9519(5) 0.060(3) Uani 1 1 d . A -1 C84 C 0.2112(7) 0.3158(6) 1.0023(5) 0.076(4) Uani 1 1 d . A -1 C85 C 0.2562(7) 0.3581(6) 1.0020(5) 0.080(4) Uani 1 1 d . A -1 C86 C 0.2759(7) 0.3736(5) 0.9524(6) 0.073(4) Uani 1 1 d . A -1 H86 H 0.3059 0.4037 0.9528 0.088 Uiso 1 1 calc R . . C87 C 0.2153(6) 0.3090(5) 0.9051(4) 0.048(3) Uani 1 1 d . A -1 C88 C 0.1957(5) 0.2832(4) 0.8537(4) 0.045(3) Uani 1 1 d . A -1 C89 C 0.1510(6) 0.2153(5) 0.6967(5) 0.073(4) Uani 1 1 d . A -1 H89A H 0.1753 0.1812 0.6956 0.109 Uiso 1 1 calc R . . H89B H 0.1689 0.2401 0.6712 0.109 Uiso 1 1 calc R . . H89C H 0.1001 0.2102 0.6863 0.109 Uiso 1 1 calc R . . C90 C 0.0869(7) 0.1682(5) 0.7879(5) 0.076(4) Uani 1 1 d . A -1 H90A H 0.0647 0.1668 0.7498 0.113 Uiso 1 1 calc R . . H90B H 0.0503 0.1711 0.8120 0.113 Uiso 1 1 calc R . . H90C H 0.1144 0.1358 0.7967 0.113 Uiso 1 1 calc R . . C91 C 0.1848(7) 0.2957(6) 1.0535(5) 0.097(5) Uani 1 1 d . A -1 H91A H 0.2028 0.3185 1.0844 0.146 Uiso 1 1 calc R . . H91B H 0.2014 0.2594 1.0609 0.146 Uiso 1 1 calc R . . H91C H 0.1330 0.2963 1.0485 0.146 Uiso 1 1 calc R . . C92 C 0.2819(8) 0.3872(7) 1.0547(6) 0.119(6) Uani 1 1 d . A -1 H92A H 0.2421 0.3933 1.0751 0.179 Uiso 1 1 calc R . . H92B H 0.3025 0.4213 1.0461 0.179 Uiso 1 1 calc R . . H92C H 0.3179 0.3658 1.0768 0.179 Uiso 1 1 calc R . . C93 C 0.3882(10) 0.2711(6) 0.8630(6) 0.105(5) Uani 1 1 d . A -1 H93 H 0.3507 0.2495 0.8462 0.126 Uiso 1 1 calc R . . C94 C 0.4536(14) 0.2459(7) 0.8897(8) 0.133(8) Uani 1 1 d . A -1 C95 C 0.5084(13) 0.2766(10) 0.9137(8) 0.135(8) Uani 1 1 d . A -1 C96 C 0.5006(11) 0.3326(8) 0.9141(7) 0.116(6) Uani 1 1 d . A -1 C97 C 0.5504(10) 0.3686(9) 0.9385(7) 0.123(7) Uani 1 1 d . A -1 H97 H 0.5940 0.3553 0.9565 0.148 Uiso 1 1 calc R . . C98 C 0.5398(8) 0.4187(8) 0.9379(7) 0.113(6) Uani 1 1 d . A -1 H98 H 0.5748 0.4409 0.9572 0.135 Uiso 1 1 calc R . . C99 C 0.4769(7) 0.4429(6) 0.9091(5) 0.076(4) Uani 1 1 d . A -1 C100 C 0.4659(8) 0.4991(6) 0.9052(5) 0.086(4) Uani 1 1 d . A -1 C101 C 0.4024(7) 0.5166(5) 0.8755(5) 0.071(4) Uani 1 1 d . A -1 C102 C 0.3526(6) 0.4783(5) 0.8545(5) 0.060(3) Uani 1 1 d . A -1 H102 H 0.3091 0.4904 0.8353 0.073 Uiso 1 1 calc R . . C103 C 0.4241(7) 0.4102(5) 0.8847(5) 0.063(3) Uani 1 1 d . A -1 C104 C 0.4346(8) 0.3541(6) 0.8868(5) 0.078(4) Uani 1 1 d . A -1 C105 C 0.4499(13) 0.1844(6) 0.8865(8) 0.190(11) Uani 1 1 d . A -1 H10G H 0.4734 0.1720 0.8560 0.284 Uiso 1 1 calc R . . H10H H 0.4003 0.1732 0.8809 0.284 Uiso 1 1 calc R . . H10I H 0.4735 0.1693 0.9207 0.284 Uiso 1 1 calc R . . C106 C 0.5740(13) 0.2494(8) 0.9409(8) 0.197(12) Uani 1 1 d . A -1 H10J H 0.5783 0.2550 0.9804 0.295 Uiso 1 1 calc R . . H10K H 0.6155 0.2641 0.9268 0.295 Uiso 1 1 calc R . . H10L H 0.5708 0.2113 0.9330 0.295 Uiso 1 1 calc R . . C107 C 0.5190(8) 0.5389(6) 0.9316(7) 0.113(6) Uani 1 1 d . A -1 H10D H 0.5320 0.5634 0.9038 0.169 Uiso 1 1 calc R . . H10E H 0.5614 0.5202 0.9486 0.169 Uiso 1 1 calc R . . H10F H 0.4983 0.5588 0.9596 0.169 Uiso 1 1 calc R . . C108 C 0.3852(7) 0.5747(5) 0.8670(6) 0.088(4) Uani 1 1 d . A -1 H10A H 0.3814 0.5914 0.9023 0.132 Uiso 1 1 calc R . . H10B H 0.3402 0.5784 0.8431 0.132 Uiso 1 1 calc R . . H10C H 0.4228 0.5920 0.8501 0.132 Uiso 1 1 calc R . . C3S C -0.2359(6) 0.4790(5) 0.5160(6) 0.088(4) Uani 1 1 d . A -1 H59A H -0.2262 0.5138 0.5010 0.132 Uiso 1 1 calc R . . H59B H -0.2653 0.4834 0.5453 0.132 Uiso 1 1 calc R . . H59C H -0.2609 0.4569 0.4870 0.132 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0275(8) 0.0620(10) 0.0388(9) 0.0096(7) 0.0082(7) -0.0016(7) Co2 0.0480(10) 0.0448(9) 0.0400(9) 0.0064(6) 0.0075(7) -0.0005(7) Co3 0.0331(9) 0.0406(9) 0.0534(10) 0.0031(7) 0.0141(7) -0.0016(6) Fe1 0.0351(10) 0.0533(10) 0.0518(10) 0.0086(7) 0.0077(8) 0.0006(7) Fe2 0.0527(11) 0.0538(10) 0.0447(10) 0.0035(7) 0.0191(8) 0.0115(8) N1 0.066(7) 0.098(9) 0.069(8) 0.019(7) 0.002(6) -0.007(6) N2 0.047(6) 0.067(7) 0.097(8) 0.021(6) 0.004(6) 0.007(5) N3 0.039(7) 0.098(8) 0.102(9) 0.002(6) 0.013(6) 0.007(6) N4 0.033(6) 0.064(6) 0.039(5) 0.013(4) 0.005(4) -0.001(5) N5 0.043(6) 0.052(6) 0.045(6) 0.008(5) 0.002(5) 0.002(4) N6 0.038(6) 0.062(7) 0.063(6) 0.008(5) 0.026(5) 0.004(5) N7 0.029(5) 0.061(6) 0.049(6) 0.030(5) 0.008(5) 0.006(4) N8 0.042(6) 0.050(6) 0.049(6) 0.010(5) 0.015(5) 0.003(5) N9 0.048(6) 0.044(5) 0.048(6) -0.004(4) 0.007(5) 0.003(4) N10 0.090(8) 0.070(7) 0.061(7) 0.000(6) 0.016(6) 0.028(6) N11 0.081(9) 0.125(10) 0.112(10) 0.030(8) 0.058(8) 0.031(8) N12 0.129(11) 0.073(8) 0.063(8) 0.006(6) 0.029(7) 0.026(7) N13 0.026(5) 0.054(6) 0.059(6) 0.010(5) -0.003(5) -0.005(4) N14 0.028(6) 0.064(6) 0.062(7) -0.005(5) 0.012(5) -0.004(4) N15 0.031(5) 0.068(6) 0.028(5) 0.002(5) 0.013(4) 0.004(4) N16 0.038(5) 0.067(6) 0.024(5) 0.000(4) 0.005(4) -0.003(5) N17 0.033(5) 0.056(5) 0.038(6) 0.002(5) 0.007(4) -0.006(4) N18 0.066(7) 0.067(6) 0.034(6) -0.009(5) 0.009(5) -0.016(5) N19 0.114(10) 0.050(7) 0.056(7) 0.011(5) 0.024(7) 0.026(7) N20 0.060(7) 0.049(6) 0.051(6) 0.005(5) 0.011(5) 0.003(5) N21 0.030(5) 0.041(6) 0.054(6) 0.006(4) 0.015(4) -0.001(4) N22 0.040(6) 0.046(6) 0.064(6) 0.006(5) 0.007(5) -0.001(4) N23 0.027(6) 0.058(6) 0.065(7) -0.003(5) 0.018(5) -0.004(4) N24 0.036(6) 0.061(6) 0.067(7) -0.003(5) 0.004(5) 0.000(5) C1 0.057(8) 0.057(7) 0.055(8) 0.006(6) 0.005(7) -0.002(6) C2 0.021(6) 0.080(9) 0.070(8) 0.013(7) 0.004(6) 0.002(6) C3 0.064(9) 0.046(7) 0.060(8) 0.010(5) 0.013(7) 0.000(6) C4 0.051(8) 0.050(7) 0.035(7) 0.006(5) 0.009(6) -0.002(6) C5 0.035(6) 0.039(6) 0.047(8) 0.008(5) -0.003(6) -0.002(5) C6 0.022(6) 0.060(8) 0.038(6) 0.003(6) 0.003(5) 0.002(5) C7 0.036(7) 0.056(7) 0.041(7) 0.011(6) 0.016(6) 0.005(6) C8 0.041(7) 0.054(7) 0.048(7) -0.004(6) 0.019(6) -0.002(6) C9 0.053(8) 0.046(7) 0.039(7) -0.001(5) 0.010(6) 0.004(6) C10 0.052(7) 0.060(8) 0.052(8) -0.008(6) 0.017(6) 0.012(6) C11 0.052(8) 0.103(10) 0.057(8) 0.019(7) 0.032(7) 0.025(7) C12 0.095(11) 0.068(9) 0.050(8) 0.001(7) 0.028(8) 0.028(7) C13 0.038(8) 0.060(7) 0.081(9) -0.017(6) 0.022(7) -0.017(6) C14 0.056(9) 0.075(9) 0.095(11) -0.027(8) 0.033(9) -0.014(7) C15 0.055(9) 0.076(9) 0.095(11) -0.036(8) 0.049(9) -0.022(7) C16 0.091(11) 0.059(8) 0.052(8) -0.009(7) 0.026(8) -0.033(8) C17 0.110(13) 0.085(10) 0.060(10) -0.019(8) 0.039(9) -0.035(9) C18 0.119(13) 0.071(9) 0.058(9) -0.002(7) 0.012(9) -0.022(9) C19 0.070(10) 0.076(9) 0.050(8) 0.003(7) 0.015(7) -0.002(7) C20 0.095(12) 0.053(8) 0.064(9) -0.002(7) -0.006(9) -0.008(8) C21 0.049(8) 0.065(8) 0.077(10) -0.009(7) -0.012(8) -0.005(7) C22 0.035(8) 0.063(8) 0.076(9) -0.002(7) 0.005(6) -0.009(6) C23 0.056(9) 0.064(8) 0.057(8) -0.011(7) 0.025(7) -0.013(7) C24 0.041(8) 0.062(8) 0.070(9) -0.017(7) 0.017(7) -0.016(6) C25 0.061(10) 0.113(12) 0.160(15) -0.030(11) 0.046(10) 0.001(9) C26 0.100(12) 0.127(13) 0.128(13) -0.051(10) 0.088(11) -0.048(10) C27 0.106(12) 0.116(12) 0.088(11) 0.021(10) -0.005(9) 0.013(10) C28 0.051(8) 0.093(10) 0.085(10) 0.004(8) -0.001(7) 0.005(7) C29 0.065(8) 0.039(8) 0.093(10) 0.006(7) -0.007(7) 0.002(6) C30 0.080(10) 0.035(8) 0.117(12) 0.012(7) -0.021(9) 0.012(7) C31 0.084(11) 0.049(9) 0.115(12) 0.001(7) -0.042(9) 0.000(7) C32 0.079(10) 0.050(8) 0.080(9) 0.007(7) -0.006(8) -0.006(7) C33 0.078(10) 0.052(9) 0.128(13) 0.009(8) -0.038(9) -0.008(7) C34 0.076(10) 0.070(10) 0.082(10) -0.001(7) -0.032(8) 0.003(8) C35 0.045(8) 0.057(8) 0.073(8) 0.007(6) 0.002(7) -0.002(6) C36 0.062(9) 0.061(9) 0.076(9) 0.007(7) -0.001(7) 0.007(7) C37 0.054(8) 0.044(7) 0.068(8) -0.010(6) -0.006(7) 0.008(6) C38 0.052(8) 0.041(7) 0.051(7) 0.003(5) 0.013(6) 0.000(6) C39 0.037(7) 0.053(8) 0.053(7) 0.006(6) 0.002(6) -0.004(6) C40 0.048(8) 0.038(7) 0.056(7) 0.005(6) 0.004(6) -0.001(6) C41 0.120(13) 0.055(9) 0.177(17) 0.001(9) -0.063(12) 0.008(8) C42 0.154(16) 0.040(8) 0.189(18) -0.008(9) -0.084(14) -0.020(9) C43 0.069(10) 0.088(11) 0.164(16) 0.007(10) -0.038(10) 0.024(8) C44 0.090(10) 0.054(8) 0.098(11) 0.017(7) -0.028(8) 0.017(7) C45 0.034(7) 0.046(6) 0.054(8) 0.013(5) 0.007(6) 0.005(5) C46 0.045(8) 0.061(7) 0.045(7) 0.021(6) 0.001(6) 0.000(6) C47 0.066(9) 0.050(7) 0.064(8) 0.010(6) 0.021(7) -0.006(6) C48 0.053(8) 0.043(6) 0.053(8) 0.011(6) -0.013(6) -0.002(6) C49 0.057(8) 0.049(7) 0.060(8) 0.010(6) -0.006(7) 0.001(6) C50 0.045(8) 0.054(7) 0.057(8) 0.010(6) -0.008(7) 0.003(6) C51 0.032(7) 0.045(7) 0.081(10) -0.007(6) 0.013(7) -0.002(5) C52 0.054(9) 0.065(9) 0.089(11) 0.001(8) -0.008(8) -0.001(7) C53 0.025(7) 0.080(9) 0.113(12) -0.022(9) 0.024(8) -0.006(6) C54 0.045(9) 0.086(9) 0.080(9) -0.012(7) 0.014(8) -0.009(7) C55 0.025(7) 0.049(7) 0.064(9) 0.006(6) -0.005(6) 0.002(5) C56 0.039(7) 0.046(7) 0.062(8) -0.001(6) 0.001(6) -0.008(5) C57 0.070(9) 0.080(9) 0.080(9) 0.018(7) 0.035(8) -0.004(7) C58 0.092(10) 0.064(8) 0.059(8) 0.021(6) 0.008(7) 0.008(7) C60 0.045(9) 0.153(14) 0.146(15) -0.021(11) 0.051(9) -0.005(9) C61 0.031(6) 0.075(8) 0.045(8) 0.003(6) 0.024(5) 0.001(6) C62 0.043(7) 0.070(8) 0.039(7) 0.003(6) 0.008(6) -0.003(6) C63 0.043(7) 0.073(8) 0.042(7) -0.008(6) 0.006(6) -0.009(6) C64 0.040(7) 0.066(8) 0.040(7) 0.001(6) 0.008(5) -0.012(6) C65 0.069(9) 0.084(9) 0.053(8) -0.003(7) 0.010(7) -0.038(7) C66 0.091(10) 0.081(9) 0.032(7) -0.004(6) 0.030(6) -0.043(7) C67 0.052(7) 0.061(7) 0.026(7) -0.003(6) 0.009(5) -0.023(6) C68 0.068(8) 0.060(8) 0.046(8) 0.008(6) 0.013(6) -0.012(6) C69 0.054(7) 0.075(8) 0.036(7) 0.004(6) 0.010(6) -0.010(6) C70 0.045(7) 0.054(7) 0.054(8) 0.013(6) 0.009(6) -0.015(5) C71 0.033(6) 0.058(7) 0.037(7) 0.006(6) 0.002(5) -0.014(5) C72 0.033(6) 0.057(7) 0.036(7) 0.002(6) 0.000(5) -0.006(5) C73 0.064(8) 0.088(9) 0.034(7) -0.006(6) 0.010(6) -0.012(7) C74 0.084(10) 0.089(10) 0.064(9) -0.017(7) 0.027(7) -0.024(8) C75 0.100(10) 0.090(9) 0.041(7) 0.004(6) 0.028(7) -0.036(8) C76 0.085(9) 0.063(8) 0.037(7) -0.005(6) 0.014(6) -0.013(6) C77 0.047(7) 0.069(8) 0.041(8) -0.008(6) 0.011(6) -0.010(6) C78 0.046(7) 0.065(8) 0.041(7) 0.004(6) 0.012(6) -0.013(6) C79 0.044(7) 0.057(7) 0.066(9) -0.009(7) 0.002(6) -0.012(6) C80 0.036(7) 0.056(7) 0.071(9) 0.023(7) 0.012(6) -0.005(6) C81 0.048(8) 0.074(8) 0.075(10) 0.020(8) 0.016(7) -0.015(6) C82 0.068(9) 0.082(9) 0.055(9) 0.016(7) 0.020(7) -0.002(7) C83 0.046(7) 0.076(9) 0.055(9) 0.004(7) 0.000(6) -0.004(6) C84 0.058(9) 0.125(12) 0.045(9) 0.008(8) 0.011(7) 0.002(8) C85 0.065(9) 0.126(12) 0.049(9) -0.018(8) 0.011(7) -0.018(9) C86 0.071(9) 0.086(10) 0.066(10) -0.006(8) 0.022(8) -0.015(7) C87 0.042(7) 0.069(8) 0.035(7) 0.010(6) 0.012(5) -0.003(6) C88 0.044(7) 0.060(7) 0.031(7) 0.015(6) 0.007(6) 0.011(6) C89 0.055(8) 0.102(10) 0.066(9) -0.017(7) 0.024(7) -0.028(7) C90 0.073(9) 0.084(9) 0.072(9) 0.004(7) 0.018(7) -0.026(7) C91 0.092(11) 0.157(14) 0.047(8) 0.018(8) 0.021(8) -0.013(10) C92 0.098(12) 0.186(17) 0.072(11) -0.048(11) 0.005(9) -0.031(12) C93 0.164(17) 0.064(11) 0.099(12) 0.022(8) 0.059(11) 0.024(10) C94 0.22(2) 0.082(13) 0.104(15) 0.040(11) 0.031(15) 0.086(15) C95 0.16(2) 0.129(19) 0.111(16) 0.011(13) -0.019(13) 0.043(16) C96 0.146(18) 0.117(15) 0.083(12) 0.028(11) 0.008(12) 0.075(14) C97 0.097(14) 0.134(17) 0.121(15) -0.024(13) -0.048(11) 0.030(13) C98 0.079(12) 0.133(16) 0.115(14) -0.017(12) -0.025(10) 0.022(11) C99 0.059(9) 0.089(11) 0.077(10) -0.013(8) 0.001(8) 0.011(8) C100 0.074(11) 0.114(13) 0.068(10) -0.008(9) 0.008(8) 0.003(9) C101 0.072(10) 0.082(10) 0.065(9) -0.006(7) 0.035(8) -0.002(8) C102 0.058(8) 0.065(9) 0.061(8) -0.006(7) 0.018(6) -0.009(7) C103 0.075(10) 0.070(9) 0.044(8) 0.006(6) 0.007(7) 0.014(8) C104 0.084(11) 0.085(11) 0.065(9) -0.003(8) 0.006(8) 0.021(9) C105 0.32(3) 0.077(13) 0.169(19) 0.029(12) 0.04(2) 0.096(16) C106 0.25(3) 0.17(2) 0.157(19) 0.026(15) -0.024(18) 0.16(2) C107 0.082(11) 0.118(13) 0.129(14) -0.035(11) -0.020(10) -0.015(10) C108 0.089(10) 0.059(9) 0.118(12) 0.002(8) 0.019(9) -0.003(7) C3S 0.043(8) 0.094(10) 0.119(12) -0.040(9) -0.019(8) 0.015(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N4 2.039(9) . ? Co1 N7 2.092(11) . ? Co1 N13 2.124(9) . ? Co1 N14 2.128(9) . ? Co1 N16 2.135(8) . ? Co1 N15 2.143(8) . ? Co2 N5 2.002(10) . ? Co2 N8 2.021(9) . ? Co2 N20 2.069(9) . ? Co2 N17 2.075(8) . ? Co2 N19 2.075(10) . ? Co2 N18 2.088(9) . ? Co3 N9 2.011(10) . ? Co3 N6 2.043(11) . ? Co3 N23 2.077(9) . ? Co3 N21 2.082(8) . ? Co3 N24 2.085(9) . ? Co3 N22 2.130(8) . ? Fe1 C5 1.899(12) . ? Fe1 C1 1.909(14) . ? Fe1 C2 1.914(14) . ? Fe1 C4 1.926(13) . ? Fe1 C3 1.929(14) . ? Fe1 C6 1.942(12) . ? Fe2 C12 1.882(14) . ? Fe2 C9 1.885(12) . ? Fe2 C7 1.903(13) . ? Fe2 C8 1.916(12) . ? Fe2 C11 1.921(13) . ? Fe2 C10 1.925(13) . ? N1 C1 1.150(13) . ? N2 C2 1.174(13) . ? N3 C3 1.177(14) . ? N4 C4 1.137(12) . ? N5 C5 1.162(12) . ? N6 C6 1.167(12) . ? N7 C7 1.148(12) . ? N8 C8 1.156(12) . ? N9 C9 1.170(12) . ? N10 C10 1.174(13) . ? N11 C11 1.136(14) . ? N12 C12 1.162(14) . ? N13 C45 1.352(12) . ? N13 C56 1.369(13) . ? N14 C54 1.328(13) . ? N14 C55 1.327(13) . ? N15 C61 1.340(12) . ? N15 C72 1.361(12) . ? N16 C70 1.331(13) . ? N16 C71 1.359(12) . ? N17 C77 1.308(12) . ? N17 C88 1.367(12) . ? N18 C86 1.279(14) . ? N18 C87 1.337(13) . ? N19 C93 1.333(15) . ? N19 C104 1.353(16) . ? N20 C102 1.303(13) . ? N20 C103 1.336(14) . ? N21 C38 1.302(12) . ? N21 C39 1.378(12) . ? N22 C40 1.342(13) . ? N22 C29 1.355(13) . ? N23 C13 1.297(13) . ? N23 C24 1.328(14) . ? N24 C22 1.346(13) . ? N24 C23 1.361(13) . ? C13 C14 1.378(16) . ? C14 C15 1.377(18) . ? C14 C25 1.490(18) . ? C15 C16 1.394(18) . ? C15 C26 1.482(17) . ? C16 C17 1.445(18) . ? C16 C24 1.460(16) . ? C17 C18 1.417(19) . ? C18 C19 1.400(17) . ? C19 C23 1.384(16) . ? C19 C20 1.444(18) . ? C20 C21 1.388(17) . ? C20 C27 1.498(17) . ? C21 C22 1.374(16) . ? C21 C28 1.521(16) . ? C23 C24 1.434(16) . ? C29 C30 1.363(16) . ? C30 C31 1.353(16) . ? C30 C41 1.549(16) . ? C31 C32 1.435(16) . ? C31 C42 1.492(16) . ? C32 C40 1.379(15) . ? C32 C33 1.439(17) . ? C33 C34 1.334(16) . ? C34 C35 1.460(16) . ? C35 C39 1.394(14) . ? C35 C36 1.415(15) . ? C36 C37 1.361(15) . ? C36 C43 1.504(16) . ? C37 C38 1.401(14) . ? C37 C44 1.540(15) . ? C39 C40 1.438(14) . ? C45 C46 1.385(14) . ? C46 C47 1.367(15) . ? C46 C57 1.502(15) . ? C47 C48 1.412(15) . ? C47 C58 1.520(15) . ? C48 C56 1.428(15) . ? C48 C49 1.432(15) . ? C49 C50 1.304(15) . ? C50 C51 1.411(15) . ? C51 C52 1.374(17) . ? C51 C55 1.413(14) . ? C52 C53 1.378(17) . ? C52 C3S 1.541(16) . ? C53 C54 1.422(17) . ? C53 C60 1.547(17) . ? C55 C56 1.437(15) . ? C61 C62 1.395(14) . ? C62 C63 1.376(14) . ? C62 C73 1.507(14) . ? C63 C64 1.404(14) . ? C63 C74 1.484(15) . ? C64 C72 1.403(13) . ? C64 C65 1.439(14) . ? C65 C66 1.362(14) . ? C66 C67 1.435(14) . ? C67 C68 1.373(14) . ? C67 C71 1.380(13) . ? C68 C69 1.392(14) . ? C68 C75 1.541(14) . ? C69 C70 1.407(14) . ? C69 C76 1.498(14) . ? C71 C72 1.436(14) . ? C77 C78 1.387(14) . ? C78 C79 1.373(14) . ? C78 C89 1.495(15) . ? C79 C80 1.409(15) . ? C79 C90 1.498(15) . ? C80 C88 1.390(15) . ? C80 C81 1.448(15) . ? C81 C82 1.339(16) . ? C82 C83 1.426(16) . ? C83 C87 1.409(14) . ? C83 C84 1.431(16) . ? C84 C85 1.371(18) . ? C84 C91 1.510(16) . ? C85 C86 1.384(17) . ? C85 C92 1.515(17) . ? C87 C88 1.432(14) . ? C93 C94 1.47(2) . ? C94 C95 1.37(3) . ? C94 C105 1.55(2) . ? C95 C96 1.42(2) . ? C95 C106 1.50(2) . ? C96 C97 1.39(2) . ? C96 C104 1.45(2) . ? C97 C98 1.28(2) . ? C98 C99 1.447(19) . ? C99 C103 1.378(17) . ? C99 C100 1.432(18) . ? C100 C101 1.402(17) . ? C100 C107 1.511(19) . ? C101 C102 1.405(16) . ? C101 C108 1.512(16) . ? C103 C104 1.430(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N7 90.8(3) . . ? N4 Co1 N13 90.5(3) . . ? N7 Co1 N13 99.5(3) . . ? N4 Co1 N14 167.8(3) . . ? N7 Co1 N14 90.8(3) . . ? N13 Co1 N14 77.3(3) . . ? N4 Co1 N16 97.1(3) . . ? N7 Co1 N16 91.2(3) . . ? N13 Co1 N16 166.7(3) . . ? N14 Co1 N16 94.9(3) . . ? N4 Co1 N15 95.1(3) . . ? N7 Co1 N15 166.5(3) . . ? N13 Co1 N15 92.6(3) . . ? N14 Co1 N15 86.0(3) . . ? N16 Co1 N15 75.9(3) . . ? N5 Co2 N8 94.3(3) . . ? N5 Co2 N20 93.0(3) . . ? N8 Co2 N20 91.6(4) . . ? N5 Co2 N17 91.7(3) . . ? N8 Co2 N17 91.6(3) . . ? N20 Co2 N17 174.1(3) . . ? N5 Co2 N19 90.1(4) . . ? N8 Co2 N19 169.8(4) . . ? N20 Co2 N19 79.0(4) . . ? N17 Co2 N19 97.4(4) . . ? N5 Co2 N18 168.6(4) . . ? N8 Co2 N18 92.4(3) . . ? N20 Co2 N18 96.1(4) . . ? N17 Co2 N18 78.9(3) . . ? N19 Co2 N18 84.9(4) . . ? N9 Co3 N6 90.6(3) . . ? N9 Co3 N23 173.4(4) . . ? N6 Co3 N23 89.0(3) . . ? N9 Co3 N21 96.9(3) . . ? N6 Co3 N21 94.9(3) . . ? N23 Co3 N21 89.6(4) . . ? N9 Co3 N24 95.1(4) . . ? N6 Co3 N24 99.0(3) . . ? N23 Co3 N24 78.5(4) . . ? N21 Co3 N24 161.5(3) . . ? N9 Co3 N22 93.5(3) . . ? N6 Co3 N22 172.5(3) . . ? N23 Co3 N22 87.6(3) . . ? N21 Co3 N22 78.4(3) . . ? N24 Co3 N22 86.9(3) . . ? C5 Fe1 C1 176.8(4) . . ? C5 Fe1 C2 89.3(5) . . ? C1 Fe1 C2 88.3(5) . . ? C5 Fe1 C4 87.5(4) . . ? C1 Fe1 C4 90.3(5) . . ? C2 Fe1 C4 86.9(4) . . ? C5 Fe1 C3 93.1(5) . . ? C1 Fe1 C3 89.1(5) . . ? C2 Fe1 C3 92.6(4) . . ? C4 Fe1 C3 179.2(5) . . ? C5 Fe1 C6 86.5(4) . . ? C1 Fe1 C6 96.0(4) . . ? C2 Fe1 C6 175.7(5) . . ? C4 Fe1 C6 93.6(4) . . ? C3 Fe1 C6 86.9(4) . . ? C12 Fe2 C9 91.0(5) . . ? C12 Fe2 C7 176.3(5) . . ? C9 Fe2 C7 90.4(4) . . ? C12 Fe2 C8 89.7(5) . . ? C9 Fe2 C8 88.3(4) . . ? C7 Fe2 C8 86.9(4) . . ? C12 Fe2 C11 90.2(6) . . ? C9 Fe2 C11 177.8(5) . . ? C7 Fe2 C11 88.5(5) . . ? C8 Fe2 C11 93.5(5) . . ? C12 Fe2 C10 89.5(5) . . ? C9 Fe2 C10 86.7(4) . . ? C7 Fe2 C10 93.9(4) . . ? C8 Fe2 C10 174.9(5) . . ? C11 Fe2 C10 91.5(5) . . ? C4 N4 Co1 156.4(8) . . ? C5 N5 Co2 162.9(8) . . ? C6 N6 Co3 158.9(9) . . ? C7 N7 Co1 163.6(8) . . ? C8 N8 Co2 161.2(8) . . ? C9 N9 Co3 164.5(8) . . ? C45 N13 C56 115.6(9) . . ? C45 N13 Co1 130.8(7) . . ? C56 N13 Co1 113.6(7) . . ? C54 N14 C55 116.3(10) . . ? C54 N14 Co1 128.3(9) . . ? C55 N14 Co1 115.4(7) . . ? C61 N15 C72 115.0(9) . . ? C61 N15 Co1 129.2(7) . . ? C72 N15 Co1 115.8(6) . . ? C70 N16 C71 117.5(8) . . ? C70 N16 Co1 126.5(7) . . ? C71 N16 Co1 116.0(6) . . ? C77 N17 C88 117.2(9) . . ? C77 N17 Co2 128.6(7) . . ? C88 N17 Co2 114.2(7) . . ? C86 N18 C87 117.3(10) . . ? C86 N18 Co2 128.9(9) . . ? C87 N18 Co2 113.5(7) . . ? C93 N19 C104 119.2(13) . . ? C93 N19 Co2 127.4(12) . . ? C104 N19 Co2 113.3(8) . . ? C102 N20 C103 117.5(10) . . ? C102 N20 Co2 128.2(8) . . ? C103 N20 Co2 114.3(8) . . ? C38 N21 C39 117.8(9) . . ? C38 N21 Co3 128.8(7) . . ? C39 N21 Co3 112.9(6) . . ? C40 N22 C29 116.9(9) . . ? C40 N22 Co3 113.7(7) . . ? C29 N22 Co3 129.0(8) . . ? C13 N23 C24 116.7(10) . . ? C13 N23 Co3 129.5(9) . . ? C24 N23 Co3 113.9(7) . . ? C22 N24 C23 117.6(10) . . ? C22 N24 Co3 127.7(8) . . ? C23 N24 Co3 114.6(8) . . ? N1 C1 Fe1 176.4(11) . . ? N2 C2 Fe1 177.6(11) . . ? N3 C3 Fe1 177.4(10) . . ? N4 C4 Fe1 177.5(10) . . ? N5 C5 Fe1 175.9(9) . . ? N6 C6 Fe1 171.7(9) . . ? N7 C7 Fe2 173.7(9) . . ? N8 C8 Fe2 174.4(9) . . ? N9 C9 Fe2 178.2(10) . . ? N10 C10 Fe2 176.3(11) . . ? N11 C11 Fe2 177.5(14) . . ? N12 C12 Fe2 178.8(12) . . ? N23 C13 C14 126.8(13) . . ? C15 C14 C13 119.4(13) . . ? C15 C14 C25 119.4(13) . . ? C13 C14 C25 121.2(15) . . ? C14 C15 C16 116.4(11) . . ? C14 C15 C26 123.0(14) . . ? C16 C15 C26 120.6(15) . . ? C15 C16 C17 125.4(13) . . ? C15 C16 C24 119.3(12) . . ? C17 C16 C24 115.4(13) . . ? C18 C17 C16 121.8(13) . . ? C19 C18 C17 121.9(13) . . ? C23 C19 C18 117.7(13) . . ? C23 C19 C20 118.5(11) . . ? C18 C19 C20 123.7(13) . . ? C21 C20 C19 117.9(11) . . ? C21 C20 C27 121.7(14) . . ? C19 C20 C27 120.4(13) . . ? C22 C21 C20 118.9(12) . . ? C22 C21 C28 118.4(13) . . ? C20 C21 C28 122.6(12) . . ? N24 C22 C21 124.5(11) . . ? N24 C23 C19 122.6(11) . . ? N24 C23 C24 114.3(11) . . ? C19 C23 C24 123.0(12) . . ? N23 C24 C23 118.6(11) . . ? N23 C24 C16 121.5(11) . . ? C23 C24 C16 119.9(13) . . ? N22 C29 C30 123.2(11) . . ? C31 C30 C29 121.1(11) . . ? C31 C30 C41 120.8(12) . . ? C29 C30 C41 117.8(12) . . ? C30 C31 C32 116.8(11) . . ? C30 C31 C42 122.1(11) . . ? C32 C31 C42 121.0(12) . . ? C40 C32 C31 118.8(11) . . ? C40 C32 C33 118.4(11) . . ? C31 C32 C33 122.7(11) . . ? C34 C33 C32 120.2(12) . . ? C33 C34 C35 123.7(12) . . ? C39 C35 C36 119.2(10) . . ? C39 C35 C34 115.6(10) . . ? C36 C35 C34 125.1(11) . . ? C37 C36 C35 117.7(11) . . ? C37 C36 C43 121.1(11) . . ? C35 C36 C43 121.2(12) . . ? C36 C37 C38 119.7(10) . . ? C36 C37 C44 123.0(10) . . ? C38 C37 C44 117.3(10) . . ? N21 C38 C37 124.0(10) . . ? N21 C39 C35 121.5(9) . . ? N21 C39 C40 117.6(9) . . ? C35 C39 C40 120.9(10) . . ? N22 C40 C32 123.0(10) . . ? N22 C40 C39 115.9(9) . . ? C32 C40 C39 121.1(10) . . ? N13 C45 C46 126.1(10) . . ? C47 C46 C45 118.4(10) . . ? C47 C46 C57 124.0(10) . . ? C45 C46 C57 117.5(10) . . ? C46 C47 C48 119.1(10) . . ? C46 C47 C58 123.6(11) . . ? C48 C47 C58 117.3(11) . . ? C47 C48 C56 118.6(10) . . ? C47 C48 C49 124.4(11) . . ? C56 C48 C49 116.9(11) . . ? C50 C49 C48 122.3(11) . . ? C49 C50 C51 122.7(11) . . ? C52 C51 C50 123.8(11) . . ? C52 C51 C55 116.9(11) . . ? C50 C51 C55 119.3(11) . . ? C51 C52 C53 119.9(11) . . ? C51 C52 C3S 123.2(13) . . ? C53 C52 C3S 116.9(13) . . ? C52 C53 C54 118.0(11) . . ? C52 C53 C60 127.1(13) . . ? C54 C53 C60 114.7(13) . . ? N14 C54 C53 123.5(12) . . ? N14 C55 C51 125.3(10) . . ? N14 C55 C56 116.6(9) . . ? C51 C55 C56 118.1(11) . . ? N13 C56 C48 122.2(10) . . ? N13 C56 C55 117.1(10) . . ? C48 C56 C55 120.7(10) . . ? N15 C61 C62 125.1(9) . . ? C63 C62 C61 119.3(10) . . ? C63 C62 C73 122.1(10) . . ? C61 C62 C73 118.6(10) . . ? C62 C63 C64 117.8(10) . . ? C62 C63 C74 119.9(10) . . ? C64 C63 C74 122.2(10) . . ? C72 C64 C63 118.6(9) . . ? C72 C64 C65 118.0(10) . . ? C63 C64 C65 123.4(10) . . ? C66 C65 C64 120.8(11) . . ? C65 C66 C67 122.4(10) . . ? C68 C67 C71 119.9(9) . . ? C68 C67 C66 123.0(9) . . ? C71 C67 C66 117.1(9) . . ? C67 C68 C69 119.8(10) . . ? C67 C68 C75 121.7(10) . . ? C69 C68 C75 118.5(10) . . ? C68 C69 C70 116.5(10) . . ? C68 C69 C76 125.2(10) . . ? C70 C69 C76 118.3(10) . . ? N16 C70 C69 124.3(10) . . ? N16 C71 C67 121.9(9) . . ? N16 C71 C72 116.2(9) . . ? C67 C71 C72 121.9(10) . . ? N15 C72 C64 124.1(9) . . ? N15 C72 C71 116.0(9) . . ? C64 C72 C71 119.9(9) . . ? N17 C77 C78 124.8(10) . . ? C79 C78 C77 119.3(10) . . ? C79 C78 C89 122.0(10) . . ? C77 C78 C89 118.7(10) . . ? C78 C79 C80 117.2(10) . . ? C78 C79 C90 121.7(11) . . ? C80 C79 C90 121.1(11) . . ? C88 C80 C79 119.7(10) . . ? C88 C80 C81 115.4(11) . . ? C79 C80 C81 124.8(11) . . ? C82 C81 C80 123.2(11) . . ? C81 C82 C83 121.1(11) . . ? C87 C83 C82 118.5(11) . . ? C87 C83 C84 116.8(11) . . ? C82 C83 C84 124.7(12) . . ? C85 C84 C83 118.2(11) . . ? C85 C84 C91 123.0(13) . . ? C83 C84 C91 118.7(13) . . ? C84 C85 C86 117.9(12) . . ? C84 C85 C92 120.3(13) . . ? C86 C85 C92 121.8(14) . . ? N18 C86 C85 126.5(12) . . ? N18 C87 C83 123.2(10) . . ? N18 C87 C88 117.9(9) . . ? C83 C87 C88 118.9(11) . . ? N17 C88 C80 121.7(10) . . ? N17 C88 C87 115.4(10) . . ? C80 C88 C87 122.8(10) . . ? N19 C93 C94 120.8(17) . . ? C95 C94 C93 120.0(16) . . ? C95 C94 C105 128(2) . . ? C93 C94 C105 112(2) . . ? C94 C95 C96 119.3(19) . . ? C94 C95 C106 118(2) . . ? C96 C95 C106 122(2) . . ? C97 C96 C95 125.7(18) . . ? C97 C96 C104 117.3(16) . . ? C95 C96 C104 117(2) . . ? C98 C97 C96 122.7(17) . . ? C97 C98 C99 122.9(17) . . ? C103 C99 C100 118.0(12) . . ? C103 C99 C98 118.2(14) . . ? C100 C99 C98 123.8(15) . . ? C101 C100 C99 117.0(13) . . ? C101 C100 C107 120.1(14) . . ? C99 C100 C107 122.9(13) . . ? C100 C101 C102 118.2(13) . . ? C100 C101 C108 122.3(13) . . ? C102 C101 C108 119.4(13) . . ? N20 C102 C101 124.6(12) . . ? N20 C103 C99 124.4(12) . . ? N20 C103 C104 116.5(13) . . ? C99 C103 C104 119.0(13) . . ? N19 C104 C103 116.7(12) . . ? N19 C104 C96 123.6(15) . . ? C103 C104 C96 119.7(16) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.975 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.162 #end================================== data_{[Co(tmphen)2]3[Fe(CN)6]2}_190K _audit_creation_method SHELXL-97 _chemical_name_systematic ; {[Co(tmphen)2]3[Fe(CN)6]2}.8H2O ; _chemical_name_common '((Co(tmphen)2)3(Fe(CN)6)2).8H2O' _chemical_melting_point ? _chemical_formula_moiety 'C108 H112 Co3 Fe2 N24 O8' _chemical_formula_sum 'C108 H112 Co3 Fe2 N24 O8' _chemical_formula_weight 2162.7 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.223(4) _cell_length_b 25.188(5) _cell_length_c 24.805(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.45(3) _cell_angle_gamma 90.00 _cell_volume 11909(4) _cell_formula_units_Z 4 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used 12463 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 14.77 _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4436 _exptl_absorpt_coefficient_mu 0.707 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8658 _exptl_absorpt_correction_T_max 0.9200 _exptl_absorpt_process_details 'SADABS: Bruker,2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER APEX' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57258 _diffrn_reflns_av_R_equivalents 0.1878 _diffrn_reflns_av_sigmaI/netI 0.1664 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 20.82 _reflns_number_total 12463 _reflns_number_gt 6495 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER, 2000)' _computing_cell_refinement 'SAINT (BRUKER, 2001)' _computing_data_reduction 'SAINT (BRUKER, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1605P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0079(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12463 _refine_ls_number_parameters 1355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1801 _refine_ls_R_factor_gt 0.0997 _refine_ls_wR_factor_ref 0.2933 _refine_ls_wR_factor_gt 0.2431 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.112 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.06134(5) 0.37155(4) 0.61659(4) 0.0492(3) Uani 1 1 d . A -1 Co2 Co 0.29330(5) 0.36799(4) 0.83232(4) 0.0511(3) Uani 1 1 d . A -1 Co3 Co 0.35593(5) 0.54595(4) 0.66312(4) 0.0478(3) Uani 1 1 d . A -1 Fe1 Fe 0.32405(5) 0.34883(4) 0.63414(4) 0.0480(3) Uani 1 1 d . A -1 Fe2 Fe 0.13792(5) 0.51810(4) 0.75314(4) 0.0534(3) Uani 1 1 d . A -1 O15S O 0.6928(7) 0.4866(6) 1.0099(6) 0.121(5) Uiso 0.50 1 d P B -15 O11S O 0.5000(10) 0.2920(7) 1.0658(7) 0.172(7) Uiso 0.50 1 d P C -11 O2S O 0.0695(9) 0.0875(7) 0.4932(7) 0.159(6) Uiso 0.50 1 d P D -2 O16S O 0.5674(9) 0.7267(7) 0.9531(7) 0.153(6) Uiso 0.50 1 d P E -16 O9S O 0.6323(17) 0.3210(13) 0.6585(13) 0.146(11) Uiso 0.25 1 d P F -9 O10S O 0.6327(9) 0.3778(7) 0.6755(7) 0.157(6) Uiso 0.50 1 d P G -10 O24S O 0.1240(9) 0.4784(7) 0.9255(7) 0.151(6) Uiso 0.50 1 d P H -24 O6S O 0.2516(17) 0.0646(13) 0.7879(13) 0.143(11) Uiso 0.25 1 d P I -6 O23S O 0.2307(12) 0.8180(9) 0.5951(9) 0.088(7) Uiso 0.25 1 d P J -23 O22S O 0.2157(16) 0.8533(12) 0.6271(12) 0.131(10) Uiso 0.25 1 d P K -22 O21S O 0.2544(12) 0.6832(9) 0.7829(9) 0.090(7) Uiso 0.25 1 d P L -21 O13S O 0.7314(14) 0.4043(11) 1.0172(11) 0.111(9) Uiso 0.25 1 d P M -13 O3S O 0.0792(13) 0.0783(10) 0.6356(10) 0.099(8) Uiso 0.25 1 d P N -3 O27S O -0.2769(14) 0.1579(11) 0.5540(11) 0.116(9) Uiso 0.25 1 d P O -27 O12S O 0.5568(10) 0.2946(7) 1.0780(7) 0.164(7) Uiso 0.50 1 d P P -12 O26S O 0.0887(10) 0.0574(7) 0.4610(8) 0.169(7) Uiso 0.50 1 d P Q -26 O25S O -0.1473(17) 0.4559(13) 0.7711(13) 0.150(12) Uiso 0.25 1 d P R -25 O8S O 0.3042(19) 0.1504(14) 0.7849(14) 0.162(13) Uiso 0.25 1 d P S -8 O17S O 0.2347(19) 0.7776(14) 0.8131(14) 0.161(13) Uiso 0.25 1 d P T -17 O18S O 0.2589(19) 0.7239(15) 0.8148(14) 0.164(13) Uiso 0.25 1 d P U -18 O4S O 0.1762(17) 0.0643(13) 0.6711(13) 0.147(12) Uiso 0.25 1 d P V -4 O5S O 0.213(2) 0.0562(15) 0.7493(16) 0.178(14) Uiso 0.25 1 d P W -5 O14S O 0.7140(13) 0.4544(10) 1.0073(10) 0.094(8) Uiso 0.25 1 d P X -14 O7S O 0.2770(19) 0.1009(15) 0.7905(14) 0.162(13) Uiso 0.25 1 d P Y -7 N1 N 0.3094(3) 0.3246(3) 0.5129(3) 0.081(3) Uani 1 1 d . A -1 N2 N 0.3222(4) 0.2291(3) 0.6532(3) 0.084(3) Uani 1 1 d . A -1 N3 N 0.4863(3) 0.3547(3) 0.6384(3) 0.077(2) Uani 1 1 d . A -1 N4 N 0.1634(3) 0.3445(2) 0.6273(2) 0.0505(19) Uani 1 1 d . A -1 N5 N 0.3268(3) 0.3657(2) 0.7565(2) 0.055(2) Uani 1 1 d . A -1 N6 N 0.3302(3) 0.4708(2) 0.6304(2) 0.0492(18) Uani 1 1 d . A -1 N7 N 0.0913(3) 0.4418(2) 0.6580(2) 0.0468(18) Uani 1 1 d . A -1 N8 N 0.2130(3) 0.4212(2) 0.8095(2) 0.058(2) Uani 1 1 d . A -1 N9 N 0.2767(3) 0.5422(2) 0.7091(2) 0.0513(19) Uani 1 1 d . A -1 N10 N 0.0846(4) 0.6202(3) 0.6917(3) 0.080(2) Uani 1 1 d . A -1 N11 N -0.0051(4) 0.4936(3) 0.7912(3) 0.120(3) Uani 1 1 d . A -1 N12 N 0.1854(4) 0.5835(3) 0.8557(3) 0.093(3) Uani 1 1 d . A -1 N13 N 0.0712(3) 0.3963(2) 0.5347(2) 0.0525(19) Uani 1 1 d . A -1 N14 N -0.0397(3) 0.4041(2) 0.5884(2) 0.0520(19) Uani 1 1 d . A -1 N15 N 0.0147(3) 0.2960(2) 0.5899(2) 0.0487(18) Uani 1 1 d . A -1 N16 N 0.0299(3) 0.3369(2) 0.6893(2) 0.0491(18) Uani 1 1 d . A -1 N17 N 0.2255(3) 0.3021(2) 0.8121(2) 0.0528(19) Uani 1 1 d . A -1 N18 N 0.2583(3) 0.3506(2) 0.9084(2) 0.059(2) Uani 1 1 d . A -1 N19 N 0.3846(4) 0.3243(3) 0.8661(3) 0.073(2) Uani 1 1 d . A -1 N20 N 0.3659(3) 0.4282(2) 0.8618(2) 0.061(2) Uani 1 1 d . A -1 N21 N 0.4362(3) 0.5186(2) 0.7226(2) 0.0473(18) Uani 1 1 d . A -1 N22 N 0.3977(3) 0.6189(2) 0.7010(2) 0.054(2) Uani 1 1 d . A -1 N23 N 0.4311(3) 0.5539(2) 0.6076(2) 0.0510(19) Uani 1 1 d . A -1 N24 N 0.3017(3) 0.5943(2) 0.6003(2) 0.061(2) Uani 1 1 d . A -1 C1 C 0.3160(4) 0.3352(3) 0.5595(3) 0.062(3) Uani 1 1 d . A -1 C2 C 0.3242(4) 0.2743(3) 0.6472(3) 0.061(3) Uani 1 1 d . A -1 C3 C 0.4261(4) 0.3513(3) 0.6376(3) 0.060(3) Uani 1 1 d . A -1 C4 C 0.2230(4) 0.3465(3) 0.6301(3) 0.047(2) Uani 1 1 d . A -1 C5 C 0.3289(3) 0.3600(3) 0.7104(3) 0.051(2) Uani 1 1 d . A -1 C6 C 0.3256(3) 0.4249(3) 0.6273(3) 0.045(2) Uani 1 1 d . A -1 C7 C 0.1103(3) 0.4728(3) 0.6926(3) 0.048(2) Uani 1 1 d . A -1 C8 C 0.1816(4) 0.4573(3) 0.7894(3) 0.053(2) Uani 1 1 d . A -1 C9 C 0.2249(4) 0.5324(3) 0.7267(3) 0.047(2) Uani 1 1 d . A -1 C10 C 0.1033(4) 0.5810(3) 0.7158(3) 0.065(3) Uani 1 1 d . A -1 C11 C 0.0469(4) 0.5031(4) 0.7770(3) 0.083(3) Uani 1 1 d . A -1 C12 C 0.1655(4) 0.5597(3) 0.8165(3) 0.071(3) Uani 1 1 d . A -1 C13 C 0.4948(3) 0.5326(3) 0.6094(3) 0.061(3) Uani 1 1 d . A -1 H13 H 0.5108 0.5109 0.6399 0.073 Uiso 1 1 calc R A -1 C14 C 0.5380(4) 0.5393(3) 0.5718(3) 0.071(3) Uani 1 1 d . A -1 C15 C 0.5174(4) 0.5679(3) 0.5258(3) 0.072(3) Uani 1 1 d . A -1 C16 C 0.4490(4) 0.5915(3) 0.5213(3) 0.062(3) Uani 1 1 d . A -1 C17 C 0.4224(5) 0.6239(3) 0.4775(3) 0.082(3) Uani 1 1 d . A -1 H17 H 0.4495 0.6298 0.4487 0.099 Uiso 1 1 calc R A -1 C18 C 0.3567(5) 0.6477(4) 0.4757(3) 0.088(3) Uani 1 1 d . A -1 H18 H 0.3405 0.6696 0.4455 0.106 Uiso 1 1 calc R A -1 C19 C 0.3122(4) 0.6406(3) 0.5173(3) 0.071(3) Uani 1 1 d . A -1 C20 C 0.2471(5) 0.6658(4) 0.5173(3) 0.081(3) Uani 1 1 d . A -1 C21 C 0.2096(4) 0.6524(3) 0.5606(4) 0.074(3) Uani 1 1 d . A -1 C22 C 0.2383(4) 0.6169(3) 0.6006(3) 0.067(3) Uani 1 1 d . A -1 H22 H 0.2119 0.6084 0.6293 0.081 Uiso 1 1 calc R A -1 C23 C 0.3383(4) 0.6066(3) 0.5592(3) 0.059(2) Uani 1 1 d . A -1 C24 C 0.4080(4) 0.5831(3) 0.5631(3) 0.062(3) Uani 1 1 d . A -1 C25 C 0.6097(4) 0.5138(4) 0.5811(4) 0.100(4) Uani 1 1 d . A -1 H25A H 0.6136 0.4873 0.5528 0.150 Uiso 1 1 calc R A -1 H25B H 0.6162 0.4965 0.6168 0.150 Uiso 1 1 calc R A -1 H25C H 0.6458 0.5411 0.5798 0.150 Uiso 1 1 calc R A -1 C26 C 0.5634(4) 0.5747(4) 0.4818(4) 0.118(4) Uani 1 1 d . A -1 H26A H 0.5845 0.5405 0.4744 0.177 Uiso 1 1 calc R A -1 H26B H 0.6006 0.6004 0.4937 0.177 Uiso 1 1 calc R A -1 H26C H 0.5352 0.5877 0.4487 0.177 Uiso 1 1 calc R A -1 C27 C 0.2135(6) 0.7022(4) 0.4742(4) 0.125(4) Uani 1 1 d . A -1 H27A H 0.1911 0.7317 0.4911 0.188 Uiso 1 1 calc R A -1 H27B H 0.1780 0.6826 0.4500 0.188 Uiso 1 1 calc R A -1 H27C H 0.2492 0.7161 0.4532 0.188 Uiso 1 1 calc R A -1 C28 C 0.1382(4) 0.6767(3) 0.5679(4) 0.085(3) Uani 1 1 d . A -1 H28A H 0.1433 0.7152 0.5728 0.127 Uiso 1 1 calc R A -1 H28B H 0.1212 0.6611 0.5999 0.127 Uiso 1 1 calc R A -1 H28C H 0.1046 0.6693 0.5355 0.127 Uiso 1 1 calc R A -1 C29 C 0.3764(5) 0.6690(3) 0.6926(4) 0.078(3) Uani 1 1 d . A -1 H29 H 0.3328 0.6745 0.6705 0.093 Uiso 1 1 calc R A -1 C30 C 0.4117(5) 0.7131(3) 0.7130(4) 0.085(3) Uani 1 1 d . A -1 C31 C 0.4732(5) 0.7072(3) 0.7464(4) 0.096(4) Uani 1 1 d . A -1 C32 C 0.4986(4) 0.6543(3) 0.7592(4) 0.069(3) Uani 1 1 d . A -1 C33 C 0.5636(5) 0.6409(3) 0.7930(4) 0.105(4) Uani 1 1 d . A -1 H33 H 0.5928 0.6687 0.8087 0.126 Uiso 1 1 calc R A -1 C34 C 0.5833(5) 0.5916(3) 0.8023(4) 0.104(4) Uani 1 1 d . A -1 H34 H 0.6258 0.5849 0.8253 0.124 Uiso 1 1 calc R A -1 C35 C 0.5425(4) 0.5472(3) 0.7788(3) 0.073(3) Uani 1 1 d . A -1 C36 C 0.5622(4) 0.4934(3) 0.7886(3) 0.074(3) Uani 1 1 d . A -1 C37 C 0.5168(4) 0.4545(3) 0.7672(3) 0.058(3) Uani 1 1 d . A -1 C38 C 0.4557(4) 0.4706(3) 0.7345(3) 0.057(3) Uani 1 1 d . A -1 H38 H 0.4252 0.4432 0.7195 0.069 Uiso 1 1 calc R A -1 C39 C 0.4799(4) 0.5581(3) 0.7454(3) 0.053(2) Uani 1 1 d . A -1 C40 C 0.4591(4) 0.6116(3) 0.7356(3) 0.056(3) Uani 1 1 d . A -1 C41 C 0.3804(5) 0.7680(3) 0.6982(4) 0.110(4) Uani 1 1 d . A -1 H41A H 0.3795 0.7889 0.7314 0.165 Uiso 1 1 calc R A -1 H41B H 0.3325 0.7639 0.6796 0.165 Uiso 1 1 calc R A -1 H41C H 0.4092 0.7863 0.6741 0.165 Uiso 1 1 calc R A -1 C42 C 0.5135(6) 0.7538(4) 0.7698(5) 0.147(5) Uani 1 1 d . A -1 H42A H 0.4845 0.7858 0.7638 0.221 Uiso 1 1 calc R A -1 H42B H 0.5559 0.7581 0.7521 0.221 Uiso 1 1 calc R A -1 H42C H 0.5268 0.7484 0.8089 0.221 Uiso 1 1 calc R A -1 C43 C 0.6311(5) 0.4793(4) 0.8238(4) 0.117(4) Uani 1 1 d . A -1 H43A H 0.6209 0.4621 0.8573 0.176 Uiso 1 1 calc R A -1 H43B H 0.6583 0.5118 0.8329 0.176 Uiso 1 1 calc R A -1 H43C H 0.6582 0.4551 0.8038 0.176 Uiso 1 1 calc R A -1 C44 C 0.5319(4) 0.3955(3) 0.7758(4) 0.082(3) Uani 1 1 d . A -1 H44A H 0.4889 0.3752 0.7650 0.123 Uiso 1 1 calc R A -1 H44B H 0.5484 0.3889 0.8142 0.123 Uiso 1 1 calc R A -1 H44C H 0.5680 0.3845 0.7536 0.123 Uiso 1 1 calc R A -1 C45 C 0.1262(4) 0.3917(3) 0.5070(3) 0.057(2) Uani 1 1 d . A -1 H45 H 0.1679 0.3765 0.5254 0.068 Uiso 1 1 calc R A -1 C46 C 0.1268(4) 0.4075(3) 0.4532(3) 0.055(2) Uani 1 1 d . A -1 C47 C 0.0683(4) 0.4313(3) 0.4264(3) 0.061(3) Uani 1 1 d . A -1 C48 C 0.0076(4) 0.4378(3) 0.4537(3) 0.059(3) Uani 1 1 d . A -1 C49 C -0.0548(4) 0.4608(3) 0.4298(3) 0.069(3) Uani 1 1 d . A -1 H49 H -0.0579 0.4728 0.3933 0.082 Uiso 1 1 calc R A -1 C50 C -0.1107(4) 0.4666(3) 0.4565(3) 0.071(3) Uani 1 1 d . A -1 H50 H -0.1518 0.4834 0.4390 0.085 Uiso 1 1 calc R A -1 C51 C -0.1092(3) 0.4478(3) 0.5109(3) 0.062(3) Uani 1 1 d . A -1 C52 C -0.1667(4) 0.4504(3) 0.5404(3) 0.071(3) Uani 1 1 d . A -1 C53 C -0.1612(4) 0.4304(3) 0.5942(4) 0.079(3) Uani 1 1 d . A -1 C54 C -0.0948(4) 0.4066(3) 0.6156(3) 0.072(3) Uani 1 1 d . A -1 H54 H -0.0903 0.3920 0.6511 0.087 Uiso 1 1 calc R A -1 C55 C -0.0471(3) 0.4235(3) 0.5373(3) 0.047(2) Uani 1 1 d . A -1 C56 C 0.0134(4) 0.4192(3) 0.5081(3) 0.057(3) Uani 1 1 d . A -1 C57 C 0.1934(4) 0.3982(4) 0.4269(3) 0.085(3) Uani 1 1 d . A -1 H57A H 0.1831 0.3738 0.3962 0.127 Uiso 1 1 calc R A -1 H57B H 0.2298 0.3828 0.4537 0.127 Uiso 1 1 calc R A -1 H57C H 0.2100 0.4321 0.4139 0.127 Uiso 1 1 calc R A -1 C58 C 0.0637(4) 0.4518(3) 0.3682(3) 0.071(3) Uani 1 1 d . A -1 H58A H 0.1084 0.4454 0.3542 0.106 Uiso 1 1 calc R A -1 H58B H 0.0539 0.4900 0.3676 0.106 Uiso 1 1 calc R A -1 H58C H 0.0260 0.4333 0.3453 0.106 Uiso 1 1 calc R A -1 C59 C -0.2358(4) 0.4771(4) 0.5153(4) 0.093(4) Uani 1 1 d . A -1 H59A H -0.2731 0.4688 0.5374 0.140 Uiso 1 1 calc R A -1 H59B H -0.2491 0.4637 0.4783 0.140 Uiso 1 1 calc R A -1 H59C H -0.2292 0.5156 0.5142 0.140 Uiso 1 1 calc R A -1 C60 C -0.2179(4) 0.4308(4) 0.6289(4) 0.118(4) Uani 1 1 d . A -1 H60A H -0.2293 0.4676 0.6373 0.176 Uiso 1 1 calc R A -1 H60B H -0.2024 0.4117 0.6628 0.176 Uiso 1 1 calc R A -1 H60C H -0.2595 0.4134 0.6098 0.176 Uiso 1 1 calc R A -1 C61 C 0.0074(3) 0.2758(3) 0.5398(3) 0.056(2) Uani 1 1 d . A -1 H61 H 0.0248 0.2956 0.5119 0.067 Uiso 1 1 calc R A -1 C62 C -0.0249(4) 0.2265(3) 0.5260(3) 0.056(2) Uani 1 1 d . A -1 C63 C -0.0522(4) 0.1971(3) 0.5635(3) 0.062(3) Uani 1 1 d . A -1 C64 C -0.0465(4) 0.2190(3) 0.6164(3) 0.058(2) Uani 1 1 d . A -1 C65 C -0.0749(4) 0.1937(3) 0.6623(3) 0.079(3) Uani 1 1 d . A -1 H65 H -0.0984 0.1605 0.6570 0.095 Uiso 1 1 calc R A -1 C66 C -0.0682(4) 0.2168(3) 0.7122(3) 0.080(3) Uani 1 1 d . A -1 H66 H -0.0880 0.1993 0.7406 0.096 Uiso 1 1 calc R A -1 C67 C -0.0335(4) 0.2650(3) 0.7238(3) 0.056(2) Uani 1 1 d . A -1 C68 C -0.0232(4) 0.2874(3) 0.7756(3) 0.063(3) Uani 1 1 d . A -1 C69 C 0.0140(4) 0.3343(3) 0.7845(3) 0.056(2) Uani 1 1 d . A -1 C70 C 0.0418(4) 0.3564(3) 0.7403(3) 0.062(3) Uani 1 1 d . A -1 H70 H 0.0708 0.3870 0.7465 0.074 Uiso 1 1 calc R A -1 C71 C -0.0056(3) 0.2904(3) 0.6825(3) 0.046(2) Uani 1 1 d . A -1 C72 C -0.0128(3) 0.2677(3) 0.6280(3) 0.048(2) Uani 1 1 d . A -1 C73 C -0.0279(4) 0.2077(3) 0.4670(3) 0.077(3) Uani 1 1 d . A -1 H73A H -0.0035 0.1736 0.4662 0.115 Uiso 1 1 calc R A -1 H73B H -0.0050 0.2340 0.4461 0.115 Uiso 1 1 calc R A -1 H73C H -0.0769 0.2034 0.4511 0.115 Uiso 1 1 calc R A -1 C74 C -0.0869(5) 0.1457(3) 0.5495(3) 0.087(3) Uani 1 1 d . A -1 H74A H -0.1309 0.1517 0.5257 0.130 Uiso 1 1 calc R A -1 H74B H -0.0967 0.1279 0.5828 0.130 Uiso 1 1 calc R A -1 H74C H -0.0559 0.1232 0.5308 0.130 Uiso 1 1 calc R A -1 C75 C -0.0554(5) 0.2623(3) 0.8231(3) 0.090(3) Uani 1 1 d . A -1 H75A H -0.0180 0.2540 0.8527 0.135 Uiso 1 1 calc R A -1 H75B H -0.0802 0.2297 0.8107 0.135 Uiso 1 1 calc R A -1 H75C H -0.0884 0.2873 0.8362 0.135 Uiso 1 1 calc R A -1 C76 C 0.0306(5) 0.3621(3) 0.8379(3) 0.081(3) Uani 1 1 d . A -1 H76A H -0.0120 0.3791 0.8476 0.122 Uiso 1 1 calc R A -1 H76B H 0.0666 0.3891 0.8351 0.122 Uiso 1 1 calc R A -1 H76C H 0.0479 0.3363 0.8660 0.122 Uiso 1 1 calc R A -1 C77 C 0.2076(4) 0.2804(3) 0.7644(3) 0.060(3) Uani 1 1 d . A -1 H77 H 0.2257 0.2959 0.7341 0.072 Uiso 1 1 calc R A -1 C78 C 0.1634(4) 0.2358(3) 0.7547(3) 0.061(3) Uani 1 1 d . A -1 C79 C 0.1343(4) 0.2149(3) 0.7973(3) 0.061(3) Uani 1 1 d . A -1 C80 C 0.1501(4) 0.2391(3) 0.8480(3) 0.057(2) Uani 1 1 d . A -1 C81 C 0.1244(4) 0.2222(3) 0.8984(3) 0.077(3) Uani 1 1 d . A -1 H81 H 0.0920 0.1935 0.8964 0.092 Uiso 1 1 calc R A -1 C82 C 0.1435(4) 0.2443(3) 0.9464(3) 0.071(3) Uani 1 1 d . A -1 H82 H 0.1257 0.2299 0.9773 0.085 Uiso 1 1 calc R A -1 C83 C 0.1889(4) 0.2880(3) 0.9536(3) 0.061(3) Uani 1 1 d . A -1 C84 C 0.2094(4) 0.3138(4) 1.0034(3) 0.075(3) Uani 1 1 d . A -1 C85 C 0.2545(5) 0.3566(4) 1.0037(3) 0.076(3) Uani 1 1 d . A -1 C86 C 0.2756(4) 0.3729(3) 0.9554(3) 0.073(3) Uani 1 1 d . A -1 H86 H 0.3054 0.4032 0.9565 0.087 Uiso 1 1 calc R A -1 C87 C 0.2156(4) 0.3076(3) 0.9062(3) 0.056(2) Uani 1 1 d . A -1 C88 C 0.1959(4) 0.2828(3) 0.8544(3) 0.053(2) Uani 1 1 d . A -1 C89 C 0.1511(4) 0.2146(3) 0.6986(3) 0.079(3) Uani 1 1 d . A -1 H89A H 0.1766 0.1810 0.6969 0.119 Uiso 1 1 calc R A -1 H89B H 0.1679 0.2402 0.6735 0.119 Uiso 1 1 calc R A -1 H89C H 0.1008 0.2085 0.6883 0.119 Uiso 1 1 calc R A -1 C90 C 0.0895(4) 0.1663(3) 0.7891(3) 0.072(3) Uani 1 1 d . A -1 H90A H 0.0664 0.1652 0.7515 0.108 Uiso 1 1 calc R A -1 H90B H 0.0539 0.1672 0.8140 0.108 Uiso 1 1 calc R A -1 H90C H 0.1189 0.1346 0.7965 0.108 Uiso 1 1 calc R A -1 C91 C 0.1837(5) 0.2953(4) 1.0549(3) 0.107(4) Uani 1 1 d . A -1 H91A H 0.1904 0.2569 1.0587 0.161 Uiso 1 1 calc R A -1 H91B H 0.1337 0.3037 1.0536 0.161 Uiso 1 1 calc R A -1 H91C H 0.2102 0.3133 1.0861 0.161 Uiso 1 1 calc R A -1 C92 C 0.2786(6) 0.3873(4) 1.0557(4) 0.121(5) Uani 1 1 d . A -1 H92A H 0.2399 0.4093 1.0652 0.181 Uiso 1 1 calc R A -1 H92B H 0.3183 0.4101 1.0500 0.181 Uiso 1 1 calc R A -1 H92C H 0.2931 0.3623 1.0853 0.181 Uiso 1 1 calc R A -1 C93 C 0.3931(5) 0.2708(4) 0.8675(4) 0.100(4) Uani 1 1 d . A -1 H93 H 0.3568 0.2486 0.8504 0.120 Uiso 1 1 calc R A -1 C94 C 0.4551(5) 0.2477(4) 0.8939(4) 0.117(4) Uani 1 1 d . A -1 C95 C 0.5112(5) 0.2775(4) 0.9145(4) 0.111(4) Uani 1 1 d . A -1 C96 C 0.5024(5) 0.3342(4) 0.9162(4) 0.092(3) Uani 1 1 d . A -1 C97 C 0.5527(5) 0.3710(4) 0.9386(5) 0.121(5) Uani 1 1 d . A -1 H97 H 0.5962 0.3580 0.9562 0.145 Uiso 1 1 calc R A -1 C98 C 0.5430(5) 0.4220(4) 0.9365(4) 0.115(4) Uani 1 1 d . A -1 H98 H 0.5788 0.4445 0.9538 0.138 Uiso 1 1 calc R A -1 C99 C 0.4813(5) 0.4456(4) 0.9096(4) 0.086(3) Uani 1 1 d . A -1 C100 C 0.4703(5) 0.5014(4) 0.9064(3) 0.093(4) Uani 1 1 d . A -1 C101 C 0.4082(5) 0.5188(3) 0.8776(4) 0.081(3) Uani 1 1 d . A -1 C102 C 0.3563(4) 0.4789(3) 0.8564(3) 0.072(3) Uani 1 1 d . A -1 H102 H 0.3129 0.4909 0.8376 0.086 Uiso 1 1 calc R A -1 C103 C 0.4282(4) 0.4100(3) 0.8875(3) 0.071(3) Uani 1 1 d . A -1 C104 C 0.4400(4) 0.3545(3) 0.8895(3) 0.070(3) Uani 1 1 d . A -1 C105 C 0.4550(7) 0.1863(4) 0.8898(5) 0.175(6) Uani 1 1 d . A -1 H10A H 0.4927 0.1748 0.8693 0.263 Uiso 1 1 calc R A -1 H10B H 0.4098 0.1742 0.8711 0.263 Uiso 1 1 calc R A -1 H10C H 0.4626 0.1709 0.9264 0.263 Uiso 1 1 calc R A -1 C106 C 0.5785(6) 0.2517(5) 0.9414(5) 0.183(6) Uani 1 1 d . A -1 H10D H 0.5814 0.2552 0.9809 0.275 Uiso 1 1 calc R A -1 H10E H 0.6190 0.2694 0.9289 0.275 Uiso 1 1 calc R A -1 H10F H 0.5786 0.2140 0.9316 0.275 Uiso 1 1 calc R A -1 C107 C 0.5219(5) 0.5412(4) 0.9310(4) 0.121(4) Uani 1 1 d . A -1 H10G H 0.5657 0.5233 0.9452 0.182 Uiso 1 1 calc R A -1 H10H H 0.5029 0.5596 0.9608 0.182 Uiso 1 1 calc R A -1 H10I H 0.5311 0.5671 0.9033 0.182 Uiso 1 1 calc R A -1 C108 C 0.3879(5) 0.5762(3) 0.8673(4) 0.102(4) Uani 1 1 d . A -1 H10J H 0.3832 0.5937 0.9020 0.153 Uiso 1 1 calc R A -1 H10K H 0.3431 0.5780 0.8435 0.153 Uiso 1 1 calc R A -1 H10L H 0.4243 0.5942 0.8499 0.153 Uiso 1 1 calc R A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0330(5) 0.0670(7) 0.0484(6) 0.0104(5) 0.0090(5) -0.0011(5) Co2 0.0526(6) 0.0500(6) 0.0510(6) 0.0064(5) 0.0075(5) 0.0011(5) Co3 0.0338(5) 0.0467(6) 0.0639(7) 0.0006(5) 0.0098(5) -0.0009(5) Fe1 0.0343(5) 0.0510(6) 0.0590(7) 0.0026(6) 0.0073(5) 0.0001(5) Fe2 0.0545(6) 0.0567(7) 0.0519(7) 0.0042(6) 0.0185(5) 0.0102(6) N1 0.052(4) 0.102(5) 0.086(5) 0.014(4) 0.004(4) -0.003(4) N2 0.073(5) 0.065(5) 0.112(6) -0.009(4) -0.002(4) -0.006(4) N3 0.036(3) 0.100(5) 0.099(5) 0.003(4) 0.020(4) 0.002(4) N4 0.038(3) 0.071(4) 0.043(3) 0.008(3) 0.005(3) 0.004(3) N5 0.043(3) 0.054(4) 0.067(4) 0.002(3) 0.002(3) -0.009(3) N6 0.035(3) 0.055(4) 0.060(4) 0.004(3) 0.017(3) 0.003(3) N7 0.033(3) 0.058(4) 0.050(3) 0.021(3) 0.008(3) -0.004(3) N8 0.051(4) 0.059(4) 0.064(4) 0.005(3) 0.012(3) -0.001(3) N9 0.048(3) 0.046(4) 0.061(4) 0.000(3) 0.011(3) -0.002(3) N10 0.086(5) 0.075(5) 0.083(5) -0.004(4) 0.022(4) 0.019(4) N11 0.086(5) 0.140(7) 0.148(7) 0.031(6) 0.069(5) 0.030(5) N12 0.129(6) 0.087(5) 0.063(5) -0.012(4) 0.014(4) 0.013(5) N13 0.039(3) 0.070(4) 0.049(4) 0.013(3) 0.004(3) -0.004(3) N14 0.025(3) 0.079(4) 0.053(4) 0.002(3) 0.011(3) -0.003(3) N15 0.034(3) 0.082(4) 0.032(3) 0.001(3) 0.012(3) 0.006(3) N16 0.033(3) 0.074(4) 0.041(3) 0.009(3) 0.008(3) -0.005(3) N17 0.055(4) 0.071(4) 0.031(3) 0.005(3) 0.000(3) -0.005(3) N18 0.054(4) 0.088(5) 0.036(3) 0.013(3) 0.007(3) -0.001(3) N19 0.091(5) 0.068(4) 0.062(4) 0.013(4) 0.017(4) 0.027(4) N20 0.076(4) 0.042(4) 0.063(4) 0.004(3) 0.007(4) 0.005(3) N21 0.035(3) 0.035(3) 0.070(4) -0.006(3) 0.001(3) 0.004(3) N22 0.051(4) 0.040(4) 0.072(4) 0.002(3) 0.006(3) 0.008(3) N23 0.041(3) 0.054(4) 0.060(4) -0.004(3) 0.012(3) -0.005(3) N24 0.046(4) 0.075(4) 0.064(4) 0.000(4) 0.009(3) -0.002(3) C1 0.036(4) 0.084(6) 0.067(5) 0.010(5) 0.007(4) -0.006(4) C2 0.048(4) 0.064(5) 0.071(5) -0.015(5) 0.011(4) -0.006(4) C3 0.051(5) 0.064(5) 0.065(5) 0.003(4) 0.012(4) -0.003(4) C4 0.047(4) 0.050(4) 0.048(4) 0.010(4) 0.013(4) 0.006(4) C5 0.032(4) 0.047(5) 0.072(5) 0.004(4) 0.004(4) -0.004(3) C6 0.026(4) 0.049(4) 0.060(5) -0.001(4) 0.002(4) 0.000(4) C7 0.040(4) 0.056(5) 0.047(5) 0.010(4) 0.002(4) 0.006(4) C8 0.051(4) 0.063(5) 0.050(4) -0.004(4) 0.024(4) -0.005(4) C9 0.059(5) 0.044(4) 0.037(4) 0.006(4) -0.001(4) 0.010(4) C10 0.065(5) 0.069(6) 0.066(5) -0.003(5) 0.028(4) 0.012(4) C11 0.073(5) 0.108(7) 0.077(6) 0.015(5) 0.039(5) 0.021(5) C12 0.078(5) 0.078(6) 0.060(5) 0.012(5) 0.021(4) 0.028(5) C13 0.033(4) 0.056(5) 0.097(6) -0.027(4) 0.020(4) 0.007(4) C14 0.049(4) 0.070(5) 0.102(6) -0.024(5) 0.043(4) -0.004(4) C15 0.073(5) 0.075(5) 0.075(5) -0.025(5) 0.040(4) -0.036(4) C16 0.058(5) 0.058(5) 0.072(5) -0.005(4) 0.015(4) -0.020(4) C17 0.087(6) 0.089(6) 0.078(6) -0.008(5) 0.036(5) -0.007(5) C18 0.127(8) 0.087(7) 0.049(5) 0.001(5) 0.006(5) -0.015(6) C19 0.088(6) 0.067(6) 0.057(5) 0.009(5) 0.006(5) -0.016(5) C20 0.079(6) 0.092(7) 0.071(6) 0.005(5) 0.013(5) -0.009(5) C21 0.061(5) 0.051(5) 0.100(7) -0.005(5) -0.027(5) -0.006(4) C22 0.047(5) 0.083(6) 0.070(6) -0.007(5) -0.002(4) -0.007(4) C23 0.064(5) 0.064(5) 0.055(5) -0.008(4) 0.028(4) -0.006(4) C24 0.062(5) 0.064(5) 0.064(5) -0.018(4) 0.026(4) -0.017(4) C25 0.054(5) 0.100(7) 0.154(8) -0.044(6) 0.045(5) -0.011(5) C26 0.099(6) 0.132(8) 0.141(7) -0.023(7) 0.085(5) -0.041(6) C27 0.139(9) 0.139(9) 0.091(7) 0.052(7) -0.009(7) 0.041(7) C28 0.060(5) 0.088(6) 0.104(7) 0.014(6) -0.001(5) 0.014(5) C29 0.082(6) 0.053(5) 0.095(7) -0.003(5) 0.003(5) 0.014(5) C30 0.094(6) 0.021(4) 0.138(8) -0.004(5) 0.005(6) -0.011(4) C31 0.089(7) 0.058(6) 0.132(8) -0.012(6) -0.020(6) -0.028(5) C32 0.070(5) 0.022(4) 0.109(7) 0.004(4) -0.014(5) -0.010(4) C33 0.094(7) 0.062(6) 0.141(9) -0.014(6) -0.050(7) -0.021(5) C34 0.106(7) 0.050(6) 0.138(9) 0.005(6) -0.053(7) -0.004(5) C35 0.062(5) 0.054(5) 0.094(6) 0.002(5) -0.021(5) 0.002(4) C36 0.061(5) 0.065(6) 0.091(6) 0.000(5) -0.003(5) 0.023(4) C37 0.050(4) 0.039(4) 0.085(6) -0.010(4) 0.004(4) 0.004(4) C38 0.043(4) 0.050(5) 0.079(6) -0.006(4) 0.009(4) 0.005(4) C39 0.060(5) 0.042(5) 0.056(5) 0.010(4) 0.002(4) 0.012(4) C40 0.046(4) 0.048(5) 0.071(5) 0.003(4) 0.003(4) 0.006(4) C41 0.118(8) 0.065(6) 0.136(9) 0.010(6) -0.028(7) 0.000(6) C42 0.174(10) 0.060(7) 0.179(11) -0.002(7) -0.084(9) -0.019(7) C43 0.100(7) 0.066(6) 0.168(10) 0.011(7) -0.049(7) 0.002(6) C44 0.087(6) 0.053(5) 0.102(7) 0.010(5) -0.007(6) 0.007(5) C45 0.048(4) 0.063(5) 0.062(5) 0.015(4) 0.016(4) -0.013(4) C46 0.058(5) 0.061(5) 0.048(5) 0.018(4) 0.009(4) -0.009(4) C47 0.075(5) 0.052(5) 0.054(5) 0.014(4) 0.002(4) -0.008(4) C48 0.061(5) 0.050(5) 0.062(5) 0.019(4) -0.006(4) -0.008(4) C49 0.061(5) 0.074(6) 0.070(6) 0.008(5) 0.005(5) 0.011(5) C50 0.069(5) 0.063(5) 0.070(6) 0.001(5) -0.036(5) 0.004(5) C51 0.024(4) 0.070(5) 0.091(6) -0.017(5) 0.000(4) -0.007(4) C52 0.059(5) 0.067(5) 0.080(6) -0.028(5) -0.017(5) 0.005(4) C53 0.038(4) 0.096(6) 0.103(7) -0.027(6) 0.013(5) -0.006(5) C54 0.050(5) 0.088(6) 0.082(6) -0.004(5) 0.020(5) -0.016(5) C55 0.029(4) 0.050(5) 0.062(5) 0.001(4) 0.007(4) 0.004(3) C56 0.045(4) 0.061(5) 0.064(5) 0.004(4) 0.001(4) 0.002(4) C57 0.077(6) 0.103(7) 0.080(6) 0.024(5) 0.031(5) 0.002(5) C58 0.080(6) 0.072(6) 0.061(5) 0.013(5) 0.008(5) 0.011(5) C59 0.045(5) 0.098(7) 0.131(8) -0.017(6) -0.007(5) 0.015(5) C60 0.048(5) 0.156(9) 0.158(9) -0.014(8) 0.050(6) 0.013(6) C61 0.038(4) 0.091(6) 0.044(4) 0.020(4) 0.025(3) 0.004(4) C62 0.048(4) 0.070(5) 0.054(5) -0.004(4) 0.017(4) -0.005(4) C63 0.066(5) 0.079(6) 0.045(5) -0.007(4) 0.022(4) -0.017(4) C64 0.045(4) 0.074(5) 0.055(5) 0.016(4) 0.012(4) -0.019(4) C65 0.075(6) 0.065(6) 0.098(7) 0.007(5) 0.011(5) -0.026(5) C66 0.105(6) 0.084(6) 0.054(5) -0.013(5) 0.024(5) -0.045(5) C67 0.064(5) 0.070(5) 0.038(4) -0.001(4) 0.018(4) -0.021(4) C68 0.062(5) 0.073(5) 0.057(5) 0.010(4) 0.020(4) -0.006(4) C69 0.080(5) 0.064(5) 0.027(4) 0.008(4) 0.016(4) -0.007(4) C70 0.062(5) 0.077(6) 0.047(5) 0.000(5) 0.009(4) -0.005(4) C71 0.033(4) 0.052(5) 0.053(5) -0.001(4) 0.007(4) -0.011(4) C72 0.042(4) 0.073(5) 0.029(4) 0.008(4) 0.002(3) -0.010(4) C73 0.091(6) 0.074(6) 0.064(6) -0.013(5) 0.008(5) -0.001(5) C74 0.095(6) 0.091(7) 0.074(6) -0.022(5) 0.009(5) -0.035(5) C75 0.135(7) 0.095(6) 0.044(5) 0.001(5) 0.032(5) -0.053(6) C76 0.102(6) 0.091(6) 0.052(5) 0.003(5) 0.016(5) -0.021(5) C77 0.059(5) 0.075(6) 0.046(5) 0.012(4) 0.008(4) -0.005(4) C78 0.071(5) 0.065(5) 0.047(5) -0.002(4) 0.011(4) -0.019(4) C79 0.063(5) 0.064(5) 0.057(5) -0.006(4) 0.005(4) -0.013(4) C80 0.044(4) 0.057(5) 0.076(5) 0.015(4) 0.029(4) -0.006(4) C81 0.056(5) 0.069(6) 0.111(7) 0.016(5) 0.034(5) -0.013(4) C82 0.069(5) 0.100(7) 0.042(5) 0.008(5) 0.007(4) -0.014(5) C83 0.047(5) 0.080(6) 0.051(5) 0.012(5) -0.013(4) 0.002(4) C84 0.065(5) 0.103(7) 0.056(5) 0.006(5) -0.001(5) 0.003(5) C85 0.082(6) 0.117(7) 0.025(4) -0.006(5) -0.010(4) 0.001(6) C86 0.090(6) 0.081(6) 0.047(5) 0.008(5) 0.008(5) -0.009(5) C87 0.041(4) 0.082(6) 0.044(5) 0.017(4) 0.005(4) 0.006(4) C88 0.046(4) 0.065(5) 0.046(5) 0.007(4) 0.001(4) 0.006(4) C89 0.061(5) 0.087(6) 0.092(6) -0.008(5) 0.018(5) -0.020(5) C90 0.072(5) 0.063(5) 0.085(6) 0.008(5) 0.025(5) -0.017(5) C91 0.111(7) 0.170(10) 0.043(5) 0.016(6) 0.016(5) -0.042(7) C92 0.125(9) 0.151(10) 0.084(7) -0.016(7) 0.004(7) -0.010(8) C93 0.136(8) 0.075(6) 0.095(7) 0.009(6) 0.039(6) 0.020(6) C94 0.103(7) 0.087(6) 0.159(9) 0.068(6) 0.013(7) 0.064(5) C95 0.081(7) 0.132(8) 0.118(8) 0.054(7) 0.004(6) 0.032(6) C96 0.089(6) 0.089(6) 0.098(7) 0.040(6) 0.016(5) 0.044(5) C97 0.067(6) 0.134(9) 0.151(10) -0.002(8) -0.024(7) 0.016(7) C98 0.086(7) 0.128(9) 0.117(8) 0.002(7) -0.037(7) 0.011(7) C99 0.073(6) 0.084(6) 0.096(7) -0.007(6) -0.009(6) -0.001(5) C100 0.073(6) 0.138(8) 0.061(6) -0.005(6) -0.017(5) 0.019(6) C101 0.106(7) 0.054(5) 0.085(6) -0.025(5) 0.019(5) -0.021(5) C102 0.059(5) 0.091(6) 0.064(5) 0.004(5) 0.006(4) 0.010(5) C103 0.055(5) 0.095(6) 0.063(5) 0.022(5) 0.004(4) 0.032(5) C104 0.076(5) 0.061(5) 0.075(6) 0.020(5) 0.016(5) 0.029(5) C105 0.273(14) 0.075(7) 0.181(12) 0.037(8) 0.043(11) 0.095(8) C106 0.150(9) 0.189(10) 0.199(13) 0.065(9) -0.020(9) 0.121(8) C107 0.089(7) 0.117(8) 0.146(9) -0.036(7) -0.026(7) -0.042(6) C108 0.091(7) 0.050(5) 0.167(9) -0.032(6) 0.023(7) -0.016(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N4 2.062(5) . ? Co1 N7 2.089(6) . ? Co1 N14 2.140(5) . ? Co1 N13 2.155(6) . ? Co1 N16 2.160(5) . ? Co1 N15 2.169(6) . ? Co2 N5 2.066(6) . ? Co2 N8 2.067(6) . ? Co2 N20 2.126(6) . ? Co2 N17 2.129(6) . ? Co2 N18 2.130(6) . ? Co2 N19 2.148(6) . ? Co3 N9 2.019(6) . ? Co3 N6 2.094(6) . ? Co3 N21 2.107(5) . ? Co3 N23 2.131(6) . ? Co3 N24 2.139(6) . ? Co3 N22 2.170(6) . ? Fe1 C1 1.869(8) . ? Fe1 C5 1.902(8) . ? Fe1 C2 1.906(8) . ? Fe1 C6 1.923(7) . ? Fe1 C4 1.932(7) . ? Fe1 C3 1.953(8) . ? Fe2 C7 1.906(7) . ? Fe2 C12 1.906(8) . ? Fe2 C9 1.908(8) . ? Fe2 C10 1.910(8) . ? Fe2 C8 1.914(7) . ? Fe2 C11 1.955(9) . ? N1 C1 1.179(10) . ? N2 C2 1.149(10) . ? N3 C3 1.159(9) . ? N4 C4 1.140(8) . ? N5 C5 1.160(9) . ? N6 C6 1.162(8) . ? N7 C7 1.183(8) . ? N8 C8 1.167(9) . ? N9 C9 1.165(9) . ? N10 C10 1.186(10) . ? N11 C11 1.129(11) . ? N12 C12 1.164(10) . ? N13 C45 1.339(9) . ? N13 C56 1.346(9) . ? N14 C54 1.328(9) . ? N14 C55 1.349(9) . ? N15 C61 1.333(8) . ? N15 C72 1.347(8) . ? N16 C70 1.347(9) . ? N16 C71 1.355(8) . ? N17 C77 1.309(9) . ? N17 C88 1.348(9) . ? N18 C86 1.298(9) . ? N18 C87 1.356(9) . ? N19 C93 1.357(11) . ? N19 C104 1.375(10) . ? N20 C102 1.294(10) . ? N20 C103 1.361(9) . ? N21 C38 1.288(8) . ? N21 C39 1.376(9) . ? N22 C29 1.335(9) . ? N22 C40 1.379(9) . ? N23 C13 1.331(8) . ? N23 C24 1.353(9) . ? N24 C22 1.346(9) . ? N24 C23 1.348(9) . ? C13 C14 1.339(11) . ? C14 C15 1.364(11) . ? C14 C25 1.511(10) . ? C15 C16 1.433(11) . ? C15 C26 1.501(12) . ? C16 C24 1.398(11) . ? C16 C17 1.402(11) . ? C17 C18 1.393(12) . ? C18 C19 1.434(12) . ? C19 C23 1.389(10) . ? C19 C20 1.403(12) . ? C20 C21 1.411(12) . ? C20 C27 1.491(12) . ? C21 C22 1.393(11) . ? C21 C28 1.533(11) . ? C23 C24 1.457(10) . ? C29 C30 1.363(11) . ? C30 C31 1.361(12) . ? C30 C41 1.533(11) . ? C31 C32 1.439(11) . ? C31 C42 1.484(12) . ? C32 C40 1.400(10) . ? C32 C33 1.451(12) . ? C33 C34 1.309(12) . ? C34 C35 1.445(11) . ? C35 C39 1.396(10) . ? C35 C36 1.419(11) . ? C36 C37 1.372(10) . ? C36 C43 1.531(11) . ? C37 C38 1.397(10) . ? C37 C44 1.525(10) . ? C39 C40 1.419(10) . ? C45 C46 1.393(10) . ? C46 C47 1.368(10) . ? C46 C57 1.529(11) . ? C47 C48 1.433(11) . ? C47 C58 1.526(10) . ? C48 C49 1.394(10) . ? C48 C56 1.419(10) . ? C49 C50 1.341(11) . ? C50 C51 1.427(11) . ? C51 C52 1.405(11) . ? C51 C55 1.423(9) . ? C52 C53 1.416(12) . ? C52 C59 1.547(11) . ? C53 C54 1.447(11) . ? C53 C60 1.474(12) . ? C55 C56 1.451(10) . ? C61 C62 1.410(10) . ? C62 C63 1.346(10) . ? C62 C73 1.532(10) . ? C63 C64 1.415(10) . ? C63 C74 1.478(11) . ? C64 C72 1.400(10) . ? C64 C65 1.471(11) . ? C65 C66 1.359(11) . ? C66 C67 1.398(11) . ? C67 C71 1.375(10) . ? C67 C68 1.393(10) . ? C68 C69 1.383(10) . ? C68 C75 1.536(11) . ? C69 C70 1.397(10) . ? C69 C76 1.496(10) . ? C71 C72 1.459(9) . ? C77 C78 1.410(10) . ? C78 C79 1.365(11) . ? C78 C89 1.480(11) . ? C79 C80 1.397(10) . ? C79 C90 1.496(10) . ? C80 C88 1.405(10) . ? C80 C81 1.465(11) . ? C81 C82 1.323(11) . ? C82 C83 1.403(11) . ? C83 C84 1.404(11) . ? C83 C87 1.431(10) . ? C84 C85 1.382(12) . ? C84 C91 1.503(11) . ? C85 C86 1.379(11) . ? C85 C92 1.523(12) . ? C87 C88 1.432(10) . ? C93 C94 1.408(13) . ? C94 C95 1.358(14) . ? C94 C105 1.551(13) . ? C95 C96 1.439(13) . ? C95 C106 1.522(14) . ? C96 C104 1.392(11) . ? C96 C97 1.402(13) . ? C97 C98 1.298(14) . ? C98 C99 1.414(13) . ? C99 C103 1.415(12) . ? C99 C100 1.424(13) . ? C100 C101 1.380(12) . ? C100 C107 1.484(13) . ? C101 C102 1.466(11) . ? C101 C108 1.511(11) . ? C103 C104 1.414(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N7 91.1(2) . . ? N4 Co1 N14 167.7(2) . . ? N7 Co1 N14 91.0(2) . . ? N4 Co1 N13 91.0(2) . . ? N7 Co1 N13 99.6(2) . . ? N14 Co1 N13 76.6(2) . . ? N4 Co1 N16 97.1(2) . . ? N7 Co1 N16 91.2(2) . . ? N14 Co1 N16 95.0(2) . . ? N13 Co1 N16 166.4(2) . . ? N4 Co1 N15 95.6(2) . . ? N7 Co1 N15 165.8(2) . . ? N14 Co1 N15 85.1(2) . . ? N13 Co1 N15 92.8(2) . . ? N16 Co1 N15 75.6(2) . . ? N5 Co2 N8 94.5(2) . . ? N5 Co2 N20 93.7(2) . . ? N8 Co2 N20 93.7(2) . . ? N5 Co2 N17 91.0(2) . . ? N8 Co2 N17 91.7(2) . . ? N20 Co2 N17 172.5(2) . . ? N5 Co2 N18 166.5(2) . . ? N8 Co2 N18 93.8(2) . . ? N20 Co2 N18 96.4(2) . . ? N17 Co2 N18 78.1(2) . . ? N5 Co2 N19 90.3(2) . . ? N8 Co2 N19 169.3(2) . . ? N20 Co2 N19 76.4(2) . . ? N17 Co2 N19 97.8(2) . . ? N18 Co2 N19 83.3(2) . . ? N9 Co3 N6 91.1(2) . . ? N9 Co3 N21 97.3(2) . . ? N6 Co3 N21 95.2(2) . . ? N9 Co3 N23 173.5(2) . . ? N6 Co3 N23 88.9(2) . . ? N21 Co3 N23 89.2(2) . . ? N9 Co3 N24 96.0(2) . . ? N6 Co3 N24 99.4(2) . . ? N21 Co3 N24 160.0(2) . . ? N23 Co3 N24 77.5(2) . . ? N9 Co3 N22 93.4(2) . . ? N6 Co3 N22 171.6(2) . . ? N21 Co3 N22 77.2(2) . . ? N23 Co3 N22 87.5(2) . . ? N24 Co3 N22 87.2(2) . . ? C1 Fe1 C5 177.2(3) . . ? C1 Fe1 C2 89.1(3) . . ? C5 Fe1 C2 88.8(3) . . ? C1 Fe1 C6 95.5(3) . . ? C5 Fe1 C6 86.6(3) . . ? C2 Fe1 C6 175.3(3) . . ? C1 Fe1 C4 89.4(3) . . ? C5 Fe1 C4 88.6(3) . . ? C2 Fe1 C4 87.6(3) . . ? C6 Fe1 C4 93.0(3) . . ? C1 Fe1 C3 90.2(3) . . ? C5 Fe1 C3 91.8(3) . . ? C2 Fe1 C3 92.5(3) . . ? C6 Fe1 C3 86.9(3) . . ? C4 Fe1 C3 179.6(3) . . ? C7 Fe2 C12 176.5(3) . . ? C7 Fe2 C9 90.5(3) . . ? C12 Fe2 C9 91.0(3) . . ? C7 Fe2 C10 94.0(3) . . ? C12 Fe2 C10 89.2(3) . . ? C9 Fe2 C10 86.7(3) . . ? C7 Fe2 C8 87.2(3) . . ? C12 Fe2 C8 89.6(3) . . ? C9 Fe2 C8 87.7(3) . . ? C10 Fe2 C8 174.3(3) . . ? C7 Fe2 C11 87.4(3) . . ? C12 Fe2 C11 91.2(4) . . ? C9 Fe2 C11 177.6(3) . . ? C10 Fe2 C11 92.2(4) . . ? C8 Fe2 C11 93.4(3) . . ? C4 N4 Co1 157.7(6) . . ? C5 N5 Co2 163.1(5) . . ? C6 N6 Co3 159.7(5) . . ? C7 N7 Co1 162.8(5) . . ? C8 N8 Co2 161.5(6) . . ? C9 N9 Co3 165.0(5) . . ? C45 N13 C56 116.1(6) . . ? C45 N13 Co1 129.1(5) . . ? C56 N13 Co1 114.7(5) . . ? C54 N14 C55 117.7(6) . . ? C54 N14 Co1 127.1(5) . . ? C55 N14 Co1 115.2(4) . . ? C61 N15 C72 116.5(6) . . ? C61 N15 Co1 127.6(5) . . ? C72 N15 Co1 115.8(4) . . ? C70 N16 C71 117.0(6) . . ? C70 N16 Co1 127.2(5) . . ? C71 N16 Co1 115.8(4) . . ? C77 N17 C88 117.8(6) . . ? C77 N17 Co2 128.2(5) . . ? C88 N17 Co2 113.9(4) . . ? C86 N18 C87 117.8(6) . . ? C86 N18 Co2 129.2(6) . . ? C87 N18 Co2 112.8(5) . . ? C93 N19 C104 117.1(7) . . ? C93 N19 Co2 127.5(6) . . ? C104 N19 Co2 115.4(5) . . ? C102 N20 C103 119.2(7) . . ? C102 N20 Co2 126.1(5) . . ? C103 N20 Co2 114.7(5) . . ? C38 N21 C39 116.0(6) . . ? C38 N21 Co3 129.2(5) . . ? C39 N21 Co3 113.9(4) . . ? C29 N22 C40 116.3(6) . . ? C29 N22 Co3 130.2(5) . . ? C40 N22 Co3 113.3(4) . . ? C13 N23 C24 116.8(6) . . ? C13 N23 Co3 129.6(5) . . ? C24 N23 Co3 113.5(5) . . ? C22 N24 C23 117.9(6) . . ? C22 N24 Co3 126.4(5) . . ? C23 N24 Co3 115.4(5) . . ? N1 C1 Fe1 177.1(7) . . ? N2 C2 Fe1 177.2(7) . . ? N3 C3 Fe1 177.1(7) . . ? N4 C4 Fe1 179.0(7) . . ? N5 C5 Fe1 175.0(6) . . ? N6 C6 Fe1 170.9(6) . . ? N7 C7 Fe2 174.6(6) . . ? N8 C8 Fe2 174.6(6) . . ? N9 C9 Fe2 177.4(6) . . ? N10 C10 Fe2 177.1(7) . . ? N11 C11 Fe2 178.7(9) . . ? N12 C12 Fe2 176.6(8) . . ? N23 C13 C14 125.2(7) . . ? C13 C14 C15 120.6(7) . . ? C13 C14 C25 118.5(7) . . ? C15 C14 C25 120.9(7) . . ? C14 C15 C16 116.7(7) . . ? C14 C15 C26 122.2(7) . . ? C16 C15 C26 121.1(7) . . ? C24 C16 C17 118.6(7) . . ? C24 C16 C15 118.6(7) . . ? C17 C16 C15 122.8(8) . . ? C18 C17 C16 120.9(8) . . ? C17 C18 C19 123.1(8) . . ? C23 C19 C20 120.9(8) . . ? C23 C19 C18 115.1(8) . . ? C20 C19 C18 124.0(8) . . ? C19 C20 C21 115.8(8) . . ? C19 C20 C27 125.5(8) . . ? C21 C20 C27 118.5(8) . . ? C22 C21 C20 120.0(8) . . ? C22 C21 C28 116.8(8) . . ? C20 C21 C28 123.1(7) . . ? N24 C22 C21 122.9(8) . . ? N24 C23 C19 122.3(7) . . ? N24 C23 C24 115.0(7) . . ? C19 C23 C24 122.7(7) . . ? N23 C24 C16 122.0(7) . . ? N23 C24 C23 118.5(7) . . ? C16 C24 C23 119.4(7) . . ? N22 C29 C30 125.9(8) . . ? C31 C30 C29 119.0(7) . . ? C31 C30 C41 121.9(7) . . ? C29 C30 C41 119.0(8) . . ? C30 C31 C32 118.7(7) . . ? C30 C31 C42 121.2(8) . . ? C32 C31 C42 120.1(8) . . ? C40 C32 C31 117.8(7) . . ? C40 C32 C33 116.3(7) . . ? C31 C32 C33 125.8(7) . . ? C34 C33 C32 122.0(8) . . ? C33 C34 C35 122.3(8) . . ? C39 C35 C36 118.6(7) . . ? C39 C35 C34 117.9(7) . . ? C36 C35 C34 123.5(7) . . ? C37 C36 C35 118.2(7) . . ? C37 C36 C43 121.0(7) . . ? C35 C36 C43 120.7(7) . . ? C36 C37 C38 117.5(7) . . ? C36 C37 C44 122.8(7) . . ? C38 C37 C44 119.6(7) . . ? N21 C38 C37 127.1(7) . . ? N21 C39 C35 122.4(6) . . ? N21 C39 C40 118.2(6) . . ? C35 C39 C40 119.4(7) . . ? N22 C40 C32 122.2(6) . . ? N22 C40 C39 115.7(6) . . ? C32 C40 C39 122.1(7) . . ? N13 C45 C46 124.9(7) . . ? C47 C46 C45 118.9(7) . . ? C47 C46 C57 122.7(7) . . ? C45 C46 C57 118.5(6) . . ? C46 C47 C48 119.2(7) . . ? C46 C47 C58 123.5(7) . . ? C48 C47 C58 117.3(7) . . ? C49 C48 C56 119.9(7) . . ? C49 C48 C47 123.7(7) . . ? C56 C48 C47 116.3(7) . . ? C50 C49 C48 122.4(8) . . ? C49 C50 C51 120.7(7) . . ? C52 C51 C55 116.7(7) . . ? C52 C51 C50 123.8(7) . . ? C55 C51 C50 119.4(7) . . ? C51 C52 C53 120.5(7) . . ? C51 C52 C59 120.2(7) . . ? C53 C52 C59 119.3(8) . . ? C52 C53 C54 116.5(7) . . ? C52 C53 C60 125.3(7) . . ? C54 C53 C60 118.2(8) . . ? N14 C54 C53 123.9(8) . . ? N14 C55 C51 124.6(6) . . ? N14 C55 C56 116.6(6) . . ? C51 C55 C56 118.8(7) . . ? N13 C56 C48 124.5(7) . . ? N13 C56 C55 116.8(6) . . ? C48 C56 C55 118.7(6) . . ? N15 C61 C62 123.7(7) . . ? C63 C62 C61 121.0(7) . . ? C63 C62 C73 121.3(7) . . ? C61 C62 C73 117.7(7) . . ? C62 C63 C64 115.9(7) . . ? C62 C63 C74 121.7(7) . . ? C64 C63 C74 122.5(7) . . ? C72 C64 C63 120.7(7) . . ? C72 C64 C65 115.4(7) . . ? C63 C64 C65 124.0(7) . . ? C66 C65 C64 121.2(7) . . ? C65 C66 C67 123.2(8) . . ? C71 C67 C68 118.4(7) . . ? C71 C67 C66 118.2(7) . . ? C68 C67 C66 123.3(7) . . ? C69 C68 C67 120.1(7) . . ? C69 C68 C75 118.7(7) . . ? C67 C68 C75 121.1(7) . . ? C68 C69 C70 117.3(7) . . ? C68 C69 C76 125.9(7) . . ? C70 C69 C76 116.7(7) . . ? N16 C70 C69 123.7(7) . . ? N16 C71 C67 123.3(6) . . ? N16 C71 C72 116.2(6) . . ? C67 C71 C72 120.6(6) . . ? N15 C72 C64 122.3(6) . . ? N15 C72 C71 116.3(6) . . ? C64 C72 C71 121.4(6) . . ? N17 C77 C78 124.7(7) . . ? C79 C78 C77 118.3(7) . . ? C79 C78 C89 123.8(7) . . ? C77 C78 C89 117.9(7) . . ? C78 C79 C80 117.8(7) . . ? C78 C79 C90 119.9(7) . . ? C80 C79 C90 122.2(7) . . ? C79 C80 C88 120.2(7) . . ? C79 C80 C81 125.6(7) . . ? C88 C80 C81 114.1(7) . . ? C82 C81 C80 124.0(7) . . ? C81 C82 C83 122.8(8) . . ? C82 C83 C84 125.1(7) . . ? C82 C83 C87 116.6(7) . . ? C84 C83 C87 118.3(7) . . ? C85 C84 C83 118.1(8) . . ? C85 C84 C91 120.7(7) . . ? C83 C84 C91 121.2(8) . . ? C86 C85 C84 118.8(7) . . ? C86 C85 C92 119.5(8) . . ? C84 C85 C92 121.6(8) . . ? N18 C86 C85 125.5(8) . . ? N18 C87 C83 121.4(7) . . ? N18 C87 C88 118.2(6) . . ? C83 C87 C88 120.4(7) . . ? N17 C88 C80 121.0(7) . . ? N17 C88 C87 116.8(6) . . ? C80 C88 C87 122.1(7) . . ? N19 C93 C94 120.9(9) . . ? C95 C94 C93 122.0(9) . . ? C95 C94 C105 124.7(9) . . ? C93 C94 C105 112.8(9) . . ? C94 C95 C96 117.9(9) . . ? C94 C95 C106 121.2(10) . . ? C96 C95 C106 120.4(9) . . ? C104 C96 C97 116.9(8) . . ? C104 C96 C95 116.7(8) . . ? C97 C96 C95 126.3(9) . . ? C98 C97 C96 123.5(9) . . ? C97 C98 C99 122.8(10) . . ? C98 C99 C103 115.9(8) . . ? C98 C99 C100 123.4(9) . . ? C103 C99 C100 120.7(8) . . ? C101 C100 C99 117.0(8) . . ? C101 C100 C107 119.0(9) . . ? C99 C100 C107 123.9(8) . . ? C100 C101 C102 118.1(8) . . ? C100 C101 C108 125.3(8) . . ? C102 C101 C108 116.6(8) . . ? N20 C102 C101 123.9(7) . . ? N20 C103 C104 118.5(7) . . ? N20 C103 C99 120.9(8) . . ? C104 C103 C99 120.5(7) . . ? N19 C104 C96 124.7(8) . . ? N19 C104 C103 114.9(7) . . ? C96 C104 C103 120.3(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.888 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.170 #end================================ data_{[Co(tmphen)2]3[Fe(CN)6]2}_220K #================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; '{[Co(tmphen)2]3[Fe(CN)6]2}.9H2O' ; _chemical_name_common '{[Co(tmphen)2]3[Fe(CN)6]2}.9H2O' _chemical_melting_point ? _chemical_formula_moiety 'C108 H114 Co3 Fe2 N24 O9' _chemical_formula_sum 'C108 H114 Co3 Fe2 N24 O9' _chemical_formula_weight 2180.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.261(4) _cell_length_b 25.123(5) _cell_length_c 24.782(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.74(3) _cell_angle_gamma 90.00 _cell_volume 11883(4) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 38768 _cell_measurement_theta_min 2.133 _cell_measurement_theta_max 14.214 _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4468 _exptl_absorpt_coefficient_mu 0.709 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8482 _exptl_absorpt_correction_T_max 0.8829 _exptl_absorpt_process_details 'SADABS: Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'BRUKER APEX' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38768 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 20.81 _reflns_number_total 12433 _reflns_number_gt 8615 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER, 2000)' _computing_cell_refinement 'SAINT (BRUKER, 2001)' _computing_data_reduction 'SAINT (BRUKER, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1597P)^2^+21.58P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00000(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12433 _refine_ls_number_parameters 1379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.2545 _refine_ls_wR_factor_gt 0.2234 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 2.320 _refine_ls_shift/su_mean 0.013 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.06178(5) 0.37248(5) 0.61755(4) 0.0487(4) Uani 1 1 d . . . Co3 Co 0.35631(5) 0.54662(4) 0.66314(4) 0.0453(4) Uani 1 1 d . . . Co2 Co 0.29483(6) 0.36921(4) 0.83337(4) 0.0516(4) Uani 1 1 d . . . Fe1 Fe 0.32422(6) 0.35018(5) 0.63514(5) 0.0475(4) Uani 1 1 d . . . Fe2 Fe 0.14044(6) 0.51950(5) 0.75411(5) 0.0538(4) Uani 1 1 d . . . N15 N 0.0155(3) 0.2964(3) 0.5902(3) 0.0501(18) Uani 1 1 d . . . N13 N 0.0717(3) 0.3971(3) 0.5357(3) 0.0526(18) Uani 1 1 d . . . N21 N 0.4370(3) 0.5196(3) 0.7232(3) 0.0503(18) Uani 1 1 d . . . N4 N 0.1639(4) 0.3459(3) 0.6286(3) 0.0506(18) Uani 1 1 d . . . C4 C 0.2229(5) 0.3473(3) 0.6309(3) 0.046(2) Uani 1 1 d . . . N6 N 0.3304(3) 0.4727(3) 0.6309(3) 0.0536(18) Uani 1 1 d . . . N22 N 0.3973(4) 0.6191(3) 0.7004(3) 0.0552(19) Uani 1 1 d . . . N9 N 0.2779(4) 0.5434(3) 0.7090(3) 0.0557(19) Uani 1 1 d . . . N7 N 0.0928(3) 0.4430(3) 0.6594(3) 0.0528(19) Uani 1 1 d . . . C5 C 0.3294(4) 0.3616(3) 0.7126(5) 0.053(2) Uani 1 1 d . . . N8 N 0.2162(4) 0.4220(3) 0.8107(3) 0.0563(19) Uani 1 1 d . . . N20 N 0.3660(4) 0.4294(3) 0.8626(3) 0.0600(19) Uani 1 1 d . . . N16 N 0.0314(3) 0.3383(3) 0.6905(3) 0.0553(19) Uani 1 1 d . . . N14 N -0.0398(3) 0.4055(3) 0.5892(3) 0.0534(18) Uani 1 1 d . . . N24 N 0.3021(4) 0.5944(3) 0.6008(3) 0.0567(19) Uani 1 1 d . . . C8 C 0.1843(4) 0.4584(4) 0.7905(4) 0.054(2) Uani 1 1 d . . . N5 N 0.3277(4) 0.3673(3) 0.7585(4) 0.058(2) Uani 1 1 d . . . C7 C 0.1108(4) 0.4736(4) 0.6931(4) 0.047(2) Uani 1 1 d . . . N23 N 0.4295(3) 0.5541(3) 0.6072(3) 0.0532(18) Uani 1 1 d . . . C108 C 0.4080(4) 0.5831(3) 0.5629(4) 0.055(2) Uani 1 1 d . . . N17 N 0.2276(4) 0.3038(3) 0.8133(3) 0.0572(19) Uani 1 1 d . . . N18 N 0.2594(4) 0.3523(3) 0.9091(3) 0.064(2) Uani 1 1 d . . . C6 C 0.3247(4) 0.4265(4) 0.6282(3) 0.049(2) Uani 1 1 d . . . C47 C -0.0481(4) 0.4242(3) 0.5378(4) 0.051(2) Uani 1 1 d . . . C59 C -0.0048(4) 0.2921(3) 0.6829(3) 0.050(2) Uani 1 1 d . . . C58 C 0.0420(4) 0.3583(4) 0.7402(4) 0.060(2) Uani 1 1 d . . . H58 H 0.0691 0.3894 0.7458 0.072 Uiso 1 1 calc R . . C10 C 0.1055(5) 0.5824(4) 0.7159(4) 0.063(3) Uani 1 1 d . . . C60 C -0.0120(4) 0.2686(4) 0.6292(3) 0.051(2) Uani 1 1 d . . . C96 C 0.4801(4) 0.5595(3) 0.7466(4) 0.055(2) Uani 1 1 d . . . C95 C 0.4581(5) 0.6124(3) 0.7345(4) 0.060(2) Uani 1 1 d . . . C103 C 0.3119(6) 0.6402(4) 0.5166(4) 0.071(3) Uani 1 1 d . . . C39 C 0.0655(5) 0.4311(3) 0.4265(3) 0.058(2) Uani 1 1 d . . . C85 C 0.4557(4) 0.4703(4) 0.7348(3) 0.055(2) Uani 1 1 d . . . H85 H 0.4259 0.4431 0.7194 0.066 Uiso 1 1 calc R . . N3 N 0.4860(4) 0.3556(4) 0.6407(4) 0.081(3) Uani 1 1 d . . . N19 N 0.3854(5) 0.3264(4) 0.8673(3) 0.080(3) Uani 1 1 d . . . C48 C 0.0114(4) 0.4196(3) 0.5082(3) 0.053(2) Uani 1 1 d . . . C3 C 0.4258(5) 0.3527(3) 0.6389(3) 0.056(2) Uani 1 1 d . . . C50 C -0.0243(4) 0.2264(4) 0.5263(3) 0.058(2) Uani 1 1 d . . . C37 C 0.1256(5) 0.3918(3) 0.5077(4) 0.058(2) Uani 1 1 d . . . H37 H 0.1665 0.3759 0.5256 0.069 Uiso 1 1 calc R . . C49 C 0.0079(4) 0.2751(4) 0.5405(3) 0.053(2) Uani 1 1 d . . . H49 H 0.0257 0.2943 0.5129 0.064 Uiso 1 1 calc R . . C105 C 0.2093(5) 0.6522(4) 0.5596(4) 0.069(3) Uani 1 1 d . . . C51 C -0.0515(5) 0.1980(4) 0.5655(4) 0.061(2) Uani 1 1 d . . . C97 C 0.4936(5) 0.5333(4) 0.6109(4) 0.061(2) Uani 1 1 d . . . H97 H 0.5093 0.5134 0.6423 0.074 Uiso 1 1 calc R . . C9 C 0.2268(5) 0.5336(3) 0.7267(3) 0.052(2) Uani 1 1 d . . . C64 C 0.1516(5) 0.2404(4) 0.8494(4) 0.061(2) Uani 1 1 d . . . C100 C 0.4501(5) 0.5904(4) 0.5208(4) 0.063(3) Uani 1 1 d . . . C43 C -0.1112(4) 0.4481(3) 0.5129(4) 0.062(3) Uani 1 1 d . . . C56 C -0.0229(5) 0.2891(4) 0.7769(4) 0.063(3) Uani 1 1 d . . . C40 C 0.0071(5) 0.4371(3) 0.4546(3) 0.053(2) Uani 1 1 d . . . C72 C 0.1979(4) 0.2841(4) 0.8556(3) 0.055(2) Uani 1 1 d . . . C71 C 0.2165(4) 0.3095(4) 0.9068(4) 0.058(2) Uani 1 1 d . . . C1 C 0.3144(4) 0.3365(4) 0.5578(5) 0.059(2) Uani 1 1 d . . . C45 C -0.1601(5) 0.4318(4) 0.5944(5) 0.077(3) Uani 1 1 d . . . C107 C 0.3392(5) 0.6066(3) 0.5596(4) 0.058(2) Uani 1 1 d . . . C38 C 0.1261(5) 0.4081(4) 0.4537(4) 0.058(2) Uani 1 1 d . . . C46 C -0.0949(5) 0.4081(4) 0.6159(4) 0.073(3) Uani 1 1 d . . . H46 H -0.0908 0.3936 0.6512 0.088 Uiso 1 1 calc R . . C98 C 0.5383(5) 0.5384(4) 0.5729(5) 0.068(3) Uani 1 1 d . . . C83 C 0.4286(5) 0.4127(4) 0.8888(4) 0.069(3) Uani 1 1 d . . . C52 C -0.0464(4) 0.2199(4) 0.6187(4) 0.058(2) Uani 1 1 d . . . C2 C 0.3245(4) 0.2745(4) 0.6465(4) 0.060(2) Uani 1 1 d . . . C91 C 0.4976(6) 0.6548(4) 0.7576(5) 0.085(3) Uani 1 1 d . . . C42 C -0.1125(5) 0.4668(4) 0.4582(4) 0.069(3) Uani 1 1 d . . . H42 H -0.1532 0.4835 0.4409 0.083 Uiso 1 1 calc R . . C102 C 0.3556(7) 0.6469(5) 0.4750(4) 0.089(3) Uani 1 1 d . . . H102 H 0.3394 0.6686 0.4450 0.107 Uiso 1 1 calc R . . C88 C 0.5434(5) 0.5485(4) 0.7806(4) 0.071(3) Uani 1 1 d . . . C99 C 0.5170(5) 0.5667(4) 0.5261(5) 0.076(3) Uani 1 1 d . . . C61 C 0.2101(5) 0.2814(4) 0.7652(4) 0.066(3) Uani 1 1 d . . . H61 H 0.2294 0.2957 0.7355 0.079 Uiso 1 1 calc R . . C79 C 0.4813(6) 0.4466(5) 0.9123(4) 0.082(3) Uani 1 1 d . . . C94 C 0.3758(5) 0.6679(4) 0.6910(4) 0.074(3) Uani 1 1 d . . . H94 H 0.3331 0.6730 0.6684 0.089 Uiso 1 1 calc R . . C55 C -0.0331(5) 0.2667(4) 0.7245(3) 0.061(2) Uani 1 1 d . . . C53 C -0.0742(5) 0.1956(4) 0.6621(4) 0.076(3) Uani 1 1 d . . . H53 H -0.0974 0.1628 0.6559 0.091 Uiso 1 1 calc R . . C82 C 0.3572(5) 0.4811(4) 0.8573(4) 0.067(3) Uani 1 1 d . . . H82 H 0.3146 0.4934 0.8384 0.080 Uiso 1 1 calc R . . C87 C 0.5633(5) 0.4944(4) 0.7907(4) 0.070(3) Uani 1 1 d . . . C86 C 0.5171(4) 0.4550(3) 0.7686(4) 0.057(2) Uani 1 1 d . . . N2 N 0.3222(4) 0.2302(4) 0.6543(4) 0.089(3) Uani 1 1 d . . . N10 N 0.0869(5) 0.6208(4) 0.6919(4) 0.088(3) Uani 1 1 d . . . C67 C 0.1896(5) 0.2907(4) 0.9537(4) 0.070(3) Uani 1 1 d . . . C106 C 0.2390(5) 0.6157(4) 0.5998(4) 0.064(3) Uani 1 1 d . . . H106 H 0.2124 0.6060 0.6273 0.077 Uiso 1 1 calc R . . N1 N 0.3091(4) 0.3251(4) 0.5122(4) 0.086(3) Uani 1 1 d . . . C13 C 0.1904(5) 0.3988(4) 0.4282(4) 0.081(3) Uani 1 1 d . . . H13A H 0.1797 0.3753 0.3971 0.122 Uiso 1 1 calc R . . H13B H 0.2260 0.3825 0.4545 0.122 Uiso 1 1 calc R . . H13C H 0.2077 0.4325 0.4162 0.122 Uiso 1 1 calc R . . C81 C 0.4073(5) 0.5194(4) 0.8779(4) 0.079(3) Uani 1 1 d . . . C57 C 0.0155(5) 0.3361(4) 0.7850(3) 0.062(2) Uani 1 1 d . . . C14 C 0.0607(6) 0.4512(4) 0.3690(4) 0.081(3) Uani 1 1 d . . . H14A H 0.1042 0.4438 0.3548 0.121 Uiso 1 1 calc R . . H14B H 0.0523 0.4893 0.3685 0.121 Uiso 1 1 calc R . . H14C H 0.0224 0.4334 0.3466 0.121 Uiso 1 1 calc R . . C65 C 0.1252(5) 0.2241(4) 0.8984(5) 0.078(3) Uani 1 1 d . . . H65 H 0.0926 0.1961 0.8961 0.093 Uiso 1 1 calc R . . C12 C 0.1711(5) 0.5603(4) 0.8169(5) 0.076(3) Uani 1 1 d . . . C41 C -0.0572(5) 0.4611(3) 0.4311(4) 0.062(3) Uani 1 1 d . . . H41 H -0.0609 0.4734 0.3950 0.074 Uiso 1 1 calc R . . C21 C 0.1520(5) 0.2155(4) 0.6980(4) 0.081(3) Uani 1 1 d . . . H21A H 0.1789 0.1831 0.6962 0.121 Uiso 1 1 calc R . . H21B H 0.1667 0.2415 0.6729 0.121 Uiso 1 1 calc R . . H21C H 0.1026 0.2078 0.6882 0.121 Uiso 1 1 calc R . . C15 C -0.2351(5) 0.4787(5) 0.5161(5) 0.099(4) Uani 1 1 d . . . H15A H -0.2732 0.4679 0.5355 0.148 Uiso 1 1 calc R . . H15B H -0.2455 0.4683 0.4781 0.148 Uiso 1 1 calc R . . H15C H -0.2295 0.5170 0.5185 0.148 Uiso 1 1 calc R . . C31 C 0.5147(8) 0.7554(4) 0.7680(7) 0.163(8) Uani 1 1 d . . . H31A H 0.5612 0.7438 0.7835 0.244 Uiso 1 1 calc R . . H31B H 0.4917 0.7724 0.7959 0.244 Uiso 1 1 calc R . . H31C H 0.5186 0.7805 0.7388 0.244 Uiso 1 1 calc R . . C62 C 0.1645(5) 0.2375(4) 0.7552(4) 0.066(3) Uani 1 1 d . . . C54 C -0.0690(6) 0.2172(4) 0.7121(4) 0.082(3) Uani 1 1 d . . . H54 H -0.0892 0.1995 0.7396 0.098 Uiso 1 1 calc R . . C77 C 0.5544(9) 0.3725(9) 0.9417(7) 0.137(6) Uani 1 1 d . . . H77 H 0.5962 0.3590 0.9608 0.165 Uiso 1 1 calc R . . C104 C 0.2460(6) 0.6646(4) 0.5173(4) 0.077(3) Uani 1 1 d . . . C17 C -0.0273(6) 0.2065(4) 0.4695(4) 0.087(3) Uani 1 1 d . . . H17A H -0.0022 0.1731 0.4696 0.130 Uiso 1 1 calc R . . H17B H -0.0059 0.2325 0.4479 0.130 Uiso 1 1 calc R . . H17C H -0.0758 0.2012 0.4541 0.130 Uiso 1 1 calc R . . N11 N -0.0018(6) 0.4965(5) 0.7930(5) 0.138(5) Uani 1 1 d . . . C63 C 0.1352(5) 0.2165(4) 0.7987(4) 0.070(3) Uani 1 1 d . . . C44 C -0.1668(5) 0.4514(4) 0.5417(5) 0.074(3) Uani 1 1 d . . . C90 C 0.5626(6) 0.6424(5) 0.7921(5) 0.113(5) Uani 1 1 d . . . H90 H 0.5906 0.6705 0.8079 0.136 Uiso 1 1 calc R . . C70 C 0.2767(5) 0.3761(4) 0.9560(4) 0.079(3) Uani 1 1 d . . . H70 H 0.3059 0.4062 0.9570 0.095 Uiso 1 1 calc R . . C84 C 0.4390(6) 0.3566(5) 0.8910(4) 0.079(3) Uani 1 1 d . . . C23 C 0.1845(6) 0.2977(6) 1.0555(4) 0.107(4) Uani 1 1 d . . . H23A H 0.1973 0.2607 1.0619 0.160 Uiso 1 1 calc R . . H23B H 0.1340 0.3013 1.0523 0.160 Uiso 1 1 calc R . . H23C H 0.2062 0.3192 1.0857 0.160 Uiso 1 1 calc R . . C30 C 0.6304(6) 0.4803(4) 0.8256(5) 0.108(4) Uani 1 1 d . . . H30A H 0.6248 0.4465 0.8436 0.162 Uiso 1 1 calc R . . H30B H 0.6420 0.5078 0.8528 0.162 Uiso 1 1 calc R . . H30C H 0.6677 0.4773 0.8031 0.162 Uiso 1 1 calc R . . C33 C 0.6102(5) 0.5142(5) 0.5825(5) 0.108(4) Uani 1 1 d . . . H33A H 0.6163 0.4904 0.5527 0.162 Uiso 1 1 calc R . . H33B H 0.6156 0.4944 0.6164 0.162 Uiso 1 1 calc R . . H33C H 0.6452 0.5422 0.5846 0.162 Uiso 1 1 calc R . . C80 C 0.4698(6) 0.5002(5) 0.9066(4) 0.087(3) Uani 1 1 d . . . C101 C 0.4200(7) 0.6234(5) 0.4764(4) 0.088(4) Uani 1 1 d . . . H101 H 0.4455 0.6292 0.4472 0.106 Uiso 1 1 calc R . . C74 C 0.4570(12) 0.2491(6) 0.8925(7) 0.138(6) Uani 1 1 d . . . C93 C 0.4117(6) 0.7134(4) 0.7122(5) 0.080(3) Uani 1 1 d . . . C18 C -0.0864(6) 0.1455(4) 0.5510(5) 0.096(4) Uani 1 1 d . . . H18A H -0.1315 0.1516 0.5293 0.144 Uiso 1 1 calc R . . H18B H -0.0931 0.1266 0.5840 0.144 Uiso 1 1 calc R . . H18C H -0.0572 0.1245 0.5302 0.144 Uiso 1 1 calc R . . C78 C 0.5466(7) 0.4228(8) 0.9391(6) 0.126(5) Uani 1 1 d . . . H78 H 0.5832 0.4450 0.9545 0.151 Uiso 1 1 calc R . . C11 C 0.0519(6) 0.5063(5) 0.7787(4) 0.086(3) Uani 1 1 d . . . C68 C 0.2095(5) 0.3163(5) 1.0036(4) 0.080(3) Uani 1 1 d . . . C89 C 0.5836(6) 0.5923(4) 0.8019(5) 0.100(4) Uani 1 1 d . . . H89 H 0.6267 0.5861 0.8237 0.120 Uiso 1 1 calc R . . C34 C 0.5633(6) 0.5741(5) 0.4828(5) 0.115(5) Uani 1 1 d . . . H34A H 0.5996 0.5998 0.4950 0.173 Uiso 1 1 calc R . . H34B H 0.5356 0.5869 0.4498 0.173 Uiso 1 1 calc R . . H34C H 0.5847 0.5403 0.4756 0.173 Uiso 1 1 calc R . . C27 C 0.5259(7) 0.5413(5) 0.9322(6) 0.124(5) Uani 1 1 d . . . H27A H 0.5633 0.5437 0.9097 0.186 Uiso 1 1 calc R . . H27B H 0.5451 0.5297 0.9685 0.186 Uiso 1 1 calc R . . H27C H 0.5042 0.5759 0.9343 0.186 Uiso 1 1 calc R . . C92 C 0.4721(6) 0.7076(4) 0.7455(5) 0.095(4) Uani 1 1 d . . . C29 C 0.5314(5) 0.3971(3) 0.7781(4) 0.074(3) Uani 1 1 d . . . H29A H 0.4895 0.3768 0.7654 0.111 Uiso 1 1 calc R . . H29B H 0.5448 0.3907 0.8167 0.111 Uiso 1 1 calc R . . H29C H 0.5691 0.3860 0.7583 0.111 Uiso 1 1 calc R . . C36 C 0.1382(5) 0.6752(4) 0.5653(5) 0.092(3) Uani 1 1 d . . . H36A H 0.1402 0.7137 0.5631 0.138 Uiso 1 1 calc R . . H36B H 0.1248 0.6648 0.6001 0.138 Uiso 1 1 calc R . . H36C H 0.1040 0.6618 0.5362 0.138 Uiso 1 1 calc R . . C69 C 0.2540(6) 0.3592(5) 1.0050(4) 0.089(3) Uani 1 1 d . . . C73 C 0.3949(8) 0.2726(5) 0.8689(5) 0.112(4) Uani 1 1 d . . . H73 H 0.3581 0.2506 0.8535 0.135 Uiso 1 1 calc R . . C22 C 0.0901(6) 0.1679(4) 0.7905(4) 0.090(3) Uani 1 1 d . . . H22A H 0.0651 0.1678 0.7538 0.134 Uiso 1 1 calc R . . H22B H 0.0566 0.1680 0.8165 0.134 Uiso 1 1 calc R . . H22C H 0.1192 0.1363 0.7960 0.134 Uiso 1 1 calc R . . N12 N 0.1911(6) 0.5847(4) 0.8571(4) 0.102(3) Uani 1 1 d . . . C75 C 0.5126(10) 0.2803(9) 0.9165(8) 0.149(7) Uani 1 1 d . . . C35 C 0.2135(7) 0.7017(5) 0.4736(5) 0.118(4) Uani 1 1 d . . . H35A H 0.1654 0.6911 0.4620 0.177 Uiso 1 1 calc R . . H35B H 0.2397 0.7001 0.4428 0.177 Uiso 1 1 calc R . . H35C H 0.2145 0.7377 0.4877 0.177 Uiso 1 1 calc R . . C24 C 0.2787(7) 0.3921(7) 1.0561(5) 0.139(6) Uani 1 1 d . . . H24A H 0.2386 0.4092 1.0687 0.208 Uiso 1 1 calc R . . H24B H 0.3116 0.4190 1.0476 0.208 Uiso 1 1 calc R . . H24C H 0.3014 0.3689 1.0845 0.208 Uiso 1 1 calc R . . C66 C 0.1444(5) 0.2466(5) 0.9470(5) 0.079(3) Uani 1 1 d . . . H66 H 0.1270 0.2324 0.9777 0.094 Uiso 1 1 calc R . . C28 C 0.3901(6) 0.5777(4) 0.8676(5) 0.105(4) Uani 1 1 d . . . H28A H 0.3748 0.5933 0.8998 0.157 Uiso 1 1 calc R . . H28B H 0.3529 0.5810 0.8371 0.157 Uiso 1 1 calc R . . H28C H 0.4314 0.5963 0.8591 0.157 Uiso 1 1 calc R . . C16 C -0.2172(6) 0.4328(6) 0.6309(5) 0.122(5) Uani 1 1 d . . . H16A H -0.2259 0.4693 0.6409 0.182 Uiso 1 1 calc R . . H16B H -0.2025 0.4122 0.6635 0.182 Uiso 1 1 calc R . . H16C H -0.2598 0.4176 0.6116 0.182 Uiso 1 1 calc R . . C76 C 0.5039(8) 0.3355(6) 0.9176(5) 0.109(5) Uani 1 1 d . . . C25 C 0.4547(11) 0.1863(6) 0.8893(7) 0.201(10) Uani 1 1 d . . . H25A H 0.4739 0.1745 0.8571 0.301 Uiso 1 1 calc R . . H25B H 0.4065 0.1742 0.8874 0.301 Uiso 1 1 calc R . . H25C H 0.4822 0.1714 0.9215 0.301 Uiso 1 1 calc R . . C20 C 0.0317(6) 0.3636(4) 0.8381(4) 0.081(3) Uani 1 1 d . . . H20A H -0.0112 0.3686 0.8540 0.122 Uiso 1 1 calc R . . H20B H 0.0525 0.3980 0.8326 0.122 Uiso 1 1 calc R . . H20C H 0.0643 0.3423 0.8624 0.122 Uiso 1 1 calc R . . C19 C -0.0547(6) 0.2646(5) 0.8240(4) 0.095(4) Uani 1 1 d . . . H19A H -0.0361 0.2823 0.8576 0.143 Uiso 1 1 calc R . . H19B H -0.0432 0.2270 0.8266 0.143 Uiso 1 1 calc R . . H19C H -0.1052 0.2688 0.8178 0.143 Uiso 1 1 calc R . . C32 C 0.3792(7) 0.7669(4) 0.6963(6) 0.117(5) Uani 1 1 d . . . H32A H 0.3711 0.7861 0.7289 0.175 Uiso 1 1 calc R . . H32B H 0.3350 0.7618 0.6731 0.175 Uiso 1 1 calc R . . H32C H 0.4107 0.7873 0.6769 0.175 Uiso 1 1 calc R . . C26 C 0.5785(10) 0.2517(8) 0.9435(7) 0.207(10) Uani 1 1 d . . . H26A H 0.5768 0.2147 0.9324 0.311 Uiso 1 1 calc R . . H26B H 0.5806 0.2539 0.9827 0.311 Uiso 1 1 calc R . . H26C H 0.6197 0.2685 0.9324 0.311 Uiso 1 1 calc R . . O1S O 0.1256(12) 0.0189(9) 0.4290(9) 0.096(7) Uiso 0.33 1 d P A -50 O3S O 0.0671(14) 0.0816(11) 0.4928(11) 0.118(8) Uiso 0.33 1 d P B -52 O2S O 0.0905(14) 0.0544(10) 0.4634(11) 0.110(8) Uiso 0.33 1 d P C -51 O19S O 0.6341(14) 0.3823(11) 0.6753(10) 0.179(9) Uiso 0.50 1 d P D 5 O30S O 0.749(4) 0.490(3) 0.007(3) 0.09(2) Uiso 0.10 1 d P E 11 O17S O 0.6342(13) 0.3343(11) 0.6628(10) 0.176(9) Uiso 0.50 1 d P F 12 O14S O 0.515(3) 0.2151(16) 0.5757(15) 0.168(13) Uiso 0.40 1 d P G 13 O11S O 0.451(3) 0.2324(19) 0.5556(19) 0.155(15) Uiso 0.30 1 d P H 14 O28S O 0.264(3) 0.721(3) 0.814(2) 0.24(2) Uiso 0.30 1 d P I 15 O33S O 0.3133(15) 0.3184(12) 0.4055(12) 0.119(9) Uiso 0.30 1 d P J 16 O23S O 0.924(2) 0.5746(16) 0.8665(17) 0.171(14) Uiso 0.30 1 d P K 17 O26S O 0.767(4) 0.558(3) 0.724(3) 0.18(2) Uiso 0.20 1 d P L 18 O13S O 0.775(2) 0.1802(18) 0.4139(18) 0.174(15) Uiso 0.30 1 d P M 19 O18S O 0.752(3) 0.283(3) 0.686(3) 0.18(2) Uiso 0.20 1 d P N 20 O22S O 0.853(2) 0.4621(17) 0.7698(18) 0.186(15) Uiso 0.30 1 d P O 21 O20S O 0.792(3) 0.372(3) 0.832(3) 0.18(2) Uiso 0.20 1 d P P 22 O27S O 0.730(3) 0.592(2) 0.710(2) 0.201(18) Uiso 0.30 1 d P Q 23 O25S O 0.800(3) 0.566(2) 0.809(2) 0.153(18) Uiso 0.20 1 d P R 24 O29S O 0.2563(16) 0.6844(13) 0.7857(13) 0.125(10) Uiso 0.30 1 d P S 25 O21S O 0.785(3) 0.347(3) 0.880(3) 0.16(2) Uiso 0.20 1 d P T 26 O25 O 0.885(7) 0.054(5) 0.417(6) 0.20(5) Uiso 0.10 1 d P U 27 O24S O 0.859(4) 0.564(3) 0.846(3) 0.19(2) Uiso 0.20 1 d P V 28 O16S O 0.305(4) 0.159(3) 0.776(3) 0.20(3) Uiso 0.20 1 d P W 29 O15S O 0.567(2) 0.2076(15) 0.5803(15) 0.194(15) Uiso 0.40 1 d P X 30 O10S O 0.409(2) 0.2197(15) 0.5352(16) 0.189(14) Uiso 0.40 1 d P Y 31 O31S O 0.6937(17) 0.4871(14) 0.0109(12) 0.151(11) Uiso 0.40 1 d P Z 32 O12S O 0.478(4) 0.202(3) 0.562(2) 0.19(2) Uiso 0.30 1 d P A 33 O32S O 0.710(2) 0.456(2) 0.0167(17) 0.161(16) Uiso 0.30 1 d P B 36 O34S O 0.727(2) 0.4027(19) 0.0231(17) 0.178(15) Uiso 0.30 1 d P C 37 O35S O 0.7252(14) 0.3403(11) 0.0579(11) 0.193(10) Uiso 0.50 1 d P D 38 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0325(6) 0.0643(8) 0.0494(7) 0.0098(6) 0.0061(5) -0.0043(5) Co3 0.0342(6) 0.0408(7) 0.0606(8) 0.0030(5) 0.0058(5) -0.0020(5) Co2 0.0564(8) 0.0480(7) 0.0498(7) 0.0078(5) 0.0056(6) -0.0021(6) Fe1 0.0350(7) 0.0480(8) 0.0585(8) 0.0057(6) 0.0030(5) -0.0009(5) Fe2 0.0547(8) 0.0528(8) 0.0564(8) 0.0035(6) 0.0165(6) 0.0119(6) N15 0.035(4) 0.079(5) 0.037(4) 0.007(4) 0.007(3) 0.002(3) N13 0.039(4) 0.065(5) 0.052(4) 0.015(4) -0.001(4) -0.001(4) N21 0.047(4) 0.040(5) 0.062(5) 0.008(4) 0.001(3) 0.003(4) N4 0.035(4) 0.063(5) 0.054(5) 0.014(3) 0.003(3) 0.003(4) C4 0.045(6) 0.046(5) 0.048(5) 0.015(4) 0.006(4) -0.001(4) N6 0.039(4) 0.056(5) 0.066(5) 0.009(4) 0.009(3) 0.000(4) N22 0.050(5) 0.038(5) 0.074(5) 0.000(4) -0.006(4) 0.007(3) N9 0.052(5) 0.051(5) 0.063(5) -0.001(4) 0.002(4) -0.001(4) N7 0.037(4) 0.066(5) 0.056(5) 0.019(4) 0.006(4) 0.005(4) C5 0.038(5) 0.029(5) 0.089(8) 0.010(5) -0.002(5) -0.003(4) N8 0.053(5) 0.060(5) 0.056(5) 0.003(4) 0.007(4) -0.005(4) N20 0.060(5) 0.053(5) 0.066(5) 0.007(4) 0.002(4) 0.007(4) N16 0.048(4) 0.073(5) 0.045(5) 0.001(4) 0.009(3) -0.012(4) N14 0.034(4) 0.064(5) 0.063(5) -0.008(4) 0.010(4) -0.007(3) N24 0.046(5) 0.059(5) 0.064(5) 0.001(4) 0.005(4) 0.000(4) C8 0.044(5) 0.057(6) 0.061(6) -0.012(5) 0.013(4) -0.010(5) N5 0.056(5) 0.059(5) 0.059(5) 0.009(4) 0.005(4) -0.006(4) C7 0.044(5) 0.051(6) 0.046(6) 0.011(5) 0.008(4) 0.012(4) N23 0.036(4) 0.049(4) 0.076(5) -0.003(4) 0.015(4) -0.002(3) C108 0.048(6) 0.055(6) 0.062(6) 0.001(5) 0.007(5) -0.011(5) N17 0.064(5) 0.064(5) 0.045(5) 0.004(4) 0.013(4) -0.008(4) N18 0.059(5) 0.082(6) 0.050(5) 0.007(4) 0.006(4) -0.006(5) C6 0.028(5) 0.068(7) 0.050(5) 0.013(5) 0.005(4) 0.003(4) C47 0.040(5) 0.056(6) 0.055(6) 0.004(5) -0.005(4) 0.003(4) C59 0.046(5) 0.060(6) 0.047(6) 0.008(5) 0.012(4) -0.014(5) C58 0.052(6) 0.071(6) 0.055(7) 0.006(5) 0.005(5) -0.017(5) C10 0.064(6) 0.058(7) 0.070(7) -0.018(5) 0.020(5) 0.007(5) C60 0.045(5) 0.070(6) 0.040(5) 0.004(5) 0.013(4) -0.004(5) C96 0.049(5) 0.043(6) 0.068(6) 0.005(5) -0.006(5) -0.002(5) C95 0.066(6) 0.044(6) 0.069(6) 0.003(5) 0.002(5) -0.004(5) C103 0.073(7) 0.073(7) 0.068(7) 0.012(6) 0.014(6) -0.013(6) C39 0.072(7) 0.050(5) 0.052(6) 0.010(4) 0.007(5) -0.009(5) C85 0.052(6) 0.048(6) 0.066(6) -0.002(5) 0.006(5) -0.005(5) N3 0.040(5) 0.108(7) 0.097(7) 0.007(5) 0.021(4) 0.006(5) N19 0.114(8) 0.061(6) 0.071(6) 0.018(5) 0.026(5) 0.031(6) C48 0.044(5) 0.056(6) 0.056(6) -0.004(5) -0.001(5) 0.001(4) C3 0.060(7) 0.057(6) 0.055(6) 0.002(4) 0.014(5) -0.002(5) C50 0.047(5) 0.078(7) 0.049(6) -0.003(5) 0.004(4) 0.002(5) C37 0.046(5) 0.067(6) 0.063(6) 0.011(5) 0.016(5) -0.003(4) C49 0.047(5) 0.075(7) 0.043(6) 0.009(5) 0.020(4) 0.010(5) C105 0.056(6) 0.059(6) 0.085(8) 0.001(6) -0.014(6) 0.002(5) C51 0.058(6) 0.076(7) 0.049(6) -0.001(5) 0.014(5) -0.010(5) C97 0.047(6) 0.057(6) 0.082(7) -0.012(5) 0.014(5) -0.010(5) C9 0.058(6) 0.038(5) 0.055(6) 0.001(4) -0.006(5) 0.005(5) C64 0.051(5) 0.060(6) 0.075(7) 0.013(5) 0.017(5) -0.015(5) C100 0.076(7) 0.058(6) 0.058(6) -0.003(5) 0.021(6) -0.025(5) C43 0.038(6) 0.047(6) 0.096(8) -0.014(5) -0.007(5) -0.001(4) C56 0.062(6) 0.072(7) 0.061(7) 0.018(5) 0.025(5) -0.017(5) C40 0.059(6) 0.043(5) 0.052(6) 0.010(4) -0.007(5) -0.008(4) C72 0.054(5) 0.073(6) 0.039(6) 0.006(5) 0.006(4) 0.000(5) C71 0.044(5) 0.076(7) 0.055(6) 0.015(5) 0.005(4) 0.000(5) C1 0.040(5) 0.057(6) 0.080(7) 0.000(5) 0.007(5) 0.001(4) C45 0.037(6) 0.089(8) 0.109(9) -0.017(7) 0.020(6) -0.003(5) C107 0.058(6) 0.055(6) 0.062(6) 0.005(5) 0.008(5) -0.010(5) C38 0.057(6) 0.063(6) 0.055(6) 0.017(5) 0.009(5) 0.002(5) C46 0.049(6) 0.095(8) 0.079(7) -0.002(6) 0.018(6) -0.010(6) C98 0.053(6) 0.070(7) 0.085(8) -0.009(6) 0.025(6) -0.016(5) C83 0.072(7) 0.077(8) 0.057(6) 0.015(5) 0.006(5) 0.009(6) C52 0.052(5) 0.067(6) 0.056(6) 0.005(5) 0.012(4) -0.016(5) C2 0.038(5) 0.056(7) 0.082(7) 0.007(5) -0.004(4) -0.003(5) C91 0.103(8) 0.039(6) 0.100(8) -0.004(5) -0.035(7) -0.010(6) C42 0.055(6) 0.069(7) 0.075(8) 0.006(6) -0.019(6) 0.011(5) C102 0.109(10) 0.087(8) 0.070(8) 0.015(6) 0.006(7) -0.017(8) C88 0.069(7) 0.051(6) 0.084(7) 0.002(5) -0.017(6) -0.003(5) C99 0.061(7) 0.081(7) 0.096(9) -0.037(7) 0.048(6) -0.036(6) C61 0.074(7) 0.067(7) 0.058(7) 0.008(5) 0.015(5) -0.017(5) C79 0.077(8) 0.086(9) 0.077(8) 0.003(6) -0.006(6) 0.005(7) C94 0.069(7) 0.057(7) 0.093(8) 0.007(6) -0.002(6) 0.007(6) C55 0.073(6) 0.073(7) 0.040(6) 0.004(5) 0.018(5) -0.011(5) C53 0.086(7) 0.086(7) 0.055(7) -0.004(6) 0.007(5) -0.038(6) C82 0.064(6) 0.068(7) 0.068(6) 0.003(5) 0.007(5) 0.000(6) C87 0.059(6) 0.064(7) 0.078(7) 0.011(5) -0.017(5) 0.015(5) C86 0.044(5) 0.047(6) 0.075(6) 0.002(5) -0.011(5) 0.003(5) N2 0.070(6) 0.061(6) 0.131(8) 0.014(6) -0.006(5) -0.007(5) N10 0.112(8) 0.067(6) 0.087(7) 0.003(5) 0.019(5) 0.042(5) C67 0.050(6) 0.097(8) 0.062(7) 0.021(6) 0.000(5) 0.007(6) C106 0.048(6) 0.060(6) 0.083(7) -0.008(5) 0.001(5) -0.004(5) N1 0.073(6) 0.109(7) 0.074(6) -0.006(6) 0.005(5) -0.012(5) C13 0.082(7) 0.095(8) 0.071(7) 0.021(6) 0.027(6) -0.003(6) C81 0.062(7) 0.083(8) 0.094(8) -0.013(6) 0.014(6) -0.011(6) C57 0.076(6) 0.076(7) 0.035(5) 0.009(5) 0.010(5) -0.002(6) C14 0.108(8) 0.080(7) 0.051(6) 0.012(5) -0.001(6) 0.009(6) C65 0.062(6) 0.081(7) 0.092(9) 0.022(7) 0.016(6) -0.017(5) C12 0.080(7) 0.078(8) 0.077(8) 0.019(6) 0.032(6) 0.032(6) C41 0.080(7) 0.044(5) 0.055(6) 0.006(4) -0.013(6) 0.005(5) C21 0.081(7) 0.092(8) 0.070(7) -0.017(6) 0.009(5) -0.031(6) C15 0.047(6) 0.109(9) 0.133(10) -0.027(8) -0.019(6) 0.016(6) C31 0.195(15) 0.046(7) 0.209(16) -0.012(8) -0.116(13) -0.004(8) C62 0.057(6) 0.072(7) 0.069(7) 0.001(5) 0.010(5) -0.013(5) C54 0.103(8) 0.084(8) 0.062(7) 0.005(6) 0.026(6) -0.047(7) C77 0.114(13) 0.163(17) 0.120(13) 0.026(13) -0.036(10) 0.011(14) C104 0.085(8) 0.064(7) 0.076(8) 0.006(6) -0.006(6) -0.005(6) C17 0.103(8) 0.098(8) 0.061(7) -0.021(6) 0.015(6) -0.006(7) N11 0.108(9) 0.160(11) 0.161(11) 0.040(9) 0.079(8) 0.039(8) C63 0.060(6) 0.068(7) 0.082(8) 0.010(6) 0.010(6) -0.010(5) C44 0.043(6) 0.066(7) 0.110(9) -0.014(6) 0.001(6) 0.012(5) C90 0.105(10) 0.057(8) 0.154(12) 0.000(7) -0.067(9) -0.017(7) C70 0.077(7) 0.096(8) 0.064(8) -0.003(6) 0.009(6) -0.012(6) C84 0.072(7) 0.091(9) 0.070(7) 0.017(6) -0.002(6) 0.018(7) C23 0.091(8) 0.176(13) 0.054(7) 0.018(7) 0.012(6) -0.012(8) C30 0.080(8) 0.072(8) 0.159(12) 0.010(7) -0.033(8) 0.009(6) C33 0.062(7) 0.119(10) 0.153(12) -0.035(9) 0.049(7) -0.005(7) C80 0.069(8) 0.115(10) 0.073(7) -0.022(7) -0.005(6) -0.014(7) C101 0.106(10) 0.100(9) 0.063(8) -0.012(7) 0.029(7) -0.040(8) C74 0.199(18) 0.091(11) 0.127(13) 0.054(10) 0.034(13) 0.098(13) C93 0.090(8) 0.041(6) 0.102(8) -0.006(5) -0.008(7) 0.003(6) C18 0.106(9) 0.086(8) 0.098(9) -0.021(7) 0.023(7) -0.036(7) C78 0.085(10) 0.154(15) 0.129(12) 0.005(11) -0.026(8) 0.008(10) C11 0.072(7) 0.097(8) 0.095(8) 0.025(6) 0.036(6) 0.040(6) C68 0.059(6) 0.125(10) 0.055(7) 0.018(6) 0.000(5) -0.009(7) C89 0.100(9) 0.055(7) 0.125(10) 0.001(6) -0.059(7) -0.013(6) C34 0.105(9) 0.119(10) 0.136(11) -0.027(8) 0.072(9) -0.040(8) C27 0.120(11) 0.119(11) 0.124(11) -0.028(9) -0.017(9) -0.035(9) C92 0.106(9) 0.049(7) 0.115(9) -0.002(6) -0.040(8) -0.015(6) C29 0.079(7) 0.047(6) 0.089(7) 0.014(5) -0.015(6) 0.017(5) C36 0.073(7) 0.079(8) 0.118(9) 0.007(7) -0.005(6) 0.012(6) C69 0.073(7) 0.150(11) 0.041(7) -0.011(7) -0.004(5) -0.016(8) C73 0.147(12) 0.089(10) 0.104(10) 0.028(8) 0.026(9) 0.022(9) C22 0.089(8) 0.090(8) 0.089(8) 0.003(6) 0.011(6) -0.049(7) N12 0.143(9) 0.093(7) 0.073(7) -0.013(6) 0.022(6) 0.026(6) C75 0.146(16) 0.17(2) 0.131(15) 0.061(13) 0.016(12) 0.074(15) C35 0.127(11) 0.115(10) 0.107(10) 0.041(8) -0.007(8) 0.025(8) C24 0.122(11) 0.224(17) 0.070(9) -0.018(10) 0.013(8) -0.047(11) C66 0.067(7) 0.093(8) 0.079(8) 0.019(7) 0.018(6) -0.017(6) C28 0.104(9) 0.057(7) 0.151(12) -0.014(7) 0.013(8) -0.019(6) C16 0.061(7) 0.173(14) 0.137(11) -0.002(10) 0.038(8) 0.014(8) C76 0.123(12) 0.104(11) 0.101(10) 0.048(9) 0.018(9) 0.062(10) C25 0.31(3) 0.096(12) 0.198(18) 0.045(12) 0.044(17) 0.117(15) C20 0.099(8) 0.082(7) 0.066(7) 0.006(6) 0.021(6) -0.021(6) C19 0.113(9) 0.119(9) 0.059(7) 0.004(6) 0.031(6) -0.052(8) C32 0.122(10) 0.051(7) 0.162(12) -0.007(7) -0.035(9) 0.014(7) C26 0.22(2) 0.22(2) 0.186(18) 0.066(15) 0.013(15) 0.159(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N4 2.059(7) . ? Co1 N7 2.099(9) . ? Co1 N16 2.151(7) . ? Co1 N13 2.154(7) . ? Co1 N14 2.154(7) . ? Co1 N15 2.177(7) . ? Co3 N9 2.010(8) . ? Co3 N6 2.056(8) . ? Co3 N21 2.114(6) . ? Co3 N23 2.114(7) . ? Co3 N24 2.116(7) . ? Co3 N22 2.144(7) . ? Co2 N8 2.035(8) . ? Co2 N5 2.040(9) . ? Co2 N20 2.103(7) . ? Co2 N17 2.110(7) . ? Co2 N19 2.124(9) . ? Co2 N18 2.125(7) . ? Fe1 C2 1.922(11) . ? Fe1 C6 1.925(10) . ? Fe1 C5 1.931(12) . ? Fe1 C1 1.930(11) . ? Fe1 C4 1.942(9) . ? Fe1 C3 1.947(10) . ? Fe2 C12 1.891(13) . ? Fe2 C9 1.912(11) . ? Fe2 C11 1.916(11) . ? Fe2 C8 1.919(11) . ? Fe2 C10 1.916(11) . ? Fe2 C7 1.925(10) . ? N15 C49 1.333(10) . ? N15 C60 1.357(10) . ? N13 C37 1.330(10) . ? N13 C48 1.385(10) . ? N21 C85 1.311(10) . ? N21 C96 1.377(10) . ? N4 C4 1.131(9) . ? N6 C6 1.168(10) . ? N22 C94 1.305(11) . ? N22 C95 1.360(11) . ? N9 C9 1.158(10) . ? N7 C7 1.155(10) . ? C5 N5 1.151(11) . ? N8 C8 1.175(10) . ? N20 C82 1.315(11) . ? N20 C83 1.357(12) . ? N16 C58 1.321(11) . ? N16 C59 1.354(10) . ? N14 C46 1.326(11) . ? N14 C47 1.346(10) . ? N24 C106 1.325(11) . ? N24 C107 1.358(11) . ? N23 C97 1.332(11) . ? N23 C108 1.336(10) . ? C108 C100 1.416(12) . ? C108 C107 1.443(12) . ? N17 C61 1.319(11) . ? N17 C72 1.355(10) . ? N18 C70 1.308(12) . ? N18 C71 1.353(11) . ? C47 C43 1.420(12) . ? C47 C48 1.446(12) . ? C59 C55 1.384(11) . ? C59 C60 1.446(11) . ? C58 C57 1.400(12) . ? C10 N10 1.165(11) . ? C60 C52 1.399(12) . ? C96 C88 1.412(12) . ? C96 C95 1.416(12) . ? C95 C91 1.386(13) . ? C103 C107 1.407(13) . ? C103 C104 1.412(14) . ? C103 C102 1.426(14) . ? C39 C38 1.393(12) . ? C39 C40 1.407(12) . ? C39 C14 1.503(12) . ? C85 C86 1.409(12) . ? N3 C3 1.156(10) . ? N19 C84 1.350(13) . ? N19 C73 1.363(14) . ? C48 C40 1.392(11) . ? C50 C51 1.366(12) . ? C50 C49 1.395(12) . ? C50 C17 1.487(12) . ? C37 C38 1.401(11) . ? C105 C104 1.377(14) . ? C105 C106 1.415(13) . ? C105 C36 1.510(14) . ? C51 C52 1.418(12) . ? C51 C18 1.502(13) . ? C97 C98 1.365(13) . ? C64 C63 1.391(13) . ? C64 C72 1.408(12) . ? C64 C65 1.438(13) . ? C100 C99 1.411(14) . ? C100 C101 1.436(15) . ? C43 C44 1.366(14) . ? C43 C42 1.432(13) . ? C56 C57 1.395(12) . ? C56 C55 1.405(12) . ? C56 C19 1.521(12) . ? C40 C41 1.430(12) . ? C72 C71 1.421(12) . ? C71 C67 1.418(12) . ? C1 N1 1.158(11) . ? C45 C44 1.387(14) . ? C45 C46 1.425(14) . ? C45 C16 1.516(14) . ? C38 C13 1.484(12) . ? C98 C99 1.375(14) . ? C98 C33 1.501(14) . ? C83 C79 1.390(14) . ? C83 C84 1.423(14) . ? C52 C53 1.404(12) . ? C2 N2 1.132(11) . ? C91 C92 1.434(14) . ? C91 C90 1.450(14) . ? C42 C41 1.343(13) . ? C102 C101 1.369(16) . ? C88 C89 1.409(13) . ? C88 C87 1.425(12) . ? C99 C34 1.495(14) . ? C61 C62 1.411(13) . ? C79 C80 1.369(15) . ? C79 C78 1.468(17) . ? C94 C93 1.398(13) . ? C55 C54 1.436(13) . ? C53 C54 1.345(13) . ? C82 C81 1.409(13) . ? C87 C86 1.393(12) . ? C87 C30 1.497(13) . ? C86 C29 1.494(11) . ? C67 C68 1.400(14) . ? C67 C66 1.406(14) . ? C81 C80 1.399(15) . ? C81 C28 1.517(15) . ? C57 C20 1.481(13) . ? C65 C66 1.336(14) . ? C12 N12 1.188(13) . ? C21 C62 1.510(13) . ? C15 C44 1.542(13) . ? C31 C92 1.517(14) . ? C62 C63 1.385(13) . ? C77 C78 1.27(2) . ? C77 C76 1.42(2) . ? C104 C35 1.499(14) . ? N11 C11 1.164(13) . ? C63 C22 1.498(13) . ? C90 C89 1.335(14) . ? C70 C69 1.411(14) . ? C84 C76 1.434(16) . ? C23 C68 1.506(13) . ? C80 C27 1.566(15) . ? C74 C73 1.39(2) . ? C74 C75 1.40(2) . ? C74 C25 1.58(2) . ? C93 C92 1.341(14) . ? C93 C32 1.514(14) . ? C68 C69 1.375(15) . ? C69 C24 1.535(16) . ? C75 C76 1.40(2) . ? C75 C26 1.53(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N7 90.3(3) . . ? N4 Co1 N16 97.0(3) . . ? N7 Co1 N16 90.8(3) . . ? N4 Co1 N13 90.8(3) . . ? N7 Co1 N13 99.7(3) . . ? N16 Co1 N13 167.0(3) . . ? N4 Co1 N14 167.7(3) . . ? N7 Co1 N14 91.3(3) . . ? N16 Co1 N14 95.1(3) . . ? N13 Co1 N14 76.9(3) . . ? N4 Co1 N15 95.8(3) . . ? N7 Co1 N15 166.4(3) . . ? N16 Co1 N15 76.4(3) . . ? N13 Co1 N15 92.5(3) . . ? N14 Co1 N15 85.4(2) . . ? N9 Co3 N6 91.2(3) . . ? N9 Co3 N21 97.3(3) . . ? N6 Co3 N21 95.8(3) . . ? N9 Co3 N23 172.8(3) . . ? N6 Co3 N23 88.5(3) . . ? N21 Co3 N23 89.9(3) . . ? N9 Co3 N24 95.8(3) . . ? N6 Co3 N24 99.1(3) . . ? N21 Co3 N24 159.9(3) . . ? N23 Co3 N24 77.2(3) . . ? N9 Co3 N22 92.9(3) . . ? N6 Co3 N22 172.1(3) . . ? N21 Co3 N22 77.1(3) . . ? N23 Co3 N22 88.2(3) . . ? N24 Co3 N22 87.1(3) . . ? N8 Co2 N5 94.3(3) . . ? N8 Co2 N20 93.0(3) . . ? N5 Co2 N20 93.6(3) . . ? N8 Co2 N17 91.9(3) . . ? N5 Co2 N17 91.3(3) . . ? N20 Co2 N17 172.8(3) . . ? N8 Co2 N19 168.7(3) . . ? N5 Co2 N19 90.5(3) . . ? N20 Co2 N19 76.4(4) . . ? N17 Co2 N19 98.3(4) . . ? N8 Co2 N18 93.3(3) . . ? N5 Co2 N18 167.1(3) . . ? N20 Co2 N18 96.4(3) . . ? N17 Co2 N18 78.1(3) . . ? N19 Co2 N18 83.9(3) . . ? C2 Fe1 C6 176.7(4) . . ? C2 Fe1 C5 90.2(4) . . ? C6 Fe1 C5 86.6(3) . . ? C2 Fe1 C1 88.1(4) . . ? C6 Fe1 C1 95.2(4) . . ? C5 Fe1 C1 176.8(3) . . ? C2 Fe1 C4 87.4(3) . . ? C6 Fe1 C4 92.8(3) . . ? C5 Fe1 C4 88.7(3) . . ? C1 Fe1 C4 88.6(3) . . ? C2 Fe1 C3 92.4(4) . . ? C6 Fe1 C3 87.4(3) . . ? C5 Fe1 C3 91.8(3) . . ? C1 Fe1 C3 90.9(3) . . ? C4 Fe1 C3 179.5(4) . . ? C12 Fe2 C9 90.2(4) . . ? C12 Fe2 C11 91.4(5) . . ? C9 Fe2 C11 177.6(4) . . ? C12 Fe2 C8 88.7(4) . . ? C9 Fe2 C8 88.1(3) . . ? C11 Fe2 C8 93.8(4) . . ? C12 Fe2 C10 90.6(4) . . ? C9 Fe2 C10 86.3(4) . . ? C11 Fe2 C10 91.9(4) . . ? C8 Fe2 C10 174.4(4) . . ? C12 Fe2 C7 176.1(4) . . ? C9 Fe2 C7 90.6(3) . . ? C11 Fe2 C7 87.9(4) . . ? C8 Fe2 C7 87.4(3) . . ? C10 Fe2 C7 93.3(4) . . ? C49 N15 C60 116.5(7) . . ? C49 N15 Co1 129.0(6) . . ? C60 N15 Co1 114.4(5) . . ? C37 N13 C48 116.5(7) . . ? C37 N13 Co1 129.5(6) . . ? C48 N13 Co1 113.9(5) . . ? C85 N21 C96 117.5(7) . . ? C85 N21 Co3 127.7(6) . . ? C96 N21 Co3 114.0(5) . . ? C4 N4 Co1 158.7(7) . . ? N4 C4 Fe1 179.6(9) . . ? C6 N6 Co3 159.5(7) . . ? C94 N22 C95 116.9(8) . . ? C94 N22 Co3 129.2(6) . . ? C95 N22 Co3 113.5(5) . . ? C9 N9 Co3 164.8(7) . . ? C7 N7 Co1 163.4(7) . . ? N5 C5 Fe1 175.3(8) . . ? C8 N8 Co2 162.1(7) . . ? C82 N20 C83 116.6(9) . . ? C82 N20 Co2 127.3(7) . . ? C83 N20 Co2 116.0(7) . . ? C58 N16 C59 117.8(7) . . ? C58 N16 Co1 127.3(6) . . ? C59 N16 Co1 114.8(5) . . ? C46 N14 C47 117.0(8) . . ? C46 N14 Co1 127.5(7) . . ? C47 N14 Co1 115.4(5) . . ? C106 N24 C107 117.9(8) . . ? C106 N24 Co3 127.2(6) . . ? C107 N24 Co3 114.7(6) . . ? N8 C8 Fe2 174.2(7) . . ? C5 N5 Co2 162.7(7) . . ? N7 C7 Fe2 174.7(7) . . ? C97 N23 C108 116.8(8) . . ? C97 N23 Co3 127.9(7) . . ? C108 N23 Co3 115.3(5) . . ? N23 C108 C100 122.2(8) . . ? N23 C108 C107 116.7(8) . . ? C100 C108 C107 121.1(9) . . ? C61 N17 C72 117.4(8) . . ? C61 N17 Co2 128.3(6) . . ? C72 N17 Co2 114.3(6) . . ? C70 N18 C71 118.9(8) . . ? C70 N18 Co2 128.2(7) . . ? C71 N18 Co2 112.8(6) . . ? N6 C6 Fe1 170.8(7) . . ? N14 C47 C43 122.9(8) . . ? N14 C47 C48 116.8(7) . . ? C43 C47 C48 120.2(8) . . ? N16 C59 C55 122.7(8) . . ? N16 C59 C60 117.4(7) . . ? C55 C59 C60 119.9(8) . . ? N16 C58 C57 124.2(8) . . ? N10 C10 Fe2 177.3(9) . . ? N15 C60 C52 122.5(8) . . ? N15 C60 C59 116.6(8) . . ? C52 C60 C59 120.9(7) . . ? N21 C96 C88 122.1(7) . . ? N21 C96 C95 116.6(7) . . ? C88 C96 C95 121.3(8) . . ? N22 C95 C91 122.8(8) . . ? N22 C95 C96 117.1(8) . . ? C91 C95 C96 120.1(9) . . ? C107 C103 C104 119.8(9) . . ? C107 C103 C102 115.0(10) . . ? C104 C103 C102 125.2(10) . . ? C38 C39 C40 118.6(8) . . ? C38 C39 C14 122.6(9) . . ? C40 C39 C14 118.8(8) . . ? N21 C85 C86 124.9(8) . . ? C84 N19 C73 116.9(11) . . ? C84 N19 Co2 115.2(7) . . ? C73 N19 Co2 127.9(10) . . ? N13 C48 C40 122.4(8) . . ? N13 C48 C47 116.9(8) . . ? C40 C48 C47 120.7(8) . . ? N3 C3 Fe1 178.2(9) . . ? C51 C50 C49 118.6(8) . . ? C51 C50 C17 121.9(9) . . ? C49 C50 C17 119.5(8) . . ? N13 C37 C38 125.1(8) . . ? N15 C49 C50 125.1(8) . . ? C104 C105 C106 118.8(9) . . ? C104 C105 C36 123.2(10) . . ? C106 C105 C36 117.9(10) . . ? C50 C51 C52 118.2(8) . . ? C50 C51 C18 119.3(9) . . ? C52 C51 C18 122.5(8) . . ? N23 C97 C98 125.5(10) . . ? N9 C9 Fe2 177.7(8) . . ? C63 C64 C72 119.8(8) . . ? C63 C64 C65 125.3(9) . . ? C72 C64 C65 114.9(9) . . ? C99 C100 C108 118.8(9) . . ? C99 C100 C101 125.8(10) . . ? C108 C100 C101 115.3(10) . . ? C44 C43 C47 119.0(10) . . ? C44 C43 C42 123.9(9) . . ? C47 C43 C42 117.1(9) . . ? C57 C56 C55 118.6(7) . . ? C57 C56 C19 119.5(9) . . ? C55 C56 C19 121.8(8) . . ? C48 C40 C39 119.3(8) . . ? C48 C40 C41 117.3(9) . . ? C39 C40 C41 123.4(8) . . ? N17 C72 C64 121.8(8) . . ? N17 C72 C71 116.4(8) . . ? C64 C72 C71 121.8(8) . . ? N18 C71 C67 121.2(9) . . ? N18 C71 C72 118.4(8) . . ? C67 C71 C72 120.4(9) . . ? N1 C1 Fe1 175.9(9) . . ? C44 C45 C46 117.8(9) . . ? C44 C45 C16 124.9(10) . . ? C46 C45 C16 117.3(11) . . ? N24 C107 C103 121.6(8) . . ? N24 C107 C108 116.0(8) . . ? C103 C107 C108 122.4(9) . . ? C39 C38 C37 118.1(8) . . ? C39 C38 C13 123.5(8) . . ? C37 C38 C13 118.4(8) . . ? N14 C46 C45 123.9(10) . . ? C97 C98 C99 119.1(9) . . ? C97 C98 C33 120.5(11) . . ? C99 C98 C33 120.4(10) . . ? N20 C83 C79 124.2(10) . . ? N20 C83 C84 115.8(10) . . ? C79 C83 C84 120.0(10) . . ? C60 C52 C53 117.2(8) . . ? C60 C52 C51 119.0(8) . . ? C53 C52 C51 123.8(9) . . ? N2 C2 Fe1 177.0(9) . . ? C95 C91 C92 118.0(9) . . ? C95 C91 C90 117.5(9) . . ? C92 C91 C90 124.4(9) . . ? C41 C42 C43 121.6(8) . . ? C101 C102 C103 123.4(11) . . ? C89 C88 C96 117.2(9) . . ? C89 C88 C87 123.9(9) . . ? C96 C88 C87 118.8(8) . . ? C98 C99 C100 117.5(8) . . ? C98 C99 C34 122.0(11) . . ? C100 C99 C34 120.4(12) . . ? N17 C61 C62 124.8(8) . . ? C80 C79 C83 117.4(10) . . ? C80 C79 C78 124.4(13) . . ? C83 C79 C78 118.1(12) . . ? N22 C94 C93 124.9(9) . . ? C59 C55 C56 118.9(8) . . ? C59 C55 C54 117.9(8) . . ? C56 C55 C54 123.2(8) . . ? C54 C53 C52 122.8(9) . . ? N20 C82 C81 124.5(9) . . ? C86 C87 C88 117.8(8) . . ? C86 C87 C30 120.9(9) . . ? C88 C87 C30 121.3(9) . . ? C87 C86 C85 118.7(8) . . ? C87 C86 C29 122.5(8) . . ? C85 C86 C29 118.8(8) . . ? C68 C67 C66 123.9(10) . . ? C68 C67 C71 119.1(10) . . ? C66 C67 C71 117.0(10) . . ? N24 C106 C105 123.9(9) . . ? C80 C81 C82 116.7(10) . . ? C80 C81 C28 124.9(10) . . ? C82 C81 C28 118.4(10) . . ? C56 C57 C58 117.7(8) . . ? C56 C57 C20 124.6(8) . . ? C58 C57 C20 117.7(9) . . ? C66 C65 C64 123.6(10) . . ? N12 C12 Fe2 178.1(10) . . ? C42 C41 C40 123.0(9) . . ? C63 C62 C61 117.9(9) . . ? C63 C62 C21 124.2(9) . . ? C61 C62 C21 117.9(8) . . ? C53 C54 C55 121.3(8) . . ? C78 C77 C76 124.0(16) . . ? C105 C104 C103 117.7(9) . . ? C105 C104 C35 119.0(11) . . ? C103 C104 C35 123.3(11) . . ? C62 C63 C64 118.2(9) . . ? C62 C63 C22 119.7(10) . . ? C64 C63 C22 122.1(9) . . ? C43 C44 C45 119.3(9) . . ? C43 C44 C15 119.9(11) . . ? C45 C44 C15 120.8(10) . . ? C89 C90 C91 121.6(10) . . ? N18 C70 C69 123.7(10) . . ? N19 C84 C83 116.4(9) . . ? N19 C84 C76 124.0(13) . . ? C83 C84 C76 119.5(13) . . ? C79 C80 C81 120.5(10) . . ? C79 C80 C27 120.9(11) . . ? C81 C80 C27 118.6(12) . . ? C102 C101 C100 122.7(10) . . ? C73 C74 C75 120.5(14) . . ? C73 C74 C25 113(2) . . ? C75 C74 C25 126.7(17) . . ? C92 C93 C94 119.1(9) . . ? C92 C93 C32 123.3(10) . . ? C94 C93 C32 117.5(10) . . ? C77 C78 C79 121.1(16) . . ? N11 C11 Fe2 177.8(12) . . ? C69 C68 C67 118.5(9) . . ? C69 C68 C23 119.5(10) . . ? C67 C68 C23 122.1(11) . . ? C90 C89 C88 122.1(10) . . ? C93 C92 C91 118.2(9) . . ? C93 C92 C31 121.5(10) . . ? C91 C92 C31 120.2(10) . . ? C68 C69 C70 118.7(10) . . ? C68 C69 C24 124.4(10) . . ? C70 C69 C24 116.9(11) . . ? N19 C73 C74 122.6(15) . . ? C74 C75 C76 118.6(15) . . ? C74 C75 C26 118(2) . . ? C76 C75 C26 124(2) . . ? C65 C66 C67 122.2(10) . . ? C75 C76 C77 125.5(16) . . ? C75 C76 C84 117.3(16) . . ? C77 C76 C84 117.2(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.931 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.107 #end============================================= data_{[Co(tmphen)2]3[Fe(CN)6]2}_293K #========================================================================= _audit_creation_method SHELXL-97 _chemical_name_systematic ; '{[Co(tmphen)2]3[Fe(CN)6]2}.6H2O' ; _chemical_name_common '{[Co(tmphen)2]3[Fe(CN)6]2}.6H2O' _chemical_melting_point ? _chemical_formula_moiety 'C108 H108 Co3 Fe2 N24 O6' _chemical_formula_sum 'C108 H108 Co3 Fe2 N24 O6' _chemical_formula_weight 2126.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.04(2) _cell_length_b 24.91(3) _cell_length_c 24.62(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.64(8) _cell_angle_gamma 90.00 _cell_volume 11569(25) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used '54644' _cell_measurement_theta_min '2.220' _cell_measurement_theta_max '20.494' _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max '0.18' _exptl_crystal_size_mid '0.16' _exptl_crystal_size_min '0.14' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4372 _exptl_absorpt_coefficient_mu 0.725 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min '0.8774' _exptl_absorpt_correction_T_max '0.9035' _exptl_absorpt_process_details 'SADABS: Bruker,2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'BRUKER APEX' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30410 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.0903 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 20.81 _reflns_number_total 12078 _reflns_number_gt 7612 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER, 2000)' _computing_cell_refinement 'SAINT (BRUKER, 2001)' _computing_data_reduction 'SAINT (BRUKER, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1415P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00097(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12078 _refine_ls_number_parameters 1331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1167 _refine_ls_R_factor_gt 0.0735 _refine_ls_wR_factor_ref 0.2365 _refine_ls_wR_factor_gt 0.2089 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.56088(6) 0.37089(5) 0.61630(5) 0.0490(4) Uani 1 1 d . . . Fe1 Fe 0.82377(6) 0.34881(5) 0.63268(5) 0.0491(4) Uani 1 1 d . . . O19S O 1.1940(12) 0.4813(9) 1.0074(8) 0.148(7) Uiso 0.50 1 d P A -19 N1 N 0.8092(5) 0.3246(4) 0.5110(4) 0.084(3) Uani 1 1 d . . . C1 C 0.8140(5) 0.3346(4) 0.5564(4) 0.058(3) Uani 1 1 d . . . Co2 Co 0.79067(7) 0.36860(5) 0.83018(5) 0.0555(4) Uani 1 1 d . . . Fe2 Fe 0.63469(7) 0.51810(5) 0.75169(5) 0.0506(4) Uani 1 1 d . . . O17S O 0.9398(13) 0.2277(9) 0.5496(9) 0.156(8) Uiso 0.50 1 d P B -17 N2 N 0.8248(5) 0.2284(4) 0.6531(4) 0.083(3) Uani 1 1 d . . . C2 C 0.8246(5) 0.2726(4) 0.6454(4) 0.059(3) Uani 1 1 d . . . Co3 Co 0.85389(6) 0.54612(4) 0.66225(5) 0.0508(4) Uani 1 1 d . . . O4S O 1.0024(18) 0.2907(10) 1.0637(11) 0.185(10) Uiso 0.50 1 d P C -4 N3 N 0.9847(5) 0.3529(4) 0.6377(4) 0.090(3) Uani 1 1 d . . . C3 C 0.9254(6) 0.3507(4) 0.6364(4) 0.062(3) Uani 1 1 d . . . O8S O 0.6193(13) 0.4775(9) 0.9264(10) 0.168(8) Uiso 0.50 1 d P D -8 N4 N 0.6626(5) 0.3444(3) 0.6262(3) 0.053(2) Uani 1 1 d . . . C4 C 0.7223(6) 0.3461(3) 0.6289(3) 0.051(2) Uani 1 1 d . . . O9S O 0.5886(16) 0.4458(13) 0.9613(13) 0.089(9) Uiso 0.25 1 d P E -9 N5 N 0.8251(4) 0.3657(3) 0.7551(4) 0.063(2) Uani 1 1 d . . . C5 C 0.8289(5) 0.3601(3) 0.7097(4) 0.049(2) Uani 1 1 d . . . O3S O 1.0647(16) 0.2946(10) 1.0761(11) 0.187(10) Uiso 0.50 1 d P F -3 N6 N 0.8301(4) 0.4704(3) 0.6284(3) 0.058(2) Uani 1 1 d . . . C6 C 0.8243(4) 0.4246(4) 0.6260(3) 0.048(2) Uani 1 1 d . . . O16S O 0.5699(18) 0.0836(14) 0.4871(14) 0.111(11) Uiso 0.25 1 d P G -16 N7 N 0.5895(4) 0.4408(3) 0.6566(3) 0.058(2) Uani 1 1 d . . . C7 C 0.6073(5) 0.4709(4) 0.6900(4) 0.049(2) Uani 1 1 d . . . O7S O 0.7620(18) 0.6936(15) 0.8099(13) 0.112(11) Uiso 0.25 1 d P H -7 N8 N 0.7108(4) 0.4219(3) 0.8086(3) 0.063(2) Uani 1 1 d . . . C8 C 0.6787(5) 0.4568(4) 0.7885(4) 0.054(2) Uani 1 1 d . . . O11S O 0.740(3) 0.053(2) 0.781(2) 0.23(2) Uiso 0.25 1 d P I -11 N9 N 0.7735(4) 0.5424(3) 0.7078(3) 0.060(2) Uani 1 1 d . . . C9 C 0.7223(5) 0.5334(3) 0.7248(4) 0.052(2) Uani 1 1 d . . . O10S O 0.410(2) 0.5728(15) 0.8652(16) 0.137(13) Uiso 0.25 1 d P J -10 N10 N 0.5803(5) 0.6181(4) 0.6900(4) 0.085(3) Uani 1 1 d . . . C10 C 0.5992(5) 0.5802(4) 0.7138(4) 0.063(3) Uani 1 1 d . . . O18S O 0.7168(18) 0.8461(12) 0.6207(13) 0.245(13) Uiso 0.50 1 d P K -18 N11 N 0.4925(6) 0.4928(5) 0.7909(5) 0.132(5) Uani 1 1 d . . . C11 C 0.5434(7) 0.5030(5) 0.7760(5) 0.086(4) Uani 1 1 d . . . O6S O 0.7726(19) 0.6069(15) 0.9753(15) 0.118(11) Uiso 0.25 1 d P L -6 N12 N 0.6803(5) 0.5828(4) 0.8531(4) 0.093(3) Uani 1 1 d . . . C12 C 0.6628(5) 0.5589(4) 0.8149(4) 0.065(3) Uani 1 1 d . . . O5S O 0.780(2) 0.5599(19) 0.9927(15) 0.127(13) Uiso 0.25 1 d P M -5 N13 N 0.5709(4) 0.3970(3) 0.5351(3) 0.0522(19) Uani 1 1 d . . . O2S O 1.204(4) 0.615(3) 0.709(3) 0.25(3) Uiso 0.25 1 d P N -2 N14 N 0.4588(4) 0.4024(3) 0.5887(3) 0.056(2) Uani 1 1 d . . . C14 C 0.7382(6) 0.6179(4) 0.6007(4) 0.067(3) Uani 1 1 d . . . H14 H 0.7120 0.6085 0.6286 0.081 Uiso 1 1 calc R . . O14S O 0.259(3) 0.241(3) 0.688(2) 0.19(2) Uiso 0.25 1 d P O -14 N15 N 0.5162(4) 0.2952(3) 0.5901(3) 0.0496(19) Uani 1 1 d . . . C15 C 0.7096(6) 0.6539(4) 0.5621(5) 0.081(3) Uani 1 1 d . . . O13S O 0.316(3) 0.3935(19) 0.813(2) 0.188(19) Uiso 0.25 1 d P P -13 N16 N 0.5306(4) 0.3358(3) 0.6894(3) 0.056(2) Uani 1 1 d . . . C16 C 0.7478(7) 0.6669(4) 0.5197(5) 0.079(3) Uani 1 1 d . . . O12S O 0.674(2) 0.0622(17) 0.6748(18) 0.161(16) Uiso 0.25 1 d P Q -12 N17 N 0.7232(4) 0.3010(3) 0.8110(3) 0.057(2) Uani 1 1 d . . . C17 C 0.8146(7) 0.6429(4) 0.5194(5) 0.074(3) Uani 1 1 d . . . N18 N 0.7557(4) 0.3506(3) 0.9075(3) 0.067(2) Uani 1 1 d . . . C18 C 0.8572(9) 0.6514(5) 0.4776(5) 0.100(4) Uani 1 1 d . . . H18 H 0.8412 0.6744 0.4488 0.120 Uiso 1 1 calc R . . O15S O 0.273(2) 0.285(2) 0.6860(18) 0.156(16) Uiso 0.25 1 d P R -15 N19 N 0.8823(5) 0.3243(4) 0.8638(3) 0.073(2) Uani 1 1 d . . . C19 C 0.9221(8) 0.6264(5) 0.4782(5) 0.091(4) Uani 1 1 d . . . H19 H 0.9476 0.6318 0.4490 0.109 Uiso 1 1 calc R . . N20 N 0.8627(4) 0.4287(3) 0.8585(3) 0.061(2) Uani 1 1 d . . . C20 C 0.9502(7) 0.5934(4) 0.5212(5) 0.073(3) Uani 1 1 d . . . N21 N 0.9367(4) 0.5187(3) 0.7216(3) 0.0522(19) Uani 1 1 d . . . C21 C 1.0148(7) 0.5687(5) 0.5243(5) 0.080(3) Uani 1 1 d . . . N22 N 0.8967(4) 0.6190(3) 0.7016(3) 0.058(2) Uani 1 1 d . . . C22 C 1.0369(6) 0.5393(4) 0.5707(5) 0.079(3) Uani 1 1 d . . . N23 N 0.9295(4) 0.5555(3) 0.6062(3) 0.060(2) Uani 1 1 d . . . C23 C 0.9917(6) 0.5334(4) 0.6083(4) 0.070(3) Uani 1 1 d . . . H23 H 1.0063 0.5115 0.6383 0.084 Uiso 1 1 calc R . . N24 N 0.8018(4) 0.5957(3) 0.6005(3) 0.059(2) Uani 1 1 d . . . C24 C 0.9091(5) 0.5846(4) 0.5626(4) 0.058(3) Uani 1 1 d . . . C25 C 0.8396(6) 0.6091(4) 0.5606(4) 0.056(3) Uani 1 1 d . . . C26 C 0.6376(6) 0.6769(4) 0.5678(5) 0.098(4) Uani 1 1 d . . . H26A H 0.6408 0.7153 0.5700 0.146 Uiso 1 1 calc R . . H26B H 0.6218 0.6632 0.6006 0.146 Uiso 1 1 calc R . . H26C H 0.6045 0.6669 0.5366 0.146 Uiso 1 1 calc R . . C27 C 0.7181(8) 0.7061(5) 0.4771(5) 0.134(5) Uani 1 1 d . . . H27A H 0.6952 0.7347 0.4940 0.202 Uiso 1 1 calc R . . H27B H 0.6843 0.6883 0.4507 0.202 Uiso 1 1 calc R . . H27C H 0.7557 0.7204 0.4591 0.202 Uiso 1 1 calc R . . C28 C 1.0625(7) 0.5765(5) 0.4814(5) 0.116(5) Uani 1 1 d . . . H28A H 1.1048 0.5947 0.4971 0.174 Uiso 1 1 calc R . . H28B H 1.0386 0.5977 0.4519 0.174 Uiso 1 1 calc R . . H28C H 1.0746 0.5422 0.4675 0.174 Uiso 1 1 calc R . . C29 C 1.1083(6) 0.5129(5) 0.5784(6) 0.115(5) Uani 1 1 d . . . H29A H 1.1446 0.5399 0.5797 0.172 Uiso 1 1 calc R . . H29B H 1.1121 0.4890 0.5484 0.172 Uiso 1 1 calc R . . H29C H 1.1141 0.4930 0.6121 0.172 Uiso 1 1 calc R . . C30 C 0.8734(6) 0.6681(4) 0.6937(4) 0.076(3) Uani 1 1 d . . . H30 H 0.8298 0.6731 0.6724 0.091 Uiso 1 1 calc R . . C31 C 0.9101(7) 0.7131(4) 0.7153(5) 0.083(3) Uani 1 1 d . . . C32 C 0.9719(7) 0.7063(5) 0.7463(5) 0.092(4) Uani 1 1 d . . . C33 C 0.9982(7) 0.6529(4) 0.7568(5) 0.080(3) Uani 1 1 d . . . C34 C 1.0629(7) 0.6415(5) 0.7883(5) 0.102(4) Uani 1 1 d . . . H34 H 1.0917 0.6696 0.8029 0.123 Uiso 1 1 calc R . . C35 C 1.0836(7) 0.5919(5) 0.7975(5) 0.106(4) Uani 1 1 d . . . H35 H 1.1265 0.5860 0.8194 0.128 Uiso 1 1 calc R . . C36 C 1.0438(6) 0.5462(4) 0.7757(4) 0.072(3) Uani 1 1 d . . . C37 C 1.0632(6) 0.4936(4) 0.7841(4) 0.076(3) Uani 1 1 d . . . C38 C 1.0181(6) 0.4556(4) 0.7635(4) 0.067(3) Uani 1 1 d . . . C39 C 0.9562(5) 0.4704(4) 0.7321(4) 0.064(3) Uani 1 1 d . . . H39 H 0.9262 0.4431 0.7173 0.076 Uiso 1 1 calc R . . C40 C 0.9803(5) 0.5581(4) 0.7444(4) 0.062(3) Uani 1 1 d . . . C41 C 0.9572(5) 0.6119(4) 0.7338(4) 0.060(3) Uani 1 1 d . . . C42 C 0.8763(7) 0.7662(4) 0.7027(5) 0.112(5) Uani 1 1 d . . . H42A H 0.9001 0.7845 0.6761 0.168 Uiso 1 1 calc R . . H42B H 0.8796 0.7873 0.7356 0.168 Uiso 1 1 calc R . . H42C H 0.8274 0.7612 0.6883 0.168 Uiso 1 1 calc R . . C43 C 1.0145(8) 0.7549(4) 0.7683(6) 0.157(7) Uani 1 1 d . . . H43A H 0.9829 0.7833 0.7753 0.235 Uiso 1 1 calc R . . H43B H 1.0439 0.7667 0.7418 0.235 Uiso 1 1 calc R . . H43C H 1.0438 0.7455 0.8017 0.235 Uiso 1 1 calc R . . C44 C 1.1324(7) 0.4792(5) 0.8157(6) 0.128(5) Uani 1 1 d . . . H44A H 1.1342 0.4412 0.8220 0.191 Uiso 1 1 calc R . . H44B H 1.1378 0.4977 0.8502 0.191 Uiso 1 1 calc R . . H44C H 1.1699 0.4895 0.7954 0.191 Uiso 1 1 calc R . . C45 C 1.0327(6) 0.3973(4) 0.7698(5) 0.099(4) Uani 1 1 d . . . H45A H 1.0346 0.3875 0.8077 0.148 Uiso 1 1 calc R . . H45B H 1.0774 0.3893 0.7576 0.148 Uiso 1 1 calc R . . H45C H 0.9958 0.3774 0.7483 0.148 Uiso 1 1 calc R . . C46 C 0.8529(6) 0.4800(5) 0.8547(4) 0.071(3) Uani 1 1 d . . . H46 H 0.8094 0.4923 0.8374 0.086 Uiso 1 1 calc R . . C47 C 0.9043(7) 0.5186(5) 0.8751(5) 0.089(4) Uani 1 1 d . . . C48 C 0.9657(7) 0.5010(6) 0.9021(5) 0.094(4) Uani 1 1 d . . . C49 C 0.9788(7) 0.4457(5) 0.9061(5) 0.089(4) Uani 1 1 d . . . C50 C 1.0417(8) 0.4238(8) 0.9329(7) 0.151(7) Uani 1 1 d . . . H50 H 1.0767 0.4463 0.9503 0.181 Uiso 1 1 calc R . . C51 C 1.0516(8) 0.3718(8) 0.9337(6) 0.133(6) Uani 1 1 d . . . H51 H 1.0952 0.3587 0.9499 0.160 Uiso 1 1 calc R . . C52 C 0.9990(7) 0.3338(6) 0.9110(5) 0.098(4) Uani 1 1 d . . . C53 C 1.0047(9) 0.2770(7) 0.9107(6) 0.115(5) Uani 1 1 d . . . C54 C 0.9500(9) 0.2456(6) 0.8881(6) 0.108(4) Uani 1 1 d . . . C55 C 0.8893(7) 0.2721(5) 0.8648(5) 0.094(4) Uani 1 1 d . . . H55 H 0.8514 0.2515 0.8489 0.112 Uiso 1 1 calc R . . C56 C 0.9358(6) 0.3554(5) 0.8853(4) 0.072(3) Uani 1 1 d . . . C57 C 0.9242(6) 0.4113(5) 0.8835(4) 0.072(3) Uani 1 1 d . . . C58 C 0.8840(7) 0.5758(4) 0.8656(6) 0.122(5) Uani 1 1 d . . . H58A H 0.9121 0.5914 0.8401 0.182 Uiso 1 1 calc R . . H58B H 0.8919 0.5951 0.8997 0.182 Uiso 1 1 calc R . . H58C H 0.8347 0.5780 0.8510 0.182 Uiso 1 1 calc R . . C59 C 1.0187(8) 0.5421(5) 0.9270(6) 0.144(6) Uani 1 1 d . . . H59A H 0.9941 0.5720 0.9401 0.216 Uiso 1 1 calc R . . H59B H 1.0469 0.5541 0.8998 0.216 Uiso 1 1 calc R . . H59C H 1.0489 0.5261 0.9570 0.216 Uiso 1 1 calc R . . C60 C 1.0761(8) 0.2527(6) 0.9369(7) 0.166(7) Uani 1 1 d . . . H60A H 1.1144 0.2747 0.9280 0.249 Uiso 1 1 calc R . . H60B H 1.0809 0.2171 0.9231 0.249 Uiso 1 1 calc R . . H60C H 1.0772 0.2513 0.9760 0.249 Uiso 1 1 calc R . . C61 C 0.9518(9) 0.1865(5) 0.8888(7) 0.165(7) Uani 1 1 d . . . H61A H 0.9804 0.1744 0.9216 0.248 Uiso 1 1 calc R . . H61B H 0.9716 0.1737 0.8574 0.248 Uiso 1 1 calc R . . H61C H 0.9045 0.1729 0.8880 0.248 Uiso 1 1 calc R . . C62 C 0.7728(6) 0.3731(4) 0.9539(4) 0.077(3) Uani 1 1 d . . . H62 H 0.8011 0.4036 0.9555 0.093 Uiso 1 1 calc R . . C63 C 0.7514(7) 0.3546(5) 1.0022(4) 0.085(3) Uani 1 1 d . . . C64 C 0.7085(6) 0.3110(5) 1.0017(5) 0.078(3) Uani 1 1 d . . . C65 C 0.6893(6) 0.2866(4) 0.9514(4) 0.065(3) Uani 1 1 d . . . C66 C 0.6458(6) 0.2431(5) 0.9461(5) 0.085(3) Uani 1 1 d . . . H66 H 0.6287 0.2293 0.9769 0.102 Uiso 1 1 calc R . . C67 C 0.6270(6) 0.2195(4) 0.8973(6) 0.086(3) Uani 1 1 d . . . H67 H 0.5961 0.1905 0.8957 0.103 Uiso 1 1 calc R . . C68 C 0.6518(5) 0.2365(4) 0.8472(5) 0.069(3) Uani 1 1 d . . . C69 C 0.6355(6) 0.2126(4) 0.7970(5) 0.071(3) Uani 1 1 d . . . C70 C 0.6647(6) 0.2344(4) 0.7547(4) 0.065(3) Uani 1 1 d . . . C71 C 0.7079(5) 0.2792(4) 0.7640(4) 0.067(3) Uani 1 1 d . . . H71 H 0.7267 0.2942 0.7344 0.080 Uiso 1 1 calc R . . C72 C 0.6960(5) 0.2810(4) 0.8543(4) 0.058(3) Uani 1 1 d . . . C73 C 0.7139(5) 0.3062(4) 0.9056(4) 0.058(3) Uani 1 1 d . . . C74 C 0.7784(8) 0.3864(5) 1.0534(5) 0.121(5) Uani 1 1 d . . . H74A H 0.8001 0.3624 1.0812 0.181 Uiso 1 1 calc R . . H74B H 0.7395 0.4047 1.0664 0.181 Uiso 1 1 calc R . . H74C H 0.8128 0.4122 1.0448 0.181 Uiso 1 1 calc R . . C75 C 0.6833(7) 0.2918(5) 1.0525(4) 0.110(4) Uani 1 1 d . . . H75A H 0.6332 0.2981 1.0504 0.166 Uiso 1 1 calc R . . H75B H 0.7076 0.3108 1.0833 0.166 Uiso 1 1 calc R . . H75C H 0.6926 0.2541 1.0568 0.166 Uiso 1 1 calc R . . C76 C 0.5916(6) 0.1636(4) 0.7887(5) 0.092(4) Uani 1 1 d . . . H76A H 0.6218 0.1328 0.7878 0.139 Uiso 1 1 calc R . . H76B H 0.5608 0.1662 0.7546 0.139 Uiso 1 1 calc R . . H76C H 0.5637 0.1599 0.8183 0.139 Uiso 1 1 calc R . . C77 C 0.6535(6) 0.2126(4) 0.6987(4) 0.089(3) Uani 1 1 d . . . H77A H 0.6040 0.2056 0.6882 0.133 Uiso 1 1 calc R . . H77B H 0.6798 0.1798 0.6975 0.133 Uiso 1 1 calc R . . H77C H 0.6695 0.2382 0.6739 0.133 Uiso 1 1 calc R . . C78 C 0.5410(5) 0.3559(4) 0.7388(4) 0.063(3) Uani 1 1 d . . . H78 H 0.5670 0.3875 0.7446 0.075 Uiso 1 1 calc R . . C79 C 0.5148(5) 0.3318(4) 0.7830(4) 0.064(3) Uani 1 1 d . . . C80 C 0.4778(6) 0.2857(4) 0.7757(4) 0.068(3) Uani 1 1 d . . . C81 C 0.4696(5) 0.2630(4) 0.7239(4) 0.061(3) Uani 1 1 d . . . C82 C 0.4363(6) 0.2129(5) 0.7118(4) 0.087(4) Uani 1 1 d . . . H82 H 0.4177 0.1943 0.7394 0.105 Uiso 1 1 calc R . . C83 C 0.4311(6) 0.1923(4) 0.6628(5) 0.091(4) Uani 1 1 d . . . H83 H 0.4097 0.1589 0.6569 0.109 Uiso 1 1 calc R . . C84 C 0.4565(5) 0.2184(4) 0.6180(4) 0.063(3) Uani 1 1 d . . . C85 C 0.4523(5) 0.1972(4) 0.5650(4) 0.071(3) Uani 1 1 d . . . C86 C 0.4777(5) 0.2256(4) 0.5261(4) 0.063(3) Uani 1 1 d . . . C87 C 0.5083(5) 0.2746(4) 0.5408(4) 0.061(3) Uani 1 1 d . . . H87 H 0.5247 0.2947 0.5132 0.074 Uiso 1 1 calc R . . C88 C 0.5306(6) 0.3599(4) 0.8359(4) 0.080(3) Uani 1 1 d . . . H88A H 0.5539 0.3357 0.8628 0.120 Uiso 1 1 calc R . . H88B H 0.4872 0.3723 0.8475 0.120 Uiso 1 1 calc R . . H88C H 0.5609 0.3900 0.8318 0.120 Uiso 1 1 calc R . . C89 C 0.4466(7) 0.2594(4) 0.8219(4) 0.091(4) Uani 1 1 d . . . H89A H 0.4034 0.2774 0.8273 0.137 Uiso 1 1 calc R . . H89B H 0.4796 0.2618 0.8549 0.137 Uiso 1 1 calc R . . H89C H 0.4368 0.2224 0.8132 0.137 Uiso 1 1 calc R . . C91 C 0.4756(6) 0.2078(4) 0.4691(4) 0.092(4) Uani 1 1 d . . . H91A H 0.4272 0.2053 0.4524 0.138 Uiso 1 1 calc R . . H91B H 0.4978 0.1732 0.4684 0.138 Uiso 1 1 calc R . . H91C H 0.5004 0.2331 0.4493 0.138 Uiso 1 1 calc R . . C92 C 0.4050(6) 0.4047(4) 0.6152(4) 0.073(3) Uani 1 1 d . . . H92 H 0.4091 0.3903 0.6503 0.088 Uiso 1 1 calc R . . C93 C 0.3401(6) 0.4281(5) 0.5931(7) 0.089(4) Uani 1 1 d . . . C94 C 0.3344(6) 0.4481(4) 0.5416(6) 0.083(4) Uani 1 1 d . . . C95 C 0.3901(5) 0.4452(4) 0.5127(5) 0.060(3) Uani 1 1 d . . . C97 C 0.4447(7) 0.4601(4) 0.4329(5) 0.072(3) Uani 1 1 d . . . H97 H 0.4407 0.4723 0.3969 0.087 Uiso 1 1 calc R . . C98 C 0.5076(6) 0.4384(4) 0.4554(4) 0.058(3) Uani 1 1 d . . . C99 C 0.5664(6) 0.4334(4) 0.4292(4) 0.065(3) Uani 1 1 d . . . C100 C 0.6271(6) 0.4095(4) 0.4551(4) 0.069(3) Uani 1 1 d . . . C101 C 0.6255(5) 0.3927(4) 0.5091(4) 0.061(3) Uani 1 1 d . . . H101 H 0.6664 0.3774 0.5276 0.073 Uiso 1 1 calc R . . C102 C 0.2808(7) 0.4279(6) 0.6305(6) 0.134(5) Uani 1 1 d . . . H10D H 0.2360 0.4213 0.6087 0.201 Uiso 1 1 calc R . . H10E H 0.2796 0.4621 0.6484 0.201 Uiso 1 1 calc R . . H10F H 0.2901 0.4001 0.6575 0.201 Uiso 1 1 calc R . . C103 C 0.2644(6) 0.4748(5) 0.5161(6) 0.117(5) Uani 1 1 d . . . H10J H 0.2691 0.5132 0.5187 0.175 Uiso 1 1 calc R . . H10K H 0.2265 0.4633 0.5355 0.175 Uiso 1 1 calc R . . H10L H 0.2542 0.4646 0.4783 0.175 Uiso 1 1 calc R . . C104 C 0.5652(6) 0.4538(4) 0.3710(4) 0.082(3) Uani 1 1 d . . . H10A H 0.5455 0.4893 0.3682 0.123 Uiso 1 1 calc R . . H10B H 0.5367 0.4303 0.3462 0.123 Uiso 1 1 calc R . . H10C H 0.6126 0.4546 0.3618 0.123 Uiso 1 1 calc R . . C105 C 0.6941(6) 0.4018(5) 0.4300(4) 0.094(4) Uani 1 1 d . . . H10G H 0.6841 0.3814 0.3968 0.141 Uiso 1 1 calc R . . H10H H 0.7282 0.3829 0.4553 0.141 Uiso 1 1 calc R . . H10I H 0.7130 0.4362 0.4219 0.141 Uiso 1 1 calc R . . C106 C 0.4886(5) 0.2667(4) 0.6288(3) 0.047(2) Uani 1 1 d . . . C107 C 0.4965(5) 0.2894(4) 0.6813(4) 0.052(2) Uani 1 1 d . . . C108 C 0.4173(7) 0.1443(4) 0.5515(5) 0.113(5) Uani 1 1 d . . . H10M H 0.4494 0.1158 0.5641 0.170 Uiso 1 1 calc R . . H10N H 0.4046 0.1414 0.5125 0.170 Uiso 1 1 calc R . . H10O H 0.3754 0.1416 0.5691 0.170 Uiso 1 1 calc R . . C109 C 0.4519(5) 0.4221(4) 0.5377(4) 0.053(2) Uani 1 1 d . . . C110 C 0.5109(5) 0.4190(3) 0.5097(4) 0.055(2) Uani 1 1 d . . . C111 C 0.3892(7) 0.4646(4) 0.4593(5) 0.077(3) Uani 1 1 d . . . H111 H 0.3485 0.4812 0.4420 0.092 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0456(8) 0.0558(8) 0.0457(7) 0.0043(6) 0.0072(6) -0.0053(6) Fe1 0.0459(8) 0.0466(8) 0.0557(8) 0.0000(6) 0.0098(6) 0.0012(6) N1 0.082(7) 0.098(7) 0.072(6) -0.003(6) 0.013(6) -0.002(5) C1 0.056(7) 0.062(7) 0.057(7) 0.002(6) 0.011(5) 0.000(5) Co2 0.0643(9) 0.0502(8) 0.0512(8) 0.0062(6) 0.0053(6) 0.0009(6) Fe2 0.0474(9) 0.0540(9) 0.0517(8) -0.0012(6) 0.0116(6) 0.0064(6) N2 0.088(7) 0.035(5) 0.122(8) 0.007(5) -0.009(6) 0.003(5) C2 0.044(6) 0.050(7) 0.080(7) -0.007(6) 0.001(5) 0.007(5) Co3 0.0426(8) 0.0424(8) 0.0682(9) 0.0030(6) 0.0104(6) -0.0017(6) N3 0.057(7) 0.116(8) 0.099(7) 0.000(6) 0.021(6) -0.004(6) C3 0.061(7) 0.062(7) 0.064(7) 0.005(5) 0.011(6) 0.002(6) N4 0.055(6) 0.050(5) 0.053(5) 0.007(4) 0.006(4) 0.003(4) C4 0.058(7) 0.050(6) 0.045(6) 0.008(4) 0.005(5) 0.006(5) N5 0.065(6) 0.060(6) 0.065(6) -0.006(5) 0.015(5) -0.006(4) C5 0.043(6) 0.039(6) 0.066(7) -0.006(5) 0.011(5) -0.007(4) N6 0.054(5) 0.053(5) 0.070(5) 0.001(4) 0.015(4) -0.009(4) C6 0.042(6) 0.053(6) 0.053(6) 0.007(5) 0.019(4) -0.006(5) N7 0.061(6) 0.060(6) 0.052(5) 0.008(4) 0.002(4) -0.006(4) C7 0.046(6) 0.045(6) 0.059(6) 0.021(5) 0.015(5) 0.000(5) N8 0.061(6) 0.056(6) 0.072(6) 0.003(5) 0.014(5) 0.003(4) C8 0.049(6) 0.056(7) 0.056(6) -0.013(5) 0.009(5) -0.006(5) N9 0.050(6) 0.055(5) 0.077(6) 0.000(4) 0.012(5) 0.004(4) C9 0.052(7) 0.043(6) 0.058(6) 0.004(5) -0.005(5) 0.009(5) N10 0.099(8) 0.061(6) 0.091(7) -0.007(5) 0.004(6) 0.023(5) C10 0.070(7) 0.058(7) 0.060(7) -0.018(6) 0.011(6) 0.013(6) N11 0.088(9) 0.156(11) 0.165(12) 0.022(9) 0.065(9) 0.008(8) C11 0.075(9) 0.109(10) 0.078(8) -0.007(7) 0.029(7) 0.010(7) N12 0.106(8) 0.086(7) 0.084(7) -0.015(6) 0.000(6) 0.026(6) C12 0.069(7) 0.068(8) 0.057(7) -0.006(6) 0.007(6) 0.019(6) N13 0.047(5) 0.063(5) 0.048(5) 0.008(4) 0.011(4) -0.001(4) N14 0.051(6) 0.064(5) 0.056(5) -0.005(4) 0.016(4) -0.004(4) C14 0.058(8) 0.057(7) 0.083(8) 0.003(6) -0.007(6) -0.004(6) N15 0.043(5) 0.062(5) 0.043(5) -0.001(4) 0.003(4) -0.001(4) C15 0.090(9) 0.055(7) 0.093(9) 0.000(7) -0.013(8) 0.004(7) N16 0.054(5) 0.063(6) 0.053(6) 0.010(4) 0.009(4) -0.011(4) C16 0.108(11) 0.058(7) 0.069(8) 0.017(6) -0.003(7) -0.002(7) N17 0.064(6) 0.057(5) 0.050(5) 0.000(5) 0.005(4) 0.002(4) C17 0.085(9) 0.060(7) 0.077(8) 0.013(6) 0.013(7) -0.005(6) N18 0.072(6) 0.065(6) 0.065(7) 0.018(5) 0.013(5) 0.000(5) C18 0.156(14) 0.068(9) 0.077(9) 0.015(7) 0.015(10) -0.016(9) N19 0.081(7) 0.073(7) 0.064(6) 0.004(5) 0.004(5) 0.013(6) C19 0.124(12) 0.081(9) 0.074(9) 0.000(8) 0.033(8) -0.026(8) N20 0.069(6) 0.046(6) 0.064(5) 0.006(4) -0.010(5) 0.007(4) C20 0.086(9) 0.065(8) 0.070(8) 0.011(6) 0.021(7) -0.025(7) N21 0.050(5) 0.038(5) 0.069(5) -0.003(4) 0.006(4) 0.000(4) C21 0.060(8) 0.084(8) 0.104(10) -0.033(8) 0.042(8) -0.031(7) N22 0.060(6) 0.035(5) 0.078(6) 0.002(4) 0.009(5) 0.009(4) C22 0.070(9) 0.075(8) 0.093(9) -0.007(7) 0.012(8) -0.006(6) N23 0.056(6) 0.055(5) 0.071(6) 0.002(5) 0.020(5) -0.004(4) C23 0.051(7) 0.079(8) 0.086(8) -0.006(6) 0.033(6) 0.000(6) N24 0.052(6) 0.054(5) 0.070(6) 0.006(4) 0.003(5) 0.003(4) C24 0.057(7) 0.060(7) 0.062(7) -0.010(6) 0.019(6) -0.015(6) C25 0.070(8) 0.045(6) 0.053(6) 0.004(5) 0.010(6) -0.012(5) C26 0.084(9) 0.089(9) 0.114(10) -0.003(7) -0.010(7) 0.025(7) C27 0.161(15) 0.117(11) 0.117(11) 0.050(9) -0.011(10) 0.012(10) C28 0.122(11) 0.117(10) 0.128(11) -0.021(8) 0.088(10) -0.051(8) C29 0.058(8) 0.138(11) 0.157(12) -0.030(9) 0.046(8) 0.003(8) C30 0.075(8) 0.052(8) 0.098(8) -0.004(6) 0.003(6) 0.001(6) C31 0.095(10) 0.043(7) 0.106(9) 0.002(6) -0.009(8) -0.002(7) C32 0.088(10) 0.065(9) 0.116(10) -0.019(7) -0.015(8) -0.013(7) C33 0.099(9) 0.038(7) 0.097(9) -0.006(6) -0.007(7) -0.007(7) C34 0.095(10) 0.061(9) 0.133(11) 0.001(7) -0.047(8) -0.013(7) C35 0.098(10) 0.067(9) 0.137(12) 0.008(8) -0.049(8) -0.013(8) C36 0.062(8) 0.065(8) 0.084(8) 0.008(6) -0.013(6) -0.012(6) C37 0.076(8) 0.049(8) 0.095(8) 0.011(6) -0.021(7) 0.014(6) C38 0.072(8) 0.043(7) 0.083(7) 0.003(6) -0.006(6) 0.010(6) C39 0.063(7) 0.033(6) 0.094(8) -0.004(5) 0.007(6) 0.007(5) C40 0.055(7) 0.049(7) 0.080(7) 0.000(6) 0.006(6) -0.006(6) C41 0.057(7) 0.040(7) 0.082(7) 0.001(5) 0.002(6) -0.006(6) C42 0.140(12) 0.048(8) 0.137(11) 0.003(7) -0.024(9) 0.007(7) C43 0.171(15) 0.048(8) 0.222(17) -0.015(9) -0.081(13) -0.035(8) C44 0.098(10) 0.079(9) 0.189(15) 0.000(9) -0.045(10) 0.017(7) C45 0.109(10) 0.049(7) 0.126(10) 0.002(6) -0.030(8) 0.020(6) C46 0.068(8) 0.077(9) 0.068(7) -0.003(6) 0.008(6) -0.001(7) C47 0.098(11) 0.073(9) 0.097(9) -0.023(7) 0.015(8) -0.014(8) C48 0.071(9) 0.110(12) 0.096(9) -0.034(8) -0.012(7) -0.018(8) C49 0.107(11) 0.075(9) 0.077(8) -0.009(7) -0.009(8) -0.001(8) C50 0.121(14) 0.126(14) 0.177(16) -0.010(12) -0.086(12) 0.010(11) C51 0.082(11) 0.162(16) 0.141(13) 0.002(13) -0.041(9) 0.002(12) C52 0.102(11) 0.101(11) 0.085(9) 0.016(8) -0.012(8) 0.038(9) C53 0.123(14) 0.120(14) 0.098(10) 0.031(9) -0.002(9) 0.062(11) C54 0.106(12) 0.104(12) 0.110(11) 0.020(9) -0.002(9) 0.026(10) C55 0.125(12) 0.055(9) 0.102(9) 0.020(7) 0.017(8) 0.028(7) C56 0.081(9) 0.071(9) 0.062(7) 0.007(6) -0.002(6) 0.021(7) C57 0.072(8) 0.087(10) 0.054(7) 0.006(6) -0.003(6) -0.001(7) C58 0.120(11) 0.060(9) 0.185(15) -0.026(8) 0.016(10) -0.012(7) C59 0.112(12) 0.134(13) 0.173(15) -0.042(11) -0.029(11) -0.026(9) C60 0.142(15) 0.155(14) 0.187(16) 0.029(12) -0.025(12) 0.085(12) C61 0.201(18) 0.058(9) 0.235(19) 0.030(10) 0.018(14) 0.071(10) C62 0.100(9) 0.086(8) 0.044(7) -0.005(6) 0.001(6) 0.003(6) C63 0.107(10) 0.108(10) 0.040(7) 0.004(7) 0.004(6) 0.016(8) C64 0.077(8) 0.095(9) 0.064(9) 0.016(7) 0.012(6) 0.004(7) C65 0.072(8) 0.066(7) 0.057(8) 0.018(6) 0.003(6) 0.003(6) C66 0.092(9) 0.105(10) 0.060(8) 0.016(7) 0.023(7) -0.011(8) C67 0.080(8) 0.063(8) 0.122(11) 0.016(8) 0.033(8) -0.007(6) C68 0.066(7) 0.068(8) 0.079(8) 0.025(6) 0.027(6) -0.008(6) C69 0.078(8) 0.070(8) 0.063(7) -0.003(6) 0.007(6) -0.017(6) C70 0.076(8) 0.068(7) 0.054(7) -0.005(6) 0.014(6) -0.007(6) C71 0.075(8) 0.069(8) 0.059(7) -0.002(6) 0.018(6) -0.014(6) C72 0.060(7) 0.066(7) 0.050(7) 0.019(6) 0.018(5) -0.001(6) C73 0.062(7) 0.072(8) 0.042(7) 0.021(6) 0.015(5) 0.015(6) C74 0.159(14) 0.137(12) 0.065(8) -0.006(8) 0.008(8) 0.002(10) C75 0.129(12) 0.146(12) 0.059(7) 0.030(7) 0.022(7) 0.002(9) C76 0.103(9) 0.077(8) 0.101(9) 0.002(7) 0.027(7) -0.043(7) C77 0.085(9) 0.097(9) 0.083(8) -0.001(7) 0.010(7) -0.030(7) C78 0.078(8) 0.066(7) 0.044(6) 0.004(6) 0.010(5) -0.008(5) C79 0.080(8) 0.073(8) 0.039(6) -0.003(5) 0.011(5) -0.015(6) C80 0.089(8) 0.065(7) 0.051(7) 0.008(6) 0.019(6) -0.016(6) C81 0.069(7) 0.072(7) 0.046(6) 0.001(6) 0.016(5) -0.022(6) C82 0.120(10) 0.089(9) 0.060(7) -0.011(7) 0.039(7) -0.044(8) C83 0.123(11) 0.060(7) 0.093(9) -0.004(7) 0.031(8) -0.045(7) C84 0.079(8) 0.060(7) 0.054(7) 0.003(6) 0.022(6) -0.015(6) C85 0.076(8) 0.067(7) 0.070(8) 0.007(6) 0.013(6) -0.018(6) C86 0.068(7) 0.064(7) 0.057(7) -0.009(6) 0.014(5) -0.017(6) C87 0.059(7) 0.070(8) 0.058(7) 0.004(6) 0.021(5) 0.004(6) C88 0.118(10) 0.073(7) 0.050(6) -0.006(6) 0.018(6) -0.014(6) C89 0.136(11) 0.092(8) 0.051(6) 0.006(6) 0.035(7) -0.039(7) C91 0.119(10) 0.086(8) 0.073(8) -0.026(6) 0.018(7) -0.023(7) C92 0.056(8) 0.099(9) 0.068(7) -0.003(6) 0.020(7) 0.004(6) C93 0.049(8) 0.079(8) 0.142(12) -0.024(8) 0.029(8) -0.008(6) C94 0.069(9) 0.066(8) 0.108(10) -0.015(7) -0.013(8) 0.023(6) C95 0.034(7) 0.055(7) 0.089(9) -0.018(6) -0.003(6) 0.013(5) C97 0.091(10) 0.054(7) 0.065(7) 0.000(5) -0.019(8) 0.002(6) C98 0.065(8) 0.059(7) 0.049(6) 0.010(5) -0.001(6) 0.004(5) C99 0.087(9) 0.052(6) 0.053(7) 0.001(5) -0.005(7) 0.001(6) C100 0.074(8) 0.065(7) 0.068(7) 0.011(6) 0.012(6) -0.010(6) C101 0.059(7) 0.067(7) 0.057(7) 0.010(5) 0.010(6) 0.001(5) C102 0.071(10) 0.181(14) 0.158(14) -0.002(11) 0.043(9) 0.021(9) C103 0.069(9) 0.108(10) 0.165(13) -0.042(9) -0.015(8) 0.009(7) C104 0.103(9) 0.085(8) 0.056(7) 0.013(6) 0.008(6) -0.007(6) C105 0.095(9) 0.112(10) 0.084(8) 0.018(7) 0.046(7) 0.006(7) C106 0.054(6) 0.048(6) 0.041(6) 0.005(5) 0.010(5) -0.016(5) C107 0.049(6) 0.060(7) 0.048(6) 0.001(5) 0.010(5) -0.009(5) C108 0.154(13) 0.085(9) 0.100(9) -0.024(7) 0.013(9) -0.063(9) C109 0.046(7) 0.058(6) 0.057(7) -0.013(5) 0.006(6) -0.007(5) C110 0.054(7) 0.049(6) 0.060(7) -0.002(5) -0.002(6) 0.003(5) C111 0.084(10) 0.066(8) 0.071(8) 0.010(6) -0.025(7) 0.008(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N4 2.031(9) . ? Co1 N7 2.042(9) . ? Co1 N14 2.122(8) . ? Co1 N15 2.133(7) . ? Co1 N13 2.135(8) . ? Co1 N16 2.146(7) . ? Fe1 C6 1.894(10) . ? Fe1 C1 1.895(11) . ? Fe1 C5 1.907(11) . ? Fe1 C2 1.923(11) . ? Fe1 C4 1.923(11) . ? Fe1 C3 1.925(12) . ? N1 C1 1.136(11) . ? Co2 N8 2.035(9) . ? Co2 N5 2.042(9) . ? Co2 N20 2.086(8) . ? Co2 N17 2.131(8) . ? Co2 N19 2.135(9) . ? Co2 N18 2.145(8) . ? Fe2 C12 1.877(11) . ? Fe2 C10 1.884(12) . ? Fe2 C8 1.912(11) . ? Fe2 C9 1.912(11) . ? Fe2 C7 1.935(11) . ? Fe2 C11 1.948(13) . ? N2 C2 1.117(10) . ? Co3 N9 2.016(9) . ? Co3 N6 2.087(9) . ? Co3 N24 2.103(8) . ? Co3 N21 2.115(8) . ? Co3 N23 2.136(8) . ? Co3 N22 2.165(8) . ? N3 C3 1.127(11) . ? N4 C4 1.129(10) . ? N5 C5 1.138(10) . ? N6 C6 1.148(10) . ? N7 C7 1.132(10) . ? N8 C8 1.137(10) . ? N9 C9 1.134(10) . ? N10 C10 1.143(11) . ? N11 C11 1.111(13) . ? N12 C12 1.124(11) . ? N13 C101 1.297(11) . ? N13 C110 1.343(11) . ? N14 C92 1.288(11) . ? N14 C109 1.338(11) . ? C14 N24 1.331(11) . ? C14 C15 1.367(14) . ? N15 C87 1.309(11) . ? N15 C106 1.349(10) . ? C15 C16 1.387(15) . ? C15 C26 1.509(15) . ? N16 C78 1.306(11) . ? N16 C107 1.327(10) . ? C16 C17 1.407(15) . ? C16 C27 1.488(14) . ? N17 C71 1.277(11) . ? N17 C72 1.342(11) . ? C17 C25 1.355(13) . ? C17 C18 1.409(16) . ? N18 C62 1.276(11) . ? N18 C73 1.358(12) . ? C18 C19 1.381(16) . ? N19 C55 1.307(12) . ? N19 C56 1.333(13) . ? C19 C20 1.390(15) . ? N20 C46 1.295(11) . ? N20 C57 1.321(12) . ? C20 C21 1.367(15) . ? C20 C24 1.384(13) . ? N21 C39 1.276(10) . ? N21 C40 1.358(11) . ? C21 C22 1.376(15) . ? C21 C28 1.494(14) . ? N22 C30 1.306(11) . ? N22 C41 1.320(11) . ? C22 C23 1.354(14) . ? C22 C29 1.499(15) . ? N23 C23 1.301(11) . ? N23 C24 1.309(11) . ? N24 C25 1.333(11) . ? C24 C25 1.452(13) . ? C30 C31 1.391(14) . ? C31 C32 1.325(14) . ? C31 C42 1.485(14) . ? C32 C33 1.433(14) . ? C32 C43 1.516(14) . ? C33 C41 1.361(13) . ? C33 C34 1.395(15) . ? C34 C35 1.308(14) . ? C35 C36 1.431(14) . ? C36 C37 1.370(13) . ? C36 C40 1.378(13) . ? C37 C38 1.331(13) . ? C37 C44 1.482(14) . ? C38 C39 1.370(13) . ? C38 C45 1.481(12) . ? C40 C41 1.424(12) . ? C46 C47 1.416(15) . ? C47 C48 1.340(16) . ? C47 C58 1.486(15) . ? C48 C49 1.401(15) . ? C48 C59 1.509(16) . ? C49 C50 1.400(17) . ? C49 C57 1.405(15) . ? C50 C51 1.307(18) . ? C51 C52 1.436(18) . ? C52 C56 1.391(15) . ? C52 C53 1.419(17) . ? C53 C54 1.360(18) . ? C53 C60 1.548(18) . ? C54 C55 1.387(16) . ? C54 C61 1.472(17) . ? C56 C57 1.409(14) . ? C62 C63 1.385(14) . ? C63 C64 1.356(15) . ? C63 C74 1.519(15) . ? C64 C65 1.384(14) . ? C64 C75 1.478(14) . ? C65 C66 1.360(14) . ? C65 C73 1.367(12) . ? C66 C67 1.342(14) . ? C67 C68 1.440(14) . ? C68 C69 1.371(13) . ? C68 C72 1.388(13) . ? C69 C70 1.357(13) . ? C69 C76 1.477(13) . ? C70 C71 1.388(13) . ? C70 C77 1.471(13) . ? C72 C73 1.411(13) . ? C78 C79 1.393(12) . ? C79 C80 1.346(12) . ? C79 C88 1.474(12) . ? C80 C81 1.384(12) . ? C80 C89 1.501(12) . ? C81 C107 1.391(12) . ? C81 C82 1.414(13) . ? C82 C83 1.303(13) . ? C83 C84 1.420(13) . ? C84 C106 1.360(12) . ? C84 C85 1.399(13) . ? C85 C86 1.333(12) . ? C85 C108 1.494(13) . ? C86 C87 1.377(12) . ? C86 C91 1.466(12) . ? C92 C93 1.408(15) . ? C93 C94 1.353(16) . ? C93 C102 1.547(16) . ? C94 C95 1.356(15) . ? C94 C103 1.545(15) . ? C95 C109 1.378(12) . ? C95 C111 1.400(14) . ? C97 C111 1.316(14) . ? C97 C98 1.362(14) . ? C98 C99 1.369(13) . ? C98 C110 1.417(12) . ? C99 C100 1.379(14) . ? C99 C104 1.516(13) . ? C100 C101 1.398(13) . ? C100 C105 1.501(14) . ? C106 C107 1.402(12) . ? C109 C110 1.396(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N7 91.7(3) . . ? N4 Co1 N14 167.7(3) . . ? N7 Co1 N14 90.8(3) . . ? N4 Co1 N15 94.9(3) . . ? N7 Co1 N15 166.1(3) . . ? N14 Co1 N15 85.3(3) . . ? N4 Co1 N13 90.5(3) . . ? N7 Co1 N13 98.2(3) . . ? N14 Co1 N13 77.2(3) . . ? N15 Co1 N13 93.9(3) . . ? N4 Co1 N16 97.2(3) . . ? N7 Co1 N16 91.4(3) . . ? N14 Co1 N16 94.8(3) . . ? N15 Co1 N16 75.7(3) . . ? N13 Co1 N16 167.5(3) . . ? C6 Fe1 C1 95.8(4) . . ? C6 Fe1 C5 86.5(4) . . ? C1 Fe1 C5 176.5(4) . . ? C6 Fe1 C2 175.7(4) . . ? C1 Fe1 C2 88.6(4) . . ? C5 Fe1 C2 89.2(4) . . ? C6 Fe1 C4 92.8(4) . . ? C1 Fe1 C4 88.8(4) . . ? C5 Fe1 C4 88.4(4) . . ? C2 Fe1 C4 87.7(4) . . ? C6 Fe1 C3 87.9(4) . . ? C1 Fe1 C3 91.0(4) . . ? C5 Fe1 C3 91.8(4) . . ? C2 Fe1 C3 91.7(4) . . ? C4 Fe1 C3 179.3(4) . . ? N1 C1 Fe1 177.8(10) . . ? N8 Co2 N5 96.1(3) . . ? N8 Co2 N20 93.1(3) . . ? N5 Co2 N20 93.0(3) . . ? N8 Co2 N17 92.9(3) . . ? N5 Co2 N17 91.6(3) . . ? N20 Co2 N17 172.0(3) . . ? N8 Co2 N19 169.0(4) . . ? N5 Co2 N19 89.3(3) . . ? N20 Co2 N19 76.9(4) . . ? N17 Co2 N19 96.6(4) . . ? N8 Co2 N18 93.4(3) . . ? N5 Co2 N18 165.9(3) . . ? N20 Co2 N18 97.0(3) . . ? N17 Co2 N18 77.4(3) . . ? N19 Co2 N18 83.2(3) . . ? C12 Fe2 C10 90.5(4) . . ? C12 Fe2 C8 88.9(4) . . ? C10 Fe2 C8 175.0(4) . . ? C12 Fe2 C9 90.8(4) . . ? C10 Fe2 C9 86.4(4) . . ? C8 Fe2 C9 88.6(4) . . ? C12 Fe2 C7 175.4(4) . . ? C10 Fe2 C7 93.9(4) . . ? C8 Fe2 C7 86.7(4) . . ? C9 Fe2 C7 90.3(4) . . ? C12 Fe2 C11 91.0(5) . . ? C10 Fe2 C11 92.0(5) . . ? C8 Fe2 C11 93.1(4) . . ? C9 Fe2 C11 177.6(4) . . ? C7 Fe2 C11 88.0(4) . . ? N2 C2 Fe1 179.5(11) . . ? N9 Co3 N6 92.3(3) . . ? N9 Co3 N24 96.3(3) . . ? N6 Co3 N24 100.7(3) . . ? N9 Co3 N21 98.7(3) . . ? N6 Co3 N21 94.9(3) . . ? N24 Co3 N21 157.8(3) . . ? N9 Co3 N23 172.5(3) . . ? N6 Co3 N23 88.3(3) . . ? N24 Co3 N23 76.2(3) . . ? N21 Co3 N23 88.7(3) . . ? N9 Co3 N22 93.3(3) . . ? N6 Co3 N22 170.1(3) . . ? N24 Co3 N22 86.8(3) . . ? N21 Co3 N22 76.1(3) . . ? N23 Co3 N22 87.2(3) . . ? N3 C3 Fe1 178.2(10) . . ? C4 N4 Co1 158.5(7) . . ? N4 C4 Fe1 179.4(9) . . ? C5 N5 Co2 164.3(8) . . ? N5 C5 Fe1 173.3(8) . . ? C6 N6 Co3 159.0(8) . . ? N6 C6 Fe1 171.1(8) . . ? C7 N7 Co1 162.3(7) . . ? N7 C7 Fe2 175.0(8) . . ? C8 N8 Co2 162.0(8) . . ? N8 C8 Fe2 173.4(9) . . ? C9 N9 Co3 165.5(8) . . ? N9 C9 Fe2 178.6(9) . . ? N10 C10 Fe2 177.1(10) . . ? N11 C11 Fe2 177.4(13) . . ? N12 C12 Fe2 179.0(11) . . ? C101 N13 C110 119.5(8) . . ? C101 N13 Co1 127.9(7) . . ? C110 N13 Co1 112.5(6) . . ? C92 N14 C109 118.3(9) . . ? C92 N14 Co1 127.6(7) . . ? C109 N14 Co1 114.1(6) . . ? N24 C14 C15 123.2(11) . . ? C87 N15 C106 116.2(8) . . ? C87 N15 Co1 128.3(6) . . ? C106 N15 Co1 115.4(6) . . ? C14 C15 C16 118.4(11) . . ? C14 C15 C26 117.8(12) . . ? C16 C15 C26 123.8(11) . . ? C78 N16 C107 118.9(8) . . ? C78 N16 Co1 126.8(7) . . ? C107 N16 Co1 114.2(6) . . ? C15 C16 C17 118.0(10) . . ? C15 C16 C27 119.7(12) . . ? C17 C16 C27 122.3(12) . . ? C71 N17 C72 119.8(9) . . ? C71 N17 Co2 126.5(7) . . ? C72 N17 Co2 113.7(7) . . ? C25 C17 C16 119.1(11) . . ? C25 C17 C18 117.6(12) . . ? C16 C17 C18 123.3(12) . . ? C62 N18 C73 117.7(9) . . ? C62 N18 Co2 129.1(8) . . ? C73 N18 Co2 113.0(7) . . ? C19 C18 C17 121.6(12) . . ? C55 N19 C56 119.9(10) . . ? C55 N19 Co2 126.7(9) . . ? C56 N19 Co2 113.3(7) . . ? C18 C19 C20 122.0(12) . . ? C46 N20 C57 117.9(9) . . ? C46 N20 Co2 127.0(7) . . ? C57 N20 Co2 115.1(7) . . ? C21 C20 C24 118.7(11) . . ? C21 C20 C19 124.2(12) . . ? C24 C20 C19 117.1(12) . . ? C39 N21 C40 116.9(8) . . ? C39 N21 Co3 128.0(7) . . ? C40 N21 Co3 114.2(6) . . ? C20 C21 C22 117.4(10) . . ? C20 C21 C28 121.9(13) . . ? C22 C21 C28 120.6(13) . . ? C30 N22 C41 117.8(8) . . ? C30 N22 Co3 128.1(7) . . ? C41 N22 Co3 113.8(6) . . ? C23 C22 C21 118.3(11) . . ? C23 C22 C29 120.9(12) . . ? C21 C22 C29 120.8(12) . . ? C23 N23 C24 115.9(9) . . ? C23 N23 Co3 128.0(8) . . ? C24 N23 Co3 116.0(7) . . ? N23 C23 C22 125.8(11) . . ? C14 N24 C25 118.7(9) . . ? C14 N24 Co3 125.6(7) . . ? C25 N24 Co3 115.5(7) . . ? N23 C24 C20 123.8(10) . . ? N23 C24 C25 115.4(9) . . ? C20 C24 C25 120.8(11) . . ? N24 C25 C17 122.4(10) . . ? N24 C25 C24 116.7(9) . . ? C17 C25 C24 120.9(10) . . ? N22 C30 C31 123.7(10) . . ? C32 C31 C30 118.7(10) . . ? C32 C31 C42 124.1(11) . . ? C30 C31 C42 117.2(11) . . ? C31 C32 C33 118.9(10) . . ? C31 C32 C43 119.7(11) . . ? C33 C32 C43 121.3(11) . . ? C41 C33 C34 119.6(10) . . ? C41 C33 C32 117.0(11) . . ? C34 C33 C32 123.3(11) . . ? C35 C34 C33 120.7(11) . . ? C34 C35 C36 123.7(11) . . ? C37 C36 C40 119.3(9) . . ? C37 C36 C35 125.9(11) . . ? C40 C36 C35 114.8(10) . . ? C38 C37 C36 118.4(10) . . ? C38 C37 C44 120.8(10) . . ? C36 C37 C44 120.8(11) . . ? C37 C38 C39 119.1(9) . . ? C37 C38 C45 123.5(10) . . ? C39 C38 C45 117.3(10) . . ? N21 C39 C38 125.0(9) . . ? N21 C40 C36 121.2(9) . . ? N21 C40 C41 116.6(9) . . ? C36 C40 C41 122.1(9) . . ? N22 C41 C33 123.8(9) . . ? N22 C41 C40 117.3(9) . . ? C33 C41 C40 118.9(10) . . ? N20 C46 C47 124.0(11) . . ? C48 C47 C46 118.1(11) . . ? C48 C47 C58 125.7(12) . . ? C46 C47 C58 116.2(12) . . ? C47 C48 C49 119.5(11) . . ? C47 C48 C59 118.2(13) . . ? C49 C48 C59 122.3(13) . . ? C50 C49 C48 123.5(14) . . ? C50 C49 C57 119.4(13) . . ? C48 C49 C57 117.1(12) . . ? C51 C50 C49 120.5(15) . . ? C50 C51 C52 123.7(14) . . ? C56 C52 C53 116.4(13) . . ? C56 C52 C51 116.0(13) . . ? C53 C52 C51 127.5(14) . . ? C54 C53 C52 121.3(13) . . ? C54 C53 C60 121.8(15) . . ? C52 C53 C60 116.8(16) . . ? C53 C54 C55 116.5(13) . . ? C53 C54 C61 123.7(14) . . ? C55 C54 C61 119.8(15) . . ? N19 C55 C54 124.0(13) . . ? N19 C56 C52 121.7(12) . . ? N19 C56 C57 116.9(10) . . ? C52 C56 C57 121.3(13) . . ? N20 C57 C49 123.3(11) . . ? N20 C57 C56 117.6(10) . . ? C49 C57 C56 119.0(12) . . ? N18 C62 C63 123.6(11) . . ? C64 C63 C62 120.2(11) . . ? C64 C63 C74 124.2(11) . . ? C62 C63 C74 115.5(12) . . ? C63 C64 C65 116.5(10) . . ? C63 C64 C75 120.9(12) . . ? C65 C64 C75 122.6(12) . . ? C66 C65 C73 118.5(11) . . ? C66 C65 C64 121.5(11) . . ? C73 C65 C64 120.1(11) . . ? C67 C66 C65 121.4(10) . . ? C66 C67 C68 123.9(11) . . ? C69 C68 C72 121.5(9) . . ? C69 C68 C67 125.6(11) . . ? C72 C68 C67 112.9(10) . . ? C70 C69 C68 116.7(9) . . ? C70 C69 C76 120.5(10) . . ? C68 C69 C76 122.7(10) . . ? C69 C70 C71 119.4(9) . . ? C69 C70 C77 123.2(10) . . ? C71 C70 C77 117.4(9) . . ? N17 C71 C70 123.4(9) . . ? N17 C72 C68 119.2(9) . . ? N17 C72 C73 118.2(9) . . ? C68 C72 C73 122.6(9) . . ? N18 C73 C65 121.8(10) . . ? N18 C73 C72 117.6(9) . . ? C65 C73 C72 120.6(11) . . ? N16 C78 C79 122.4(9) . . ? C80 C79 C78 120.0(9) . . ? C80 C79 C88 124.3(9) . . ? C78 C79 C88 115.7(9) . . ? C79 C80 C81 117.5(8) . . ? C79 C80 C89 121.6(9) . . ? C81 C80 C89 120.9(9) . . ? C80 C81 C107 119.6(9) . . ? C80 C81 C82 123.1(9) . . ? C107 C81 C82 117.3(9) . . ? C83 C82 C81 121.3(10) . . ? C82 C83 C84 123.3(10) . . ? C106 C84 C85 119.1(8) . . ? C106 C84 C83 116.3(9) . . ? C85 C84 C83 124.7(10) . . ? C86 C85 C84 119.2(9) . . ? C86 C85 C108 120.2(10) . . ? C84 C85 C108 120.6(10) . . ? C85 C86 C87 117.6(9) . . ? C85 C86 C91 124.0(10) . . ? C87 C86 C91 118.4(9) . . ? N15 C87 C86 125.7(9) . . ? N14 C92 C93 122.7(11) . . ? C94 C93 C92 118.1(11) . . ? C94 C93 C102 125.7(13) . . ? C92 C93 C102 116.2(13) . . ? C93 C94 C95 120.0(11) . . ? C93 C94 C103 119.8(13) . . ? C95 C94 C103 120.1(13) . . ? C94 C95 C109 118.0(11) . . ? C94 C95 C111 124.2(11) . . ? C109 C95 C111 117.8(10) . . ? C111 C97 C98 123.6(11) . . ? C97 C98 C99 125.1(10) . . ? C97 C98 C110 116.5(10) . . ? C99 C98 C110 118.4(9) . . ? C98 C99 C100 120.7(9) . . ? C98 C99 C104 120.2(10) . . ? C100 C99 C104 119.1(11) . . ? C99 C100 C101 116.4(10) . . ? C99 C100 C105 124.9(10) . . ? C101 C100 C105 118.7(10) . . ? N13 C101 C100 124.4(9) . . ? N15 C106 C84 122.2(8) . . ? N15 C106 C107 115.8(8) . . ? C84 C106 C107 122.0(8) . . ? N16 C107 C81 121.4(8) . . ? N16 C107 C106 118.6(8) . . ? C81 C107 C106 119.9(9) . . ? N14 C109 C95 122.9(9) . . ? N14 C109 C110 117.2(9) . . ? C95 C109 C110 119.9(10) . . ? N13 C110 C109 119.0(9) . . ? N13 C110 C98 120.5(9) . . ? C109 C110 C98 120.6(10) . . ? C97 C111 C95 121.6(10) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.786 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.099 #end============================= data_Na((Co(tmphen)2)3(Fe(CN)6)2)2ClO4.34H2O _audit_creation_method SHELXL-97 _chemical_name_systematic ; Na((Co(tmphen)2)3(Fe(CN)6)2)2ClO4.34H2O ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C107 H164 Cl2 Co3 Fe2 N24 Na O42' _chemical_formula_sum 'C107 H164 Cl2 Co3 Fe2 N24 Na O42' _chemical_formula_weight 2841 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.86(3) _cell_length_b 25.22(3) _cell_length_c 29.69(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.52(6) _cell_angle_gamma 90.00 _cell_volume 13997(37) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14652 _cell_measurement_theta_min 2.302 _cell_measurement_theta_max 24.061 _exptl_crystal_description 'plate' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5680 _exptl_absorpt_coefficient_mu 0.675 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.7121 _exptl_absorpt_correction_T_max 0.9866 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART Apex' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56563 _diffrn_reflns_av_R_equivalents 0.1743 _diffrn_reflns_av_sigmaI/netI 0.1788 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 20.81 _reflns_number_total 14652 _reflns_number_gt 7752 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1723P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0039(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 14652 _refine_ls_number_parameters 1493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1773 _refine_ls_R_factor_gt 0.0960 _refine_ls_wR_factor_ref 0.2996 _refine_ls_wR_factor_gt 0.2443 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 10.617 _refine_ls_shift/su_mean 0.008 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.08195(9) 0.31184(7) 0.34664(6) 0.0284(5) Uani 1 1 d . A -1 Co2 Co -0.17943(9) 0.25766(7) 0.20173(6) 0.0284(5) Uani 1 1 d . A -1 Co3 Co 0.12031(8) 0.13684(7) 0.18837(6) 0.0265(5) Uani 1 1 d . A -1 Fe4 Fe -0.03434(9) 0.14367(7) 0.30550(6) 0.0293(6) Uani 1 1 d . A -1 Fe5 Fe 0.05661(9) 0.32298(7) 0.18234(6) 0.0283(6) Uani 1 1 d . A -1 Cl1B Cl -0.0323(2) -0.07940(18) 0.11806(15) 0.0615(12) Uiso 1 1 d . . . Cl1A Cl 0.1508(2) 0.47298(19) 0.49085(15) 0.0643(12) Uiso 1 1 d . . . Na3 Na -0.1293(5) 0.3570(4) 0.0558(3) 0.044(3) Uiso 0.50 1 d P . -5 Na9 Na -0.1254(6) 0.4167(5) 0.1333(4) 0.058(3) Uiso 0.50 1 d P B -6 O13S O 0.3245(15) 0.2619(13) 0.1450(10) 0.121(10) Uiso 0.50 1 d P . . O14S O 0.2223(17) 0.2635(14) 0.0928(11) 0.139(12) Uiso 0.50 1 d P . . O4B O 0.0160(13) -0.0525(11) 0.0921(9) 0.083(8) Uiso 0.50 1 d P C -4 O41S O 0.4521(6) 0.0599(5) 0.4270(4) 0.075(3) Uiso 1 1 d . . . O37S O 0.0263(15) -0.0422(12) 0.2870(11) 0.116(10) Uiso 0.50 1 d P D -7 O42S O 0.5044(5) 0.1209(4) 0.3619(3) 0.065(3) Uiso 1 1 d . . . O5S O 0.1186(6) 0.4785(5) 0.1196(4) 0.074(3) Uiso 1 1 d . . . O27S O -0.2841(5) 0.1647(5) 0.4007(4) 0.070(3) Uiso 1 1 d . . . O38S O 0.0078(11) -0.0360(9) 0.2483(8) 0.068(6) Uiso 0.50 1 d P E -8 O3S O -0.1296(5) 0.4396(4) -0.0046(4) 0.069(3) Uiso 1 1 d . F -1 O31S O -0.3064(6) 0.0615(5) 0.4206(4) 0.081(4) Uiso 1 1 d . . . O1S O -0.1785(5) 0.5113(4) 0.1617(4) 0.067(3) Uiso 1 1 d . G -1 O25S O -0.4171(6) 0.2143(5) 0.3783(4) 0.077(3) Uiso 1 1 d . . . O45S O 0.1498(6) 0.1257(5) 0.4596(4) 0.075(3) Uiso 1 1 d . . . O44S O 0.2700(6) 0.1957(5) 0.4861(4) 0.074(3) Uiso 1 1 d . . . O2S O -0.0395(5) 0.5404(4) 0.1944(3) 0.061(3) Uiso 1 1 d . . . O40S O 0.2321(6) 0.0353(5) 0.4612(4) 0.079(4) Uiso 1 1 d . . . O51S O -0.0098(6) 0.5378(5) 0.4197(4) 0.091(4) Uiso 1 1 d . . . O39S O 0.2372(7) -0.0075(5) 0.3746(4) 0.099(4) Uiso 1 1 d . . . O8S O 0.2979(9) 0.3904(7) 0.1224(6) 0.127(5) Uiso 1 1 d . H -9 O46S O 0.0260(7) 0.1167(6) 0.5016(4) 0.102(4) Uiso 1 1 d . . . O6S O 0.1123(6) 0.4064(5) 0.0495(4) 0.090(4) Uiso 1 1 d . . . O33S O -0.2359(6) 0.0639(5) 0.2854(4) 0.094(4) Uiso 1 1 d . . . O5B O 0.0221(10) -0.0381(8) 0.1188(7) 0.047(6) Uiso 0.50 1 d P C -3 O25 O 0.1279(6) 0.0233(5) 0.3097(4) 0.088(4) Uiso 1 1 d . . . O49S O -0.4162(9) 0.2693(7) 0.1426(6) 0.145(6) Uiso 1 1 d . . . O50S O -0.1449(8) 0.4746(7) 0.5264(5) 0.131(5) Uiso 1 1 d . . . O7A O -0.3276(14) 0.0207(11) 0.0397(8) 0.089(8) Uiso 0.50 1 d P . . O34S O 0.0094(8) 0.1513(7) 0.5877(5) 0.129(5) Uiso 1 1 d . . . O7B O -0.3977(9) 0.4311(7) 0.4079(6) 0.152(6) Uiso 1 1 d . . . O48S O -0.0518(13) 0.1887(10) 0.4461(8) 0.091(8) Uiso 0.50 1 d P . . O6B O -0.4455(14) 0.4436(13) 0.3444(10) 0.105(9) Uiso 0.50 1 d P . -4 O23S O -0.4295(7) 0.2954(6) 0.3143(5) 0.115(5) Uiso 1 1 d . . . O26S O -0.2732(10) 0.2207(8) 0.4780(7) 0.062(6) Uiso 0.50 1 d P . . O15S O 0.1025(10) 0.2515(8) 0.0311(7) 0.174(7) Uiso 1 1 d . . . O43S O 0.5472(10) 0.2803(8) 0.4466(7) 0.178(8) Uiso 1 1 d . . . O6A O 0.2286(14) 0.4706(12) 0.4878(9) 0.095(9) Uiso 0.50 1 d P I -2 O22S O -0.4530(12) 0.2888(10) 0.2208(8) 0.080(7) Uiso 0.50 1 d P . . O3A O 0.1307(14) 0.4262(11) 0.4674(8) 0.088(8) Uiso 0.50 1 d P I -2 O7S O 0.2474(14) 0.3718(12) 0.0450(9) 0.108(9) Uiso 0.50 1 d P . . O29S O -0.1301(10) 0.2444(8) 0.4966(7) 0.061(6) Uiso 0.50 1 d P . . O10S O 0.3856(11) 0.2949(9) 0.0766(7) 0.198(9) Uiso 1 1 d . . . O24S O -0.5400(13) 0.2198(11) 0.1678(9) 0.099(8) Uiso 0.50 1 d P . . O18S O -0.5307(14) 0.3811(11) 0.1860(9) 0.106(9) Uiso 0.50 1 d P . . O2B O 0.5177(14) 0.3785(11) 0.4063(10) 0.098(8) Uiso 0.50 1 d P . -3 O35S O -0.042(2) 0.0128(17) 0.4763(14) 0.178(15) Uiso 0.50 1 d P . . O17S O -0.557(2) 0.4239(18) 0.1277(15) 0.072(13) Uiso 0.25 1 d P . . O3B O 0.4990(14) 0.3700(11) 0.3667(10) 0.101(9) Uiso 0.50 1 d P . -4 O5A O -0.3818(12) 0.0371(9) 0.0307(7) 0.062(6) Uiso 0.50 1 d P . -2 O32S O -0.1934(10) 0.0426(8) 0.4837(7) 0.060(6) Uiso 0.50 1 d P . . O36S O 0.0394(13) -0.0040(11) 0.4211(9) 0.097(8) Uiso 0.50 1 d P . . O4S O 0.0858(5) 0.4637(4) -0.0296(4) 0.070(3) Uiso 1 1 d . . . O21S O -0.4658(15) 0.4011(13) 0.3340(10) 0.106(9) Uiso 0.50 1 d P . -3 O9S O 0.340(2) 0.3936(15) 0.1572(13) 0.154(13) Uiso 0.50 1 d P J -10 O2A O 0.2036(14) 0.4357(11) 0.4774(9) 0.086(8) Uiso 0.50 1 d P I . O4A O 0.0896(17) 0.4604(14) 0.4589(11) 0.128(11) Uiso 0.50 1 d P I . O16S O -0.084(2) 0.0660(19) 0.4368(15) 0.074(13) Uiso 0.25 1 d P . . N1 N -0.1608(8) 0.1470(5) 0.3584(5) 0.069(4) Uani 1 1 d . A -1 N2 N 0.1648(6) 0.0702(4) 0.2054(3) 0.029(3) Uani 1 1 d . A -1 N3 N -0.0005(5) 0.3566(4) 0.3399(4) 0.030(3) Uani 1 1 d . A -1 N4 N 0.0849(5) 0.2045(5) 0.1741(3) 0.027(3) Uani 1 1 d . A -1 N5 N -0.2613(5) 0.2142(4) 0.2027(4) 0.029(3) Uani 1 1 d . A -1 N6 N 0.0639(5) 0.3105(4) 0.4095(3) 0.023(3) Uani 1 1 d . A -1 N7 N 0.1465(6) 0.3709(5) 0.3605(3) 0.029(3) Uani 1 1 d . A -1 N8 N 0.0248(5) 0.2523(5) 0.3357(3) 0.027(3) Uani 1 1 d . A -1 N10 N 0.0942(5) 0.3165(4) 0.2850(4) 0.029(3) Uani 1 1 d . A -1 N11 N 0.0357(5) 0.1064(4) 0.1525(4) 0.029(3) Uani 1 1 d . A -1 N12 N 0.0798(6) 0.1371(4) 0.2418(4) 0.033(3) Uani 1 1 d . A -1 N13 N -0.2360(5) 0.3163(4) 0.1768(4) 0.031(3) Uani 1 1 d . A -1 N15 N -0.1935(5) 0.2891(4) 0.2584(3) 0.028(3) Uani 1 1 d . A -1 N20 N -0.1765(5) 0.2264(4) 0.1431(3) 0.026(3) Uani 1 1 d . A -1 N21 N 0.1685(6) 0.2705(5) 0.3591(3) 0.036(3) Uani 1 1 d . A -1 N22 N -0.1259(6) 0.2023(4) 0.2299(4) 0.031(3) Uani 1 1 d . A -1 N23 N -0.0965(6) 0.2963(4) 0.1986(3) 0.031(3) Uani 1 1 d . A -1 N25 N 0.0315(6) 0.4418(5) 0.1895(4) 0.045(3) Uani 1 1 d . A -1 N27 N 0.2072(5) 0.1652(4) 0.2205(3) 0.028(3) Uani 1 1 d . A -1 N36 N -0.0854(6) 0.0357(6) 0.2705(4) 0.051(3) Uani 1 1 d . A -1 N37 N 0.1591(6) 0.1333(4) 0.1311(3) 0.028(3) Uani 1 1 d . A -1 N41 N 0.0155(7) 0.3302(5) 0.0791(5) 0.060(4) Uani 1 1 d . A -1 N84 N 0.2116(8) 0.3392(6) 0.1633(4) 0.064(4) Uani 1 1 d . A -1 N108 N 0.0662(8) 0.0916(6) 0.3823(4) 0.073(5) Uani 1 1 d . A -1 C1 C -0.3067(7) 0.3891(6) 0.1990(5) 0.037(4) Uani 1 1 d . A -1 C9 C 0.0760(6) 0.2835(5) 0.4862(4) 0.031(3) Uani 1 1 d . A -1 C14 C 0.2904(8) 0.2307(7) 0.2517(5) 0.048(4) Uani 1 1 d . A -1 C16 C -0.2803(7) 0.1873(5) 0.1636(5) 0.034(4) Uani 1 1 d . A -1 C17 C -0.0341(7) 0.3809(6) 0.3028(5) 0.035(4) Uani 1 1 d . A -1 H17 H -0.0202 0.3717 0.2742 0.042 Uiso 1 1 calc R A -1 C18 C -0.3569(8) 0.1685(6) 0.2329(5) 0.045(4) Uani 1 1 d . A -1 C19 C 0.0410(7) 0.3965(6) 0.1868(5) 0.035(4) Uani 1 1 d . A -1 C24 C -0.1081(6) 0.4328(5) 0.3444(5) 0.035(4) Uani 1 1 d . A -1 C26 C -0.0003(7) 0.2117(6) 0.3252(4) 0.028(3) Uani 1 1 d . A -1 C28 C -0.2675(7) 0.3555(5) 0.2897(5) 0.034(4) Uani 1 1 d . A -1 C29 C -0.0925(7) 0.1776(5) 0.2580(5) 0.028(3) Uani 1 1 d . A -1 C30 C 0.0945(7) 0.2814(6) 0.4430(5) 0.033(4) Uani 1 1 d . A -1 H30 H 0.1313 0.2577 0.4371 0.040 Uiso 1 1 calc R A -1 C31 C -0.0402(9) 0.3085(5) 0.1922(4) 0.033(4) Uani 1 1 d . A -1 C32 C -0.0090(8) 0.0821(6) 0.0777(5) 0.048(4) Uani 1 1 d . A -1 C33 C 0.1362(8) 0.0219(6) 0.1995(4) 0.041(4) Uani 1 1 d . A -1 H33 H 0.0887 0.0177 0.1849 0.050 Uiso 1 1 calc R A -1 C34 C 0.1271(9) 0.1090(5) 0.0534(5) 0.040(4) Uani 1 1 d . A -1 C35 C 0.2561(7) 0.1276(6) 0.2354(4) 0.030(3) Uani 1 1 d . A -1 C38 C -0.0846(7) 0.0751(5) 0.1355(6) 0.040(4) Uani 1 1 d . A -1 C39 C 0.2745(7) 0.0326(6) 0.2406(4) 0.030(3) Uani 1 1 d . A -1 C40 C -0.3394(7) 0.1518(6) 0.1562(5) 0.041(4) Uani 1 1 d . A -1 C42 C 0.0123(7) 0.3434(5) 0.4168(5) 0.032(4) Uani 1 1 d . A -1 C43 C 0.2478(8) -0.0188(6) 0.2344(5) 0.040(4) Uani 1 1 d . A -1 C44 C 0.0384(7) 0.1398(5) 0.2675(5) 0.027(3) Uani 1 1 d . A -1 C45 C -0.3652(9) 0.4531(7) 0.1414(6) 0.000(5) Uiso 0.50 1 d P A -1 H45A H -0.3363 0.4786 0.1269 0.000 Uiso 1 1 calc R A -1 H45B H -0.3806 0.4691 0.1686 0.000 Uiso 1 1 calc R A -1 H45C H -0.4072 0.4432 0.1201 0.000 Uiso 1 1 calc R A -1 C46 C -0.1678(7) 0.2759(5) 0.3005(5) 0.031(3) Uani 1 1 d . A -1 H46 H -0.1311 0.2499 0.3047 0.037 Uiso 1 1 calc R A -1 C47 C -0.0085(6) 0.3505(5) 0.4604(5) 0.031(3) Uani 1 1 d . A -1 C48 C 0.2454(8) 0.1407(6) 0.0788(6) 0.044(4) Uani 1 1 d . A -1 C49 C 0.2234(8) 0.1463(5) 0.1215(5) 0.038(4) Uani 1 1 d . A -1 H49 H 0.2567 0.1605 0.1452 0.046 Uiso 1 1 calc R A -1 C50 C 0.2269(8) 0.3022(7) 0.3750(4) 0.043(4) Uani 1 1 d . A -1 C52 C -0.2425(6) 0.3299(6) 0.2535(5) 0.033(4) Uani 1 1 d . A -1 C53 C 0.3375(8) 0.3689(8) 0.4026(5) 0.055(5) Uani 1 1 d . A -1 H53 H 0.3763 0.3917 0.4129 0.066 Uiso 1 1 calc R A -1 C54 C -0.2334(7) 0.1954(5) 0.1301(5) 0.037(4) Uani 1 1 d . A -1 C55 C -0.4412(8) 0.1057(7) 0.1864(6) 0.076(6) Uani 1 1 d . A -1 H55A H -0.4505 0.0927 0.2162 0.114 Uiso 1 1 calc R A -1 H55B H -0.4305 0.0757 0.1675 0.114 Uiso 1 1 calc R A -1 H55C H -0.4835 0.1245 0.1717 0.114 Uiso 1 1 calc R A -1 C56 C 0.0247(7) 0.3191(6) 0.4957(4) 0.036(4) Uani 1 1 d . A -1 C58 C 0.1545(9) 0.3343(6) 0.1710(4) 0.042(4) Uani 1 1 d . A -1 C59 C 0.1832(9) 0.4620(6) 0.3706(5) 0.044(4) Uani 1 1 d . A -1 C60 C -0.1913(6) 0.2979(5) 0.3393(4) 0.026(3) Uani 1 1 d . A -1 C61 C -0.2013(8) 0.1832(6) 0.0556(5) 0.043(4) Uani 1 1 d . A -1 C62 C -0.0645(7) 0.0767(6) 0.2848(5) 0.033(4) Uani 1 1 d . A -1 C63 C -0.0759(7) 0.4063(6) 0.3835(5) 0.040(4) Uani 1 1 d . A -1 C64 C 0.1312(8) 0.4228(6) 0.3582(4) 0.040(4) Uani 1 1 d . A -1 H64 H 0.0836 0.4335 0.3478 0.048 Uiso 1 1 calc R A -1 C65 C -0.0226(6) 0.3705(5) 0.3791(5) 0.026(3) Uani 1 1 d . A -1 C66 C 0.0718(7) 0.2487(6) 0.1764(4) 0.029(3) Uani 1 1 d . A -1 C67 C -0.0874(7) 0.4184(5) 0.3035(5) 0.034(4) Uani 1 1 d . A -1 C68 C -0.3777(7) 0.1434(6) 0.1925(6) 0.046(4) Uani 1 1 d . A -1 C69 C -0.0636(7) 0.3881(6) 0.4639(5) 0.037(4) Uani 1 1 d . A -1 H69 H -0.0793 0.3936 0.4926 0.044 Uiso 1 1 calc R A -1 C70 C 0.0831(7) 0.3185(5) 0.2460(5) 0.029(3) Uani 1 1 d . A -1 C71 C 0.3223(7) 0.1381(5) 0.2556(5) 0.034(4) Uani 1 1 d . A -1 C72 C -0.2929(7) 0.3754(6) 0.1211(5) 0.043(4) Uani 1 1 d . A -1 C73 C 0.0430(11) 0.0999(8) 0.1098(7) 0.000(5) Uiso 0.50 1 d P A -1 C74 C -0.1582(7) 0.2766(6) 0.3843(5) 0.049(4) Uani 1 1 d . A -1 H74A H -0.1476 0.3059 0.4057 0.073 Uiso 1 1 calc R A -1 H74B H -0.1138 0.2578 0.3805 0.073 Uiso 1 1 calc R A -1 H74C H -0.1915 0.2519 0.3960 0.073 Uiso 1 1 calc R A -1 C75 C -0.3221(7) 0.4054(6) 0.1545(6) 0.047(4) Uani 1 1 d . A -1 C76 C 0.1090(8) 0.1139(5) 0.0977(5) 0.039(4) Uani 1 1 d . A -1 C77 C -0.2476(8) 0.1722(6) 0.0874(5) 0.044(4) Uani 1 1 d . A -1 C78 C 0.0008(7) 0.3235(6) 0.5434(4) 0.042(4) Uani 1 1 d . A -1 H78A H -0.0477 0.3092 0.5426 0.063 Uiso 1 1 calc R A -1 H78B H 0.0013 0.3608 0.5527 0.063 Uiso 1 1 calc R A -1 H78C H 0.0337 0.3032 0.5653 0.063 Uiso 1 1 calc R A -1 C79 C 0.2134(8) 0.3568(6) 0.3750(4) 0.033(4) Uani 1 1 d . A -1 C80 C -0.0269(7) 0.0948(5) 0.1662(5) 0.033(4) Uani 1 1 d . A -1 H80 H -0.0329 0.1000 0.1971 0.040 Uiso 1 1 calc R A -1 C81 C 0.2333(7) 0.0756(6) 0.2272(4) 0.035(4) Uani 1 1 d . A -1 C82 C -0.3009(7) 0.2037(6) 0.2353(5) 0.039(4) Uani 1 1 d . A -1 H82 H -0.2894 0.2224 0.2631 0.047 Uiso 1 1 calc R A -1 C83 C 0.2516(8) 0.4462(7) 0.3873(5) 0.045(4) Uani 1 1 d . A -1 C85 C -0.1122(8) 0.1457(6) 0.3383(5) 0.042(4) Uani 1 1 d . A -1 C86 C 0.1572(8) 0.5175(6) 0.3661(5) 0.055(4) Uani 1 1 d . A -1 H86A H 0.1560 0.5326 0.3964 0.083 Uiso 1 1 calc R A -1 H86B H 0.1090 0.5180 0.3492 0.083 Uiso 1 1 calc R A -1 H86C H 0.1895 0.5384 0.3498 0.083 Uiso 1 1 calc R A -1 C87 C -0.3154(7) 0.3985(6) 0.2795(5) 0.049(4) Uani 1 1 d . A -1 H87 H -0.3356 0.4155 0.3034 0.058 Uiso 1 1 calc R A -1 C88 C -0.2432(7) 0.3368(6) 0.3340(5) 0.039(4) Uani 1 1 d . A -1 C89 C 0.1120(8) 0.2441(6) 0.5221(5) 0.053(4) Uani 1 1 d . A -1 H89A H 0.1339 0.2637 0.5489 0.079 Uiso 1 1 calc R A -1 H89B H 0.1491 0.2240 0.5092 0.079 Uiso 1 1 calc R A -1 H89C H 0.0761 0.2195 0.5310 0.079 Uiso 1 1 calc R A -1 C90 C 0.0266(9) 0.1116(6) 0.3545(6) 0.047(4) Uani 1 1 d . A -1 C91 C -0.2728(7) 0.3597(7) 0.3745(4) 0.054(5) Uani 1 1 d . A -1 H91A H -0.2930 0.3311 0.3912 0.082 Uiso 1 1 calc R A -1 H91B H -0.3104 0.3854 0.3642 0.082 Uiso 1 1 calc R A -1 H91C H -0.2344 0.3774 0.3944 0.082 Uiso 1 1 calc R A -1 C92 C -0.3329(7) 0.4158(6) 0.2363(6) 0.052(4) Uani 1 1 d . A -1 H92 H -0.3629 0.4460 0.2305 0.063 Uiso 1 1 calc R A -1 C93 C 0.3023(7) 0.2240(7) 0.3855(5) 0.040(4) Uani 1 1 d . A -1 C94 C 0.2899(8) -0.0679(6) 0.2489(5) 0.054(4) Uani 1 1 d . A -1 H94A H 0.2814 -0.0779 0.2796 0.080 Uiso 1 1 calc R A -1 H94B H 0.3410 -0.0609 0.2487 0.080 Uiso 1 1 calc R A -1 H94C H 0.2748 -0.0969 0.2278 0.080 Uiso 1 1 calc R A -1 C95 C 0.3425(7) 0.1931(6) 0.2637(4) 0.037(4) Uani 1 1 d . A -1 C96 C -0.1637(7) 0.4757(6) 0.3461(5) 0.048(4) Uani 1 1 d . A -1 H96A H -0.2077 0.4657 0.3267 0.071 Uiso 1 1 calc R A -1 H96B H -0.1456 0.5092 0.3353 0.071 Uiso 1 1 calc R A -1 H96C H -0.1738 0.4800 0.3775 0.071 Uiso 1 1 calc R A -1 C97 C 0.1780(8) -0.0243(5) 0.2155(5) 0.041(4) Uani 1 1 d . A -1 C98 C 0.1778(8) 0.2185(6) 0.3555(4) 0.041(4) Uani 1 1 d . A -1 H98 H 0.1389 0.1967 0.3435 0.049 Uiso 1 1 calc R A -1 C99 C -0.1306(8) 0.2318(5) 0.1135(5) 0.040(4) Uani 1 1 d . A -1 H99 H -0.0882 0.2516 0.1227 0.048 Uiso 1 1 calc R A -1 C100 C 0.3687(8) 0.0948(7) 0.2682(5) 0.059(5) Uani 1 1 d . A -1 H100 H 0.4166 0.1015 0.2811 0.071 Uiso 1 1 calc R A -1 C101 C -0.3029(8) 0.3909(6) 0.0715(5) 0.057(5) Uani 1 1 d . A -1 H10A H -0.3537 0.3971 0.0614 0.086 Uiso 1 1 calc R A -1 H10B H -0.2856 0.3622 0.0535 0.086 Uiso 1 1 calc R A -1 H10C H -0.2758 0.4233 0.0675 0.086 Uiso 1 1 calc R A -1 C102 C 0.0289(7) 0.3281(5) 0.1185(5) 0.035(4) Uani 1 1 d . A -1 C104 C -0.0759(8) 0.0690(6) 0.0910(5) 0.047(4) Uani 1 1 d . A -1 C105 C 0.2500(8) 0.1365(7) 0.3661(6) 0.070(5) Uani 1 1 d . A -1 H10D H 0.2870 0.1268 0.3473 0.106 Uiso 1 1 calc R A -1 H10E H 0.2037 0.1225 0.3523 0.106 Uiso 1 1 calc R A -1 H10F H 0.2620 0.1214 0.3966 0.106 Uiso 1 1 calc R A -1 C106 C -0.1395(9) 0.2108(6) 0.0703(5) 0.047(4) Uani 1 1 d . A -1 C107 C 0.3484(8) 0.3171(8) 0.4018(5) 0.051(4) Uani 1 1 d . A -1 H107 H 0.3953 0.3045 0.4116 0.062 Uiso 1 1 calc R A -1 C109 C -0.3497(8) 0.1272(6) 0.1135(5) 0.049(4) Uani 1 1 d . A -1 H109 H -0.3872 0.1020 0.1074 0.059 Uiso 1 1 calc R A -1 C110 C -0.2642(7) 0.3455(6) 0.2085(4) 0.030(3) Uani 1 1 d . A -1 C111 C 0.0092(10) 0.0757(6) 0.0322(5) 0.057(5) Uani 1 1 d . A -1 H111 H -0.0256 0.0612 0.0095 0.068 Uiso 1 1 calc R A -1 C112 C -0.0938(7) 0.4159(6) 0.4286(5) 0.043(4) Uani 1 1 d . A -1 H112 H -0.1278 0.4426 0.4331 0.052 Uiso 1 1 calc R A -1 C113 C 0.2949(7) 0.2794(7) 0.3873(4) 0.040(4) Uani 1 1 d . A -1 C114 C 0.2251(7) 0.2153(6) 0.2292(4) 0.030(3) Uani 1 1 d . A -1 H114 H 0.1910 0.2420 0.2194 0.036 Uiso 1 1 calc R A -1 C115 C 0.3076(9) 0.4856(7) 0.4049(6) 0.080(6) Uani 1 1 d . A -1 H11A H 0.2974 0.5196 0.3896 0.120 Uiso 1 1 calc R A -1 H11B H 0.3546 0.4728 0.3991 0.120 Uiso 1 1 calc R A -1 H11C H 0.3075 0.4901 0.4377 0.120 Uiso 1 1 calc R A -1 C116 C 0.3455(8) 0.0434(7) 0.2620(5) 0.049(4) Uani 1 1 d . A -1 H116 H 0.3767 0.0149 0.2719 0.059 Uiso 1 1 calc R A -1 C118 C -0.1522(7) 0.0625(7) 0.1570(6) 0.064(5) Uani 1 1 d . A -1 H11D H -0.1942 0.0761 0.1375 0.096 Uiso 1 1 calc R A -1 H11E H -0.1491 0.0793 0.1870 0.096 Uiso 1 1 calc R A -1 H11F H -0.1566 0.0240 0.1603 0.096 Uiso 1 1 calc R A -1 C119 C -0.3077(9) 0.1383(6) 0.0797(5) 0.058(5) Uani 1 1 d . A -1 H119 H -0.3196 0.1226 0.0505 0.070 Uiso 1 1 calc R A -1 C120 C 0.4164(7) 0.2082(7) 0.2855(6) 0.066(5) Uani 1 1 d . A -1 H12A H 0.4454 0.2187 0.2619 0.099 Uiso 1 1 calc R A -1 H12B H 0.4387 0.1778 0.3024 0.099 Uiso 1 1 calc R A -1 H12C H 0.4131 0.2380 0.3064 0.099 Uiso 1 1 calc R A -1 C121 C 0.3044(7) 0.2885(6) 0.2609(5) 0.050(4) Uani 1 1 d . A -1 H12D H 0.2626 0.3092 0.2482 0.075 Uiso 1 1 calc R A -1 H12E H 0.3461 0.2997 0.2467 0.075 Uiso 1 1 calc R A -1 H12F H 0.3138 0.2944 0.2938 0.075 Uiso 1 1 calc R A -1 C122 C 0.1981(10) 0.1224(7) 0.0442(5) 0.057(5) Uani 1 1 d . A -1 C125 C -0.1213(7) 0.4420(6) 0.2589(5) 0.047(4) Uani 1 1 d . A -1 H12G H -0.1109 0.4193 0.2338 0.070 Uiso 1 1 calc R A -1 H12H H -0.1017 0.4775 0.2553 0.070 Uiso 1 1 calc R A -1 H12I H -0.1732 0.4444 0.2589 0.070 Uiso 1 1 calc R A -1 C126 C 0.2667(8) 0.3918(7) 0.3881(5) 0.044(4) Uani 1 1 d . A -1 C128 C 0.3216(8) 0.1531(7) 0.0726(5) 0.067(5) Uani 1 1 d . A -1 H12J H 0.3444 0.1212 0.0621 0.100 Uiso 1 1 calc R A -1 H12K H 0.3477 0.1647 0.1016 0.100 Uiso 1 1 calc R A -1 H12L H 0.3223 0.1813 0.0500 0.100 Uiso 1 1 calc R A -1 C130 C 0.0720(9) 0.0890(6) 0.0207(5) 0.050(4) Uani 1 1 d . A -1 H130 H 0.0805 0.0852 -0.0100 0.060 Uiso 1 1 calc R A -1 C131 C -0.1358(9) 0.0458(7) 0.0586(6) 0.077(6) Uani 1 1 d . A -1 H13A H -0.1796 0.0663 0.0601 0.115 Uiso 1 1 calc R A -1 H13B H -0.1437 0.0088 0.0670 0.115 Uiso 1 1 calc R A -1 H13C H -0.1232 0.0471 0.0276 0.115 Uiso 1 1 calc R A -1 C132 C 0.2457(9) 0.1957(6) 0.3694(5) 0.046(4) Uani 1 1 d . A -1 C133 C 0.2186(9) 0.1161(7) -0.0025(5) 0.066(5) Uani 1 1 d . A -1 H13D H 0.2273 0.1511 -0.0150 0.099 Uiso 1 1 calc R A -1 H13E H 0.1797 0.0984 -0.0220 0.099 Uiso 1 1 calc R A -1 H13F H 0.2621 0.0946 -0.0010 0.099 Uiso 1 1 calc R A -1 C134 C -0.3936(8) 0.1593(7) 0.2739(5) 0.065(5) Uani 1 1 d . A -1 H13G H -0.4453 0.1640 0.2658 0.098 Uiso 1 1 calc R A -1 H13H H -0.3758 0.1847 0.2977 0.098 Uiso 1 1 calc R A -1 H13I H -0.3838 0.1231 0.2851 0.098 Uiso 1 1 calc R A -1 C135 C -0.2165(10) 0.1652(7) 0.0073(5) 0.077(6) Uani 1 1 d . A -1 H13J H -0.2327 0.1955 -0.0121 0.115 Uiso 1 1 calc R A -1 H13K H -0.2539 0.1380 0.0047 0.115 Uiso 1 1 calc R A -1 H13L H -0.1729 0.1504 -0.0024 0.115 Uiso 1 1 calc R A -1 C136 C 0.3709(8) 0.1995(7) 0.4021(5) 0.066(5) Uani 1 1 d . A -1 H13M H 0.3888 0.1803 0.3771 0.098 Uiso 1 1 calc R A -1 H13N H 0.3646 0.1746 0.4266 0.098 Uiso 1 1 calc R A -1 H13O H 0.4053 0.2270 0.4135 0.098 Uiso 1 1 calc R A -1 C138 C 0.1399(7) -0.0783(5) 0.2087(5) 0.050(4) Uani 1 1 d . A -1 H13P H 0.1685 -0.1023 0.1923 0.075 Uiso 1 1 calc R A -1 H13Q H 0.0927 -0.0733 0.1910 0.075 Uiso 1 1 calc R A -1 H13R H 0.1342 -0.0936 0.2383 0.075 Uiso 1 1 calc R A -1 C140 C -0.2518(7) 0.3314(6) 0.1343(5) 0.041(4) Uani 1 1 d . A -1 H140 H -0.2340 0.3108 0.1115 0.049 Uiso 1 1 calc R A -1 C142 C -0.0806(9) 0.2209(7) 0.0401(5) 0.066(5) Uani 1 1 d . A -1 H14A H -0.1024 0.2329 0.0100 0.099 Uiso 1 1 calc R A -1 H14B H -0.0540 0.1880 0.0369 0.099 Uiso 1 1 calc R A -1 H14C H -0.0479 0.2483 0.0540 0.099 Uiso 1 1 calc R A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0300(11) 0.0267(12) 0.0280(11) -0.0017(9) 0.0025(8) -0.0005(8) Co2 0.0272(11) 0.0263(12) 0.0313(11) -0.0018(9) 0.0028(8) 0.0006(8) Co3 0.0275(11) 0.0217(12) 0.0305(11) 0.0000(8) 0.0049(8) 0.0028(8) Fe4 0.0314(12) 0.0251(13) 0.0315(12) 0.0014(9) 0.0049(9) -0.0018(9) Fe5 0.0290(12) 0.0220(12) 0.0333(12) 0.0016(9) 0.0016(9) -0.0003(9) N1 0.091(11) 0.046(10) 0.078(11) -0.012(8) 0.042(9) -0.017(8) N2 0.035(8) 0.017(7) 0.037(7) 0.000(5) 0.016(6) 0.002(6) N3 0.032(7) 0.031(7) 0.023(7) 0.005(6) -0.004(6) -0.003(5) N4 0.023(6) 0.016(7) 0.039(7) 0.003(6) -0.005(5) -0.010(5) N5 0.033(7) 0.028(7) 0.027(7) 0.008(6) 0.005(6) 0.002(5) N6 0.028(7) 0.028(7) 0.013(6) 0.002(6) 0.003(5) 0.003(6) N7 0.036(8) 0.030(9) 0.022(6) 0.001(5) 0.011(5) -0.008(6) N8 0.028(7) 0.024(8) 0.028(7) -0.001(6) 0.005(5) 0.006(6) N10 0.028(7) 0.025(7) 0.033(8) 0.005(6) 0.006(6) -0.001(5) N11 0.019(6) 0.012(6) 0.055(8) 0.001(5) 0.007(6) -0.003(5) N12 0.030(7) 0.032(8) 0.039(7) -0.008(6) 0.009(6) 0.006(6) N13 0.020(6) 0.041(8) 0.032(7) 0.002(7) 0.001(6) 0.004(5) N15 0.033(7) 0.028(7) 0.021(7) 0.000(5) 0.000(5) 0.007(6) N20 0.026(6) 0.035(8) 0.019(6) -0.006(5) 0.005(5) -0.004(6) N21 0.039(8) 0.036(9) 0.034(7) 0.002(6) 0.012(6) -0.001(7) N22 0.026(7) 0.015(7) 0.052(8) 0.005(6) 0.003(6) 0.001(5) N23 0.030(7) 0.029(8) 0.036(7) 0.003(6) 0.011(6) 0.006(6) N25 0.044(8) 0.027(9) 0.062(9) 0.008(7) 0.000(6) 0.005(6) N27 0.022(7) 0.022(8) 0.039(7) -0.003(6) 0.004(5) 0.004(6) N36 0.064(9) 0.049(10) 0.045(8) 0.005(7) 0.021(7) -0.008(8) N37 0.036(7) 0.022(7) 0.026(7) 0.011(5) 0.008(6) 0.017(6) N41 0.082(10) 0.053(10) 0.039(9) 0.020(7) -0.009(8) 0.001(7) N84 0.056(10) 0.079(11) 0.059(10) -0.015(8) 0.020(8) -0.024(8) N108 0.099(12) 0.077(12) 0.036(9) 0.018(8) -0.013(8) 0.023(9) C1 0.039(9) 0.041(11) 0.029(10) -0.008(8) -0.002(7) 0.009(8) C9 0.028(8) 0.027(9) 0.035(9) -0.005(7) -0.003(7) 0.007(7) C14 0.034(10) 0.058(13) 0.050(10) 0.006(9) -0.004(8) -0.001(9) C16 0.043(10) 0.028(9) 0.026(9) -0.003(7) -0.008(8) 0.006(8) C17 0.034(9) 0.040(10) 0.032(10) -0.016(8) 0.010(7) -0.015(8) C18 0.042(10) 0.031(10) 0.063(12) -0.004(9) 0.008(9) -0.015(8) C19 0.029(9) 0.030(11) 0.045(10) 0.007(8) 0.005(7) 0.001(7) C24 0.023(8) 0.027(9) 0.056(11) -0.008(8) 0.012(8) 0.004(7) C26 0.029(8) 0.023(9) 0.032(9) 0.001(7) 0.007(6) 0.010(7) C28 0.028(8) 0.034(10) 0.039(10) -0.009(8) 0.003(7) 0.005(7) C29 0.030(9) 0.016(9) 0.042(9) -0.013(7) 0.023(7) -0.003(7) C30 0.030(8) 0.037(10) 0.035(10) -0.010(8) 0.017(7) 0.003(7) C31 0.054(11) 0.013(8) 0.029(9) 0.002(6) 0.002(8) 0.003(7) C32 0.058(11) 0.030(10) 0.059(12) 0.004(8) 0.021(9) 0.015(8) C33 0.047(10) 0.043(12) 0.032(9) 0.001(8) 0.002(7) 0.013(9) C34 0.064(12) 0.023(9) 0.031(10) -0.004(7) -0.004(9) 0.015(8) C35 0.013(9) 0.039(11) 0.037(9) -0.002(7) 0.007(7) 0.003(8) C38 0.023(9) 0.017(9) 0.073(13) -0.001(8) -0.017(8) -0.008(7) C39 0.027(9) 0.025(10) 0.038(9) -0.001(7) 0.001(7) 0.004(8) C40 0.030(9) 0.035(10) 0.055(11) -0.010(8) -0.005(8) -0.003(8) C42 0.028(8) 0.018(9) 0.053(11) -0.023(8) 0.011(8) -0.005(7) C43 0.035(10) 0.045(12) 0.038(9) 0.007(8) 0.005(7) 0.016(8) C44 0.023(8) 0.016(8) 0.037(9) -0.005(7) -0.014(7) 0.002(6) C46 0.036(8) 0.022(9) 0.035(10) -0.013(7) 0.009(7) 0.000(7) C47 0.016(8) 0.032(9) 0.046(10) 0.009(8) 0.005(7) 0.000(7) C48 0.064(11) 0.029(10) 0.044(11) -0.001(8) 0.031(10) -0.001(8) C49 0.044(10) 0.019(9) 0.054(11) 0.006(7) 0.014(8) 0.002(7) C50 0.037(10) 0.066(14) 0.027(9) 0.008(8) 0.010(7) -0.020(10) C52 0.018(8) 0.039(10) 0.039(10) -0.011(8) -0.002(7) -0.007(7) C53 0.041(12) 0.088(16) 0.038(10) -0.010(10) 0.010(8) -0.026(11) C54 0.039(10) 0.026(9) 0.046(11) 0.003(8) 0.004(8) -0.004(8) C55 0.055(11) 0.080(15) 0.097(15) -0.024(11) 0.022(10) -0.024(10) C56 0.037(9) 0.038(10) 0.035(9) -0.012(8) 0.009(7) -0.011(8) C58 0.068(12) 0.039(10) 0.019(8) 0.000(7) 0.005(8) 0.003(9) C59 0.059(12) 0.033(11) 0.041(10) -0.002(8) 0.013(8) -0.024(9) C60 0.026(8) 0.027(9) 0.025(9) 0.002(7) 0.000(6) -0.013(7) C61 0.064(11) 0.031(10) 0.036(10) 0.006(8) 0.013(9) 0.004(8) C62 0.027(8) 0.033(10) 0.039(9) 0.002(8) 0.002(7) -0.010(7) C63 0.040(9) 0.038(10) 0.040(11) 0.001(8) 0.002(8) -0.006(8) C64 0.049(10) 0.044(12) 0.029(9) 0.002(8) 0.013(7) 0.000(9) C65 0.019(8) 0.027(9) 0.026(9) 0.007(7) -0.015(7) -0.001(7) C66 0.033(9) 0.039(11) 0.013(7) 0.004(7) -0.004(6) -0.011(8) C67 0.032(9) 0.022(9) 0.049(10) -0.004(8) 0.010(8) -0.001(7) C68 0.025(9) 0.036(10) 0.076(12) -0.002(9) 0.005(9) -0.019(7) C69 0.037(9) 0.049(11) 0.026(9) -0.010(8) 0.012(7) -0.002(8) C70 0.034(9) 0.014(8) 0.039(10) 0.008(7) 0.001(7) 0.001(6) C71 0.022(9) 0.023(10) 0.058(10) 0.009(8) 0.010(7) 0.005(8) C72 0.045(9) 0.044(11) 0.037(10) 0.008(8) -0.008(7) 0.017(8) C74 0.056(10) 0.053(11) 0.038(10) 0.001(8) 0.003(8) -0.004(8) C75 0.030(9) 0.039(10) 0.064(12) -0.011(9) -0.015(8) 0.004(7) C76 0.074(11) 0.020(9) 0.018(9) -0.002(7) -0.011(8) 0.023(8) C77 0.068(11) 0.026(10) 0.037(10) -0.005(8) 0.001(9) 0.004(9) C78 0.033(9) 0.045(10) 0.044(10) 0.000(8) -0.006(7) 0.011(7) C79 0.032(10) 0.035(11) 0.031(9) 0.006(7) 0.007(7) -0.015(9) C80 0.043(10) 0.010(8) 0.046(9) 0.001(7) 0.001(8) 0.002(7) C81 0.031(10) 0.042(12) 0.034(9) -0.001(8) 0.010(7) 0.006(9) C82 0.042(9) 0.036(10) 0.039(10) -0.011(8) 0.003(8) -0.003(8) C83 0.047(11) 0.055(13) 0.037(10) -0.013(8) 0.023(8) -0.027(9) C85 0.047(10) 0.050(11) 0.033(9) -0.006(8) 0.018(8) -0.008(8) C86 0.080(12) 0.034(11) 0.056(11) -0.003(8) 0.022(9) -0.025(9) C87 0.034(9) 0.060(12) 0.052(12) -0.011(9) 0.004(8) 0.021(8) C88 0.042(9) 0.031(10) 0.046(11) -0.009(8) 0.008(8) 0.000(8) C89 0.064(11) 0.051(11) 0.042(10) -0.008(8) 0.008(8) -0.001(9) C90 0.065(11) 0.026(10) 0.055(11) 0.004(8) 0.023(9) 0.000(8) C91 0.053(10) 0.084(13) 0.030(9) -0.010(9) 0.018(8) 0.020(9) C92 0.049(10) 0.044(11) 0.060(12) -0.005(9) -0.010(9) 0.030(8) C93 0.021(9) 0.058(13) 0.040(9) 0.004(8) 0.003(7) 0.012(9) C94 0.066(11) 0.034(10) 0.057(11) 0.009(8) -0.005(8) 0.021(8) C95 0.031(9) 0.048(11) 0.030(9) 0.007(8) 0.001(7) -0.016(8) C96 0.039(9) 0.060(12) 0.042(10) 0.000(8) -0.001(7) -0.004(8) C97 0.064(12) 0.027(10) 0.035(9) 0.001(7) 0.023(8) 0.010(9) C98 0.051(10) 0.039(11) 0.035(9) 0.001(8) 0.015(7) 0.024(8) C99 0.047(10) 0.033(10) 0.038(10) -0.001(8) 0.005(8) -0.005(7) C100 0.037(10) 0.068(14) 0.072(12) 0.003(10) 0.003(8) -0.004(10) C101 0.076(12) 0.055(12) 0.038(10) 0.011(8) 0.000(8) 0.047(9) C102 0.038(9) 0.018(9) 0.049(11) 0.015(8) 0.005(8) 0.002(6) C104 0.061(12) 0.049(11) 0.024(9) -0.011(8) -0.021(9) 0.013(9) C105 0.063(11) 0.061(14) 0.092(14) -0.003(10) 0.030(10) 0.034(10) C106 0.074(12) 0.030(10) 0.037(10) -0.011(8) 0.011(9) -0.006(9) C107 0.022(9) 0.079(15) 0.052(11) 0.003(10) 0.000(7) -0.010(10) C109 0.038(10) 0.049(11) 0.054(11) 0.000(9) -0.017(9) -0.015(8) C110 0.029(8) 0.035(10) 0.023(9) -0.007(7) -0.010(7) 0.006(7) C111 0.084(14) 0.047(12) 0.034(11) -0.015(8) -0.008(10) 0.014(10) C112 0.030(9) 0.056(11) 0.045(11) -0.009(9) 0.008(8) 0.006(8) C113 0.021(9) 0.063(13) 0.037(9) 0.011(8) 0.013(7) 0.012(9) C114 0.024(9) 0.033(10) 0.032(9) -0.003(7) -0.005(7) 0.006(7) C115 0.071(12) 0.095(16) 0.079(13) -0.047(12) 0.029(10) -0.050(11) C116 0.039(10) 0.053(13) 0.053(11) 0.011(9) -0.001(8) 0.015(9) C118 0.041(10) 0.065(13) 0.079(13) -0.005(10) -0.014(9) -0.005(9) C119 0.081(13) 0.041(11) 0.044(11) -0.009(9) -0.021(10) -0.020(10) C120 0.041(10) 0.071(13) 0.079(13) 0.023(10) -0.016(9) -0.016(9) C121 0.050(10) 0.041(11) 0.052(10) 0.013(8) -0.021(8) -0.014(8) C122 0.085(14) 0.055(12) 0.039(11) 0.017(9) 0.035(11) 0.030(10) C125 0.048(10) 0.036(10) 0.053(10) 0.015(8) -0.002(8) 0.017(8) C126 0.049(12) 0.052(13) 0.034(9) -0.010(8) 0.016(8) -0.030(10) C128 0.073(12) 0.066(13) 0.074(12) 0.002(10) 0.058(10) -0.009(10) C130 0.069(12) 0.049(11) 0.032(10) 0.008(8) 0.011(10) 0.013(9) C131 0.075(13) 0.087(15) 0.066(13) -0.020(11) -0.002(10) -0.019(11) C132 0.059(12) 0.040(11) 0.041(10) 0.014(8) 0.017(9) 0.013(10) C133 0.078(12) 0.080(14) 0.046(11) 0.022(9) 0.029(9) 0.009(10) C134 0.065(11) 0.061(12) 0.079(13) -0.006(10) 0.041(10) -0.013(9) C135 0.130(16) 0.061(13) 0.037(11) -0.018(9) 0.009(10) -0.027(11) C136 0.057(11) 0.087(15) 0.054(11) 0.009(10) 0.010(9) 0.025(10) C138 0.056(10) 0.023(10) 0.068(11) -0.016(8) 0.003(8) -0.004(8) C140 0.033(9) 0.034(10) 0.053(12) -0.003(8) -0.001(8) 0.007(7) C142 0.100(13) 0.062(13) 0.042(10) -0.023(9) 0.036(10) -0.001(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N8 1.853(12) . ? Co1 N10 1.877(12) . ? Co1 N3 1.910(11) . ? Co1 N21 1.931(11) . ? Co1 N7 1.932(11) . ? Co1 N6 1.941(10) . ? Co2 N23 1.856(12) . ? Co2 N22 1.857(12) . ? Co2 N5 1.896(10) . ? Co2 N15 1.909(10) . ? Co2 N13 1.915(11) . ? Co2 N20 1.918(10) . ? Co3 N12 1.849(12) . ? Co3 N4 1.862(12) . ? Co3 N2 1.916(11) . ? Co3 N27 1.923(10) . ? Co3 N37 1.939(10) . ? Co3 N11 1.956(10) . ? Fe4 C62 1.861(16) . ? Fe4 C85 1.865(15) . ? Fe4 C29 1.876(17) . ? Fe4 C44 1.889(15) . ? Fe4 C26 1.896(16) . ? Fe4 C90 1.912(18) . ? Fe5 C19 1.884(16) . ? Fe5 C70 1.895(16) . ? Fe5 C102 1.903(16) . ? Fe5 C66 1.907(17) . ? Fe5 C31 1.922(17) . ? Fe5 C58 1.942(18) . ? Cl1B O2B 1.33(3) 2_545 ? Cl1B O6B 1.37(3) 2_445 ? Cl1B O4B 1.44(2) . ? Cl1B O5B 1.46(2) . ? Cl1B O7B 1.463(17) 2_445 ? Cl1B O3B 1.47(3) 2_545 ? Cl1B O21S 1.51(3) 2_445 ? Cl1A O3A 1.40(3) . ? Cl1A O50S 1.416(17) 3_566 ? Cl1A O5A 1.42(2) 4_666 ? Cl1A O4A 1.43(3) . ? Cl1A O7A 1.46(3) 4_666 ? Cl1A O2A 1.46(3) . ? Cl1A O6A 1.48(3) . ? Na3 O44S 2.938(15) 4_565 ? O44S Na3 2.938(15) 4_666 ? O50S Cl1A 1.416(17) 3_566 ? O7A O5A 1.10(3) . ? O7A Cl1A 1.46(3) 4_565 ? O7B Cl1B 1.463(17) 2_455 ? O6B Cl1B 1.37(3) 2_455 ? O6A O2A 1.03(3) . ? O3A O4A 1.17(3) . ? O3A O2A 1.39(3) . ? O2B Cl1B 1.33(3) 2 ? O3B Cl1B 1.47(3) 2 ? O5A Cl1A 1.42(2) 4_565 ? O21S Cl1B 1.51(3) 2_455 ? N1 C85 1.158(16) . ? N2 C33 1.335(17) . ? N2 C81 1.374(16) . ? N3 C65 1.332(15) . ? N3 C17 1.344(16) . ? N4 C66 1.143(15) . ? N5 C82 1.325(15) . ? N5 C16 1.353(16) . ? N6 C30 1.306(15) . ? N6 C42 1.318(15) . ? N7 C79 1.328(16) . ? N7 C64 1.340(17) . ? N8 C26 1.154(15) . ? N10 C70 1.151(15) . ? N11 C73 1.30(2) . ? N11 C80 1.330(15) . ? N12 C44 1.162(15) . ? N13 C140 1.314(16) . ? N13 C110 1.355(16) . ? N15 C46 1.324(15) . ? N15 C52 1.378(16) . ? N20 C99 1.319(15) . ? N20 C54 1.344(16) . ? N21 C98 1.329(17) . ? N21 C50 1.391(17) . ? N22 C29 1.158(15) . ? N23 C31 1.143(15) . ? N25 C19 1.161(16) . ? N27 C114 1.324(16) . ? N27 C35 1.355(16) . ? N36 C62 1.165(16) . ? N37 C49 1.324(15) . ? N37 C76 1.368(16) . ? N41 C102 1.167(16) . ? N84 C58 1.134(16) . ? N108 C90 1.153(17) . ? C1 C110 1.368(18) . ? C1 C75 1.378(19) . ? C1 C92 1.437(19) . ? C9 C56 1.375(18) . ? C9 C30 1.375(17) . ? C9 C89 1.548(19) . ? C14 C114 1.378(18) . ? C14 C95 1.378(19) . ? C14 C121 1.50(2) . ? C16 C40 1.425(18) . ? C16 C54 1.429(18) . ? C17 C67 1.383(18) . ? C18 C68 1.367(19) . ? C18 C82 1.375(18) . ? C18 C134 1.494(19) . ? C24 C67 1.372(18) . ? C24 C63 1.408(19) . ? C24 C96 1.511(18) . ? C28 C52 1.388(18) . ? C28 C88 1.415(19) . ? C28 C87 1.420(19) . ? C32 C73 1.35(2) . ? C32 C104 1.41(2) . ? C32 C111 1.45(2) . ? C33 C97 1.450(19) . ? C34 C76 1.407(18) . ? C34 C130 1.42(2) . ? C34 C122 1.44(2) . ? C35 C71 1.340(17) . ? C35 C81 1.389(18) . ? C38 C104 1.362(19) . ? C38 C80 1.413(18) . ? C38 C118 1.532(19) . ? C39 C81 1.363(18) . ? C39 C43 1.393(19) . ? C39 C116 1.431(18) . ? C40 C68 1.391(19) . ? C40 C109 1.401(19) . ? C42 C65 1.401(18) . ? C42 C47 1.412(18) . ? C43 C97 1.368(18) . ? C43 C94 1.504(19) . ? C45 C75 1.47(2) . ? C46 C60 1.400(17) . ? C47 C56 1.395(18) . ? C47 C69 1.420(18) . ? C48 C122 1.35(2) . ? C48 C49 1.392(19) . ? C48 C128 1.506(19) . ? C50 C79 1.402(19) . ? C50 C113 1.409(19) . ? C52 C110 1.402(17) . ? C53 C107 1.32(2) . ? C53 C126 1.47(2) . ? C54 C77 1.387(19) . ? C55 C68 1.521(19) . ? C56 C78 1.547(18) . ? C59 C83 1.38(2) . ? C59 C64 1.408(19) . ? C59 C86 1.48(2) . ? C60 C88 1.381(18) . ? C60 C74 1.498(17) . ? C61 C106 1.378(19) . ? C61 C77 1.396(19) . ? C61 C135 1.497(19) . ? C63 C65 1.370(18) . ? C63 C112 1.443(19) . ? C67 C125 1.512(18) . ? C69 C112 1.325(18) . ? C71 C100 1.42(2) . ? C71 C95 1.449(18) . ? C72 C140 1.381(19) . ? C72 C75 1.415(19) . ? C72 C101 1.510(18) . ? C73 C76 1.39(2) . ? C77 C119 1.42(2) . ? C79 C126 1.354(19) . ? C83 C126 1.40(2) . ? C83 C115 1.49(2) . ? C87 C92 1.355(19) . ? C88 C91 1.503(18) . ? C93 C132 1.321(19) . ? C93 C113 1.40(2) . ? C93 C136 1.461(19) . ? C95 C120 1.507(18) . ? C97 C138 1.541(19) . ? C98 C132 1.414(19) . ? C99 C106 1.379(18) . ? C100 C116 1.37(2) . ? C104 C131 1.504(19) . ? C105 C132 1.50(2) . ? C106 C142 1.537(19) . ? C107 C113 1.41(2) . ? C109 C119 1.39(2) . ? C111 C130 1.32(2) . ? C122 C133 1.50(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Co1 N10 91.3(4) . . ? N8 Co1 N3 90.8(4) . . ? N10 Co1 N3 93.6(5) . . ? N8 Co1 N21 93.1(5) . . ? N10 Co1 N21 90.7(4) . . ? N3 Co1 N21 174.2(5) . . ? N8 Co1 N7 176.0(5) . . ? N10 Co1 N7 90.3(4) . . ? N3 Co1 N7 92.8(5) . . ? N21 Co1 N7 83.2(5) . . ? N8 Co1 N6 89.1(4) . . ? N10 Co1 N6 176.0(5) . . ? N3 Co1 N6 82.4(5) . . ? N21 Co1 N6 93.3(4) . . ? N7 Co1 N6 89.6(4) . . ? N23 Co2 N22 90.3(5) . . ? N23 Co2 N5 175.9(5) . . ? N22 Co2 N5 87.4(4) . . ? N23 Co2 N15 92.4(4) . . ? N22 Co2 N15 92.6(5) . . ? N5 Co2 N15 91.1(5) . . ? N23 Co2 N13 90.3(5) . . ? N22 Co2 N13 175.9(5) . . ? N5 Co2 N13 92.2(4) . . ? N15 Co2 N13 83.3(5) . . ? N23 Co2 N20 92.6(5) . . ? N22 Co2 N20 91.3(5) . . ? N5 Co2 N20 84.1(5) . . ? N15 Co2 N20 173.7(4) . . ? N13 Co2 N20 92.7(5) . . ? N12 Co3 N4 90.9(5) . . ? N12 Co3 N2 89.6(4) . . ? N4 Co3 N2 174.7(5) . . ? N12 Co3 N27 89.6(5) . . ? N4 Co3 N27 91.7(5) . . ? N2 Co3 N27 83.1(5) . . ? N12 Co3 N37 176.7(5) . . ? N4 Co3 N37 90.5(4) . . ? N2 Co3 N37 89.3(4) . . ? N27 Co3 N37 93.3(5) . . ? N12 Co3 N11 94.0(5) . . ? N4 Co3 N11 89.6(4) . . ? N2 Co3 N11 95.6(5) . . ? N27 Co3 N11 176.1(4) . . ? N37 Co3 N11 83.0(5) . . ? C62 Fe4 C85 88.2(6) . . ? C62 Fe4 C29 92.4(6) . . ? C85 Fe4 C29 87.5(6) . . ? C62 Fe4 C44 88.3(5) . . ? C85 Fe4 C44 174.6(6) . . ? C29 Fe4 C44 88.4(5) . . ? C62 Fe4 C26 177.6(5) . . ? C85 Fe4 C26 94.2(6) . . ? C29 Fe4 C26 87.7(5) . . ? C44 Fe4 C26 89.3(5) . . ? C62 Fe4 C90 89.7(6) . . ? C85 Fe4 C90 92.9(6) . . ? C29 Fe4 C90 177.8(6) . . ? C44 Fe4 C90 91.3(6) . . ? C26 Fe4 C90 90.1(6) . . ? C19 Fe5 C70 90.6(6) . . ? C19 Fe5 C102 88.8(6) . . ? C70 Fe5 C102 179.2(6) . . ? C19 Fe5 C66 178.8(6) . . ? C70 Fe5 C66 90.6(5) . . ? C102 Fe5 C66 90.0(5) . . ? C19 Fe5 C31 90.9(5) . . ? C70 Fe5 C31 88.2(5) . . ? C102 Fe5 C31 91.3(5) . . ? C66 Fe5 C31 89.1(5) . . ? C19 Fe5 C58 91.6(6) . . ? C70 Fe5 C58 92.9(5) . . ? C102 Fe5 C58 87.7(5) . . ? C66 Fe5 C58 88.3(6) . . ? C31 Fe5 C58 177.2(6) . . ? O2B Cl1B O6B 152.2(18) 2_545 2_445 ? O2B Cl1B O4B 84.0(16) 2_545 . ? O6B Cl1B O4B 121.3(18) 2_445 . ? O2B Cl1B O5B 112.5(14) 2_545 . ? O6B Cl1B O5B 88.6(15) 2_445 . ? O4B Cl1B O5B 34.8(11) . . ? O2B Cl1B O7B 95.4(14) 2_545 2_445 ? O6B Cl1B O7B 90.0(14) 2_445 2_445 ? O4B Cl1B O7B 102.9(13) . 2_445 ? O5B Cl1B O7B 117.6(11) . 2_445 ? O2B Cl1B O3B 50.5(14) 2_545 2_545 ? O6B Cl1B O3B 106.4(17) 2_445 2_545 ? O4B Cl1B O3B 107.5(15) . 2_545 ? O5B Cl1B O3B 110.1(13) . 2_545 ? O7B Cl1B O3B 129.7(14) 2_445 2_545 ? O2B Cl1B O21S 106.5(18) 2_545 2_445 ? O6B Cl1B O21S 47.4(14) 2_445 2_445 ? O4B Cl1B O21S 139.0(15) . 2_445 ? O5B Cl1B O21S 108.8(14) . 2_445 ? O7B Cl1B O21S 115.0(13) 2_445 2_445 ? O3B Cl1B O21S 59.3(15) 2_545 2_445 ? O3A Cl1A O50S 127.2(13) . 3_566 ? O3A Cl1A O5A 98.3(14) . 4_666 ? O50S Cl1A O5A 116.4(11) 3_566 4_666 ? O3A Cl1A O4A 48.7(14) . . ? O50S Cl1A O4A 87.0(15) 3_566 . ? O5A Cl1A O4A 96.5(15) 4_666 . ? O3A Cl1A O7A 127.5(15) . 4_666 ? O50S Cl1A O7A 104.8(13) 3_566 4_666 ? O5A Cl1A O7A 44.9(10) 4_666 4_666 ? O4A Cl1A O7A 141.0(16) . 4_666 ? O3A Cl1A O2A 58.0(14) . . ? O50S Cl1A O2A 121.7(13) 3_566 . ? O5A Cl1A O2A 119.7(14) 4_666 . ? O4A Cl1A O2A 101.3(17) . . ? O7A Cl1A O2A 103.3(15) 4_666 . ? O3A Cl1A O6A 98.2(15) . . ? O50S Cl1A O6A 92.7(13) 3_566 . ? O5A Cl1A O6A 125.6(14) 4_666 . ? O4A Cl1A O6A 132.0(17) . . ? O7A Cl1A O6A 85.2(15) 4_666 . ? O2A Cl1A O6A 40.8(12) . . ? O5A O7A Cl1A 65.8(17) . 4_565 ? O2A O6A Cl1A 68(2) . . ? O4A O3A O2A 122(3) . . ? O4A O3A Cl1A 67(2) . . ? O2A O3A Cl1A 63.4(16) . . ? O7A O5A Cl1A 69.3(17) . 4_565 ? O6A O2A O3A 128(3) . . ? O6A O2A Cl1A 71(2) . . ? O3A O2A Cl1A 58.6(15) . . ? O3A O4A Cl1A 64(2) . . ? C33 N2 C81 119.4(12) . . ? C33 N2 Co3 127.6(10) . . ? C81 N2 Co3 112.9(9) . . ? C65 N3 C17 115.3(11) . . ? C65 N3 Co1 114.1(9) . . ? C17 N3 Co1 130.1(9) . . ? C66 N4 Co3 162.2(11) . . ? C82 N5 C16 114.6(11) . . ? C82 N5 Co2 131.7(10) . . ? C16 N5 Co2 113.6(9) . . ? C30 N6 C42 119.4(11) . . ? C30 N6 Co1 128.7(9) . . ? C42 N6 Co1 111.9(9) . . ? C79 N7 C64 117.7(12) . . ? C79 N7 Co1 114.2(10) . . ? C64 N7 Co1 128.1(10) . . ? C26 N8 Co1 167.3(10) . . ? C70 N10 Co1 162.6(10) . . ? C73 N11 C80 118.8(13) . . ? C73 N11 Co3 113.3(11) . . ? C80 N11 Co3 127.8(9) . . ? C44 N12 Co3 162.1(10) . . ? C140 N13 C110 116.6(12) . . ? C140 N13 Co2 129.7(10) . . ? C110 N13 Co2 113.7(9) . . ? C46 N15 C52 116.4(11) . . ? C46 N15 Co2 130.7(9) . . ? C52 N15 Co2 112.8(8) . . ? C99 N20 C54 115.9(11) . . ? C99 N20 Co2 131.5(9) . . ? C54 N20 Co2 112.6(9) . . ? C98 N21 C50 119.0(13) . . ? C98 N21 Co1 129.4(10) . . ? C50 N21 Co1 111.6(10) . . ? C29 N22 Co2 160.2(11) . . ? C31 N23 Co2 162.9(11) . . ? C114 N27 C35 117.3(11) . . ? C114 N27 Co3 129.0(9) . . ? C35 N27 Co3 113.6(9) . . ? C49 N37 C76 119.8(12) . . ? C49 N37 Co3 129.8(10) . . ? C76 N37 Co3 110.4(9) . . ? C110 C1 C75 118.8(13) . . ? C110 C1 C92 118.0(13) . . ? C75 C1 C92 123.2(14) . . ? C56 C9 C30 119.1(12) . . ? C56 C9 C89 122.4(12) . . ? C30 C9 C89 118.4(12) . . ? C114 C14 C95 119.5(15) . . ? C114 C14 C121 119.2(13) . . ? C95 C14 C121 121.2(13) . . ? N5 C16 C40 124.2(13) . . ? N5 C16 C54 114.1(12) . . ? C40 C16 C54 121.7(13) . . ? N3 C17 C67 124.5(12) . . ? C68 C18 C82 118.4(13) . . ? C68 C18 C134 122.1(13) . . ? C82 C18 C134 119.5(14) . . ? N25 C19 Fe5 179.8(14) . . ? C67 C24 C63 117.6(12) . . ? C67 C24 C96 119.9(13) . . ? C63 C24 C96 122.5(13) . . ? N8 C26 Fe4 175.0(11) . . ? C52 C28 C88 117.7(13) . . ? C52 C28 C87 117.4(13) . . ? C88 C28 C87 124.8(13) . . ? N22 C29 Fe4 174.6(12) . . ? N6 C30 C9 123.2(12) . . ? N23 C31 Fe5 175.3(12) . . ? C73 C32 C104 118.3(15) . . ? C73 C32 C111 117.2(16) . . ? C104 C32 C111 124.4(15) . . ? N2 C33 C97 119.8(13) . . ? C76 C34 C130 115.2(14) . . ? C76 C34 C122 120.0(14) . . ? C130 C34 C122 124.8(15) . . ? C71 C35 N27 124.1(13) . . ? C71 C35 C81 120.9(13) . . ? N27 C35 C81 114.9(12) . . ? C104 C38 C80 118.9(13) . . ? C104 C38 C118 126.3(13) . . ? C80 C38 C118 114.7(14) . . ? C81 C39 C43 121.3(13) . . ? C81 C39 C116 116.3(14) . . ? C43 C39 C116 122.4(13) . . ? C68 C40 C109 127.6(14) . . ? C68 C40 C16 116.8(13) . . ? C109 C40 C16 115.5(14) . . ? N6 C42 C65 117.1(12) . . ? N6 C42 C47 122.0(13) . . ? C65 C42 C47 120.8(13) . . ? C97 C43 C39 117.4(13) . . ? C97 C43 C94 118.5(14) . . ? C39 C43 C94 124.1(13) . . ? N12 C44 Fe4 175.8(11) . . ? N15 C46 C60 124.1(12) . . ? C56 C47 C42 117.7(12) . . ? C56 C47 C69 125.8(13) . . ? C42 C47 C69 116.4(13) . . ? C122 C48 C49 118.8(14) . . ? C122 C48 C128 121.6(14) . . ? C49 C48 C128 119.5(15) . . ? N37 C49 C48 124.2(14) . . ? N21 C50 C79 115.4(13) . . ? N21 C50 C113 120.5(15) . . ? C79 C50 C113 124.0(14) . . ? N15 C52 C28 123.8(13) . . ? N15 C52 C110 114.6(12) . . ? C28 C52 C110 121.5(13) . . ? C107 C53 C126 121.4(15) . . ? N20 C54 C77 124.1(13) . . ? N20 C54 C16 115.2(13) . . ? C77 C54 C16 120.7(13) . . ? C9 C56 C47 118.4(12) . . ? C9 C56 C78 122.1(13) . . ? C47 C56 C78 119.5(12) . . ? N84 C58 Fe5 177.3(14) . . ? C83 C59 C64 118.5(15) . . ? C83 C59 C86 126.1(14) . . ? C64 C59 C86 115.4(15) . . ? C88 C60 C46 119.0(12) . . ? C88 C60 C74 124.2(12) . . ? C46 C60 C74 116.8(12) . . ? C106 C61 C77 117.8(13) . . ? C106 C61 C135 120.2(14) . . ? C77 C61 C135 122.0(15) . . ? N36 C62 Fe4 177.3(14) . . ? C65 C63 C24 118.4(13) . . ? C65 C63 C112 117.7(13) . . ? C24 C63 C112 123.9(14) . . ? N7 C64 C59 122.4(14) . . ? N3 C65 C63 125.1(12) . . ? N3 C65 C42 113.6(12) . . ? C63 C65 C42 121.2(13) . . ? N4 C66 Fe5 176.1(12) . . ? C24 C67 C17 119.0(13) . . ? C24 C67 C125 122.2(13) . . ? C17 C67 C125 118.8(13) . . ? C18 C68 C40 119.4(12) . . ? C18 C68 C55 121.7(14) . . ? C40 C68 C55 118.9(14) . . ? C112 C69 C47 122.6(13) . . ? N10 C70 Fe5 175.2(11) . . ? C35 C71 C100 118.1(14) . . ? C35 C71 C95 118.3(12) . . ? C100 C71 C95 123.6(14) . . ? C140 C72 C75 119.1(13) . . ? C140 C72 C101 118.6(13) . . ? C75 C72 C101 122.3(13) . . ? N11 C73 C32 124.6(17) . . ? N11 C73 C76 115.8(17) . . ? C32 C73 C76 119.6(18) . . ? C1 C75 C72 117.4(13) . . ? C1 C75 C45 122.4(15) . . ? C72 C75 C45 120.2(15) . . ? N37 C76 C73 117.4(14) . . ? N37 C76 C34 118.8(14) . . ? C73 C76 C34 123.8(15) . . ? C54 C77 C61 118.0(14) . . ? C54 C77 C119 117.3(14) . . ? C61 C77 C119 124.7(15) . . ? N7 C79 C126 123.9(15) . . ? N7 C79 C50 115.2(12) . . ? C126 C79 C50 120.8(15) . . ? N11 C80 C38 121.3(13) . . ? C39 C81 N2 121.5(14) . . ? C39 C81 C35 123.2(14) . . ? N2 C81 C35 115.2(13) . . ? N5 C82 C18 126.5(13) . . ? C59 C83 C126 117.9(13) . . ? C59 C83 C115 121.2(16) . . ? C126 C83 C115 120.9(16) . . ? N1 C85 Fe4 179.6(16) . . ? C92 C87 C28 121.1(13) . . ? C60 C88 C28 118.6(12) . . ? C60 C88 C91 121.0(13) . . ? C28 C88 C91 120.4(13) . . ? N108 C90 Fe4 175.9(14) . . ? C87 C92 C1 120.9(14) . . ? C132 C93 C113 118.1(13) . . ? C132 C93 C136 122.1(16) . . ? C113 C93 C136 119.8(15) . . ? C14 C95 C71 116.9(12) . . ? C14 C95 C120 121.6(14) . . ? C71 C95 C120 121.4(13) . . ? C43 C97 C33 120.4(14) . . ? C43 C97 C138 123.4(13) . . ? C33 C97 C138 116.2(14) . . ? N21 C98 C132 120.1(14) . . ? N20 C99 C106 124.8(13) . . ? C116 C100 C71 121.2(14) . . ? N41 C102 Fe5 176.4(13) . . ? C38 C104 C32 118.0(13) . . ? C38 C104 C131 119.3(15) . . ? C32 C104 C131 122.6(14) . . ? C61 C106 C99 118.8(13) . . ? C61 C106 C142 123.1(13) . . ? C99 C106 C142 118.1(14) . . ? C53 C107 C113 124.3(15) . . ? C119 C109 C40 122.8(14) . . ? N13 C110 C1 124.5(12) . . ? N13 C110 C52 114.6(12) . . ? C1 C110 C52 120.7(13) . . ? C130 C111 C32 122.9(15) . . ? C69 C112 C63 121.0(14) . . ? C93 C113 C50 119.1(14) . . ? C93 C113 C107 127.6(14) . . ? C50 C113 C107 113.3(15) . . ? N27 C114 C14 123.5(13) . . ? C100 C116 C39 120.1(14) . . ? C109 C119 C77 121.7(14) . . ? C48 C122 C34 118.4(13) . . ? C48 C122 C133 121.1(16) . . ? C34 C122 C133 120.5(17) . . ? C79 C126 C83 119.4(15) . . ? C79 C126 C53 116.2(16) . . ? C83 C126 C53 124.4(15) . . ? C111 C130 C34 121.2(15) . . ? C93 C132 C98 122.9(15) . . ? C93 C132 C105 120.9(15) . . ? C98 C132 C105 116.2(15) . . ? N13 C140 C72 123.6(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.252 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.146 #end================================================= data_{[Co(bpy)2]3[Fe(CN)6]2}[Fe(CN)6]1/3 #=================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; '{[Co(bpy)2]3[Fe(CN)6]2}[Fe(CN)6]1/3' ; _chemical_name_common '{[Co(bpy)2]3[Fe(CN)6]2}[Fe(CN)6]1/3' _chemical_melting_point ? _chemical_formula_moiety 'C74 H88 Co3 Fe2.33 N26 O20' _chemical_formula_sum 'C74 H88 Co3 Fe2.33 N26 O20' _chemical_formula_weight 1968.8 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'hexagonal' _symmetry_space_group_name_H-M 'P6(3)22' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' _cell_length_a 18.530(3) _cell_length_b 18.530(3) _cell_length_c 31.483(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 9362(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8272 _cell_measurement_theta_min 2.197 _cell_measurement_theta_max 22.5785 _exptl_crystal_description 'needle' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.85 _exptl_crystal_size_mid 0.84 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3903 _exptl_absorpt_coefficient_mu 0.949 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.4992 _exptl_absorpt_correction_T_max 0.8112 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42101 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 23.28 _reflns_number_total 4514 _reflns_number_gt 3960 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1084P)^2^+24.04P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00015(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(4) _refine_ls_number_reflns 4514 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.1963 _refine_ls_wR_factor_gt 0.1892 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.074 _refine_ls_shift/su_mean 0.007 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.78102(2) 0.21898(2) 0.2500 0.0499(2) Uani 1 2 d S . . Co2 Co 1.0000 0.21142(3) 0.5000 0.02801(16) Uani 1 2 d S . . Fe1 Fe 0.6667 0.3333 0.35067(4) 0.0395(3) Uani 1 3 d S . . Fe2 Fe 1.0000 0.0000 0.59228(3) 0.0281(2) Uani 1 3 d S . . Fe1A Fe 1.3333 0.6667 0.22282(12) 0.0258(8) Uiso 0.23 3 d SP . . Fe2A Fe 1.3333 0.6667 0.2500 0.020(3) Uiso 0.08 6 d SP . . O2S O 1.1127(5) 0.1550(6) 0.2667(3) 0.102(3) Uiso 0.50 1 d P A -2 O3S O 1.1605(8) 0.3152(5) 0.2607(2) 0.092(3) Uiso 0.50 1 d P B -1 O4S O 1.2092(10) 0.4035(9) 0.3135(5) 0.080(4) Uiso 0.25 1 d P C -2 O5S O 1.2450(5) 0.4652(5) 0.0928(3) 0.097(3) Uiso 0.50 1 d P D -1 O6S O 1.2271(11) 0.4413(10) 0.1208(5) 0.073(5) Uiso 0.22 1 d P E -2 O7S O 1.1206(4) 0.5172(4) 0.1053(2) 0.155(3) Uiso 1 1 d . . . O8S O 0.5689(6) 0.0241(6) 0.4324(3) 0.115(3) Uiso 0.50 1 d P . -2 O9S O 0.5345(9) 0.0801(9) 0.4866(4) 0.072(4) Uiso 0.25 1 d P F -2 O10S O 0.5317(8) 0.1747(8) 0.5336(4) 0.150(5) Uiso 0.50 1 d P . . O11S O 0.6033(4) -0.0290(4) 0.6069(2) 0.071(2) Uiso 0.50 1 d P . . O12S O 0.7358(6) 0.0424(6) 0.6594(3) 0.098(3) Uiso 0.50 1 d P G -2 O13S O 0.7761(7) 0.0946(7) 0.6628(3) 0.119(4) Uiso 0.50 1 d P H -1 O14S O 1.1542(5) 0.1133(5) 0.2661(3) 0.085(3) Uiso 0.50 1 d P I -14 O15S O 0.6667 0.3333 0.4909(7) 0.169(8) Uiso 0.60 3 d SP . . O16S O 0.5334(8) -0.0116(12) 3.9988(15) 0.096(4) Uiso 0.25 1 d P J -3 N1 N 0.84898(19) 0.2036(2) 0.29107(13) 0.0579(10) Uani 1 1 d . . . N2 N 0.88497(19) 0.3173(2) 0.23601(14) 0.0571(12) Uani 1 1 d . . . N4 N 0.97357(17) 0.27233(18) 0.45821(11) 0.0355(9) Uani 1 1 d . . . N5 N 0.88234(16) 0.15678(18) 0.51056(10) 0.0318(9) Uani 1 1 d . . . N11 N 0.76147(19) 0.2809(2) 0.29028(12) 0.0465(11) Uani 1 1 d . . . N12 N 0.6378(2) 0.1857(2) 0.40601(18) 0.0723(15) Uani 1 1 d . . . N23 N 1.01994(16) 0.14877(16) 0.54041(10) 0.0284(9) Uani 1 1 d . . . N24 N 0.8851(2) 0.0397(2) 0.64571(13) 0.0522(12) Uani 1 1 d . . . N1A N 1.2243(9) 0.5144(10) 0.2811(5) 0.088(5) Uiso 0.33 1 d P . . N2A N 1.1730(7) 0.6265(8) 0.1654(4) 0.060(3) Uiso 0.33 1 d P . . C1 C 0.8210(3) 0.1445(3) 0.32128(17) 0.0717(16) Uani 1 1 d . . . H1 H 0.7633 0.1044 0.3226 0.086 Uiso 1 1 calc R . . C2 C 0.8757(3) 0.1411(3) 0.35094(19) 0.0835(17) Uani 1 1 d . . . H2 H 0.8559 0.1012 0.3732 0.100 Uiso 1 1 calc R . . C3 C 0.9617(3) 0.1995(3) 0.34632(19) 0.0930(16) Uani 1 1 d . . . H3 H 1.0012 0.1972 0.3647 0.112 Uiso 1 1 calc R . . C4 C 0.9870(3) 0.2572(4) 0.31630(17) 0.0864(18) Uani 1 1 d . . . H4 H 1.0446 0.2970 0.3138 0.104 Uiso 1 1 calc R . . C5 C 0.9307(2) 0.2604(3) 0.28868(16) 0.0576(13) Uani 1 1 d . . . C6 C 0.9502(2) 0.3237(3) 0.25821(17) 0.0619(14) Uani 1 1 d . . . C7 C 1.0300(3) 0.3899(4) 0.2503(2) 0.0869(19) Uani 1 1 d . . . H7 H 1.0766 0.3948 0.2656 0.104 Uiso 1 1 calc R . . C8 C 1.0407(3) 0.4492(4) 0.2197(2) 0.086(2) Uani 1 1 d . . . H8 H 1.0948 0.4947 0.2142 0.103 Uiso 1 1 calc R . . C9 C 0.9738(3) 0.4421(4) 0.1975(2) 0.080(2) Uani 1 1 d . . . H9 H 0.9807 0.4819 0.1765 0.096 Uiso 1 1 calc R . . C10 C 0.8970(3) 0.3760(3) 0.2066(2) 0.0647(16) Uani 1 1 d . . . H10 H 0.8500 0.3709 0.1918 0.078 Uiso 1 1 calc R . . C11 C 0.7312(2) 0.3058(2) 0.31416(16) 0.0444(13) Uani 1 1 d . . . C12 C 0.6478(2) 0.2407(3) 0.38564(17) 0.0486(14) Uani 1 1 d . . . C13 C 0.8406(2) 0.0990(2) 0.54029(14) 0.0396(12) Uani 1 1 d . . . H13 H 0.8707 0.0812 0.5576 0.048 Uiso 1 1 calc R . . C14 C 0.7576(3) 0.0647(3) 0.54703(17) 0.0552(16) Uani 1 1 d . . . H14 H 0.7299 0.0236 0.5684 0.066 Uiso 1 1 calc R . . C15 C 0.7140(3) 0.0922(3) 0.52114(17) 0.0602(17) Uani 1 1 d . . . H15 H 0.6562 0.0710 0.5256 0.072 Uiso 1 1 calc R . . C16 C 0.7544(2) 0.1491(3) 0.48979(15) 0.0472(14) Uani 1 1 d . . . H16 H 0.7251 0.1655 0.4710 0.057 Uiso 1 1 calc R . . C17 C 0.8407(2) 0.1824(2) 0.48620(13) 0.0406(12) Uani 1 1 d . . . C18 C 0.8916(2) 0.2462(2) 0.45568(14) 0.0374(11) Uani 1 1 d . . . C19 C 0.8628(3) 0.2832(3) 0.42574(15) 0.0494(13) Uani 1 1 d . . . H19 H 0.8051 0.2653 0.4238 0.059 Uiso 1 1 calc R . . C20 C 0.9186(3) 0.3447(3) 0.39977(15) 0.0521(14) Uani 1 1 d . . . H20 H 0.8999 0.3691 0.3792 0.062 Uiso 1 1 calc R . . C21 C 1.0005(3) 0.3707(3) 0.40333(14) 0.0536(13) Uani 1 1 d . . . H21 H 1.0397 0.4143 0.3857 0.064 Uiso 1 1 calc R . . C22 C 1.0271(2) 0.3339(3) 0.43260(13) 0.0446(12) Uani 1 1 d . . . H22 H 1.0849 0.3526 0.4347 0.054 Uiso 1 1 calc R . . C23 C 1.01723(19) 0.0927(2) 0.55879(11) 0.0279(10) Uani 1 1 d . . . C24 C 0.9290(2) 0.0229(2) 0.62699(13) 0.0359(12) Uani 1 1 d . . . C1A C 1.2644(7) 0.5700(8) 0.2597(4) 0.052(4) Uiso 0.33 1 d P . . C2A C 1.2352(9) 0.6401(9) 0.1831(5) 0.054(4) Uiso 0.33 1 d P . . Fe3A Fe 1.3333 0.6667 0.2061(4) 0.006(2) Uiso 0.06 3 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.04942(16) 0.04942(16) 0.0715(5) -0.0164(5) -0.0164(5) 0.0402(2) Co2 0.0225(3) 0.0216(2) 0.0403(4) -0.00096(18) -0.0019(4) 0.01123(16) Fe1 0.0237(3) 0.0237(3) 0.0713(7) 0.000 0.000 0.01184(14) Fe2 0.0268(2) 0.0268(2) 0.0307(4) 0.000 0.000 0.01342(12) N1 0.0707(14) 0.0745(15) 0.068(2) -0.0216(17) -0.0243(17) 0.0658(11) N2 0.0425(14) 0.0600(17) 0.086(3) -0.0129(18) -0.0059(18) 0.0384(11) N4 0.0342(13) 0.0286(12) 0.0471(19) 0.0006(14) -0.0024(14) 0.0183(10) N5 0.0249(12) 0.0318(13) 0.0376(19) -0.0079(12) -0.0058(12) 0.0134(10) N11 0.0422(14) 0.0391(14) 0.069(2) -0.0198(16) -0.0105(16) 0.0281(11) N12 0.0535(18) 0.0519(18) 0.122(4) 0.012(2) -0.013(2) 0.0344(14) N23 0.0215(12) 0.0196(12) 0.0425(18) 0.0021(12) -0.0009(13) 0.0090(9) N24 0.0421(16) 0.0517(18) 0.060(2) -0.0084(18) 0.0108(17) 0.0214(14) C1 0.099(3) 0.052(2) 0.089(4) -0.018(2) -0.032(3) 0.0566(17) C2 0.131(3) 0.074(2) 0.083(4) -0.026(2) -0.041(3) 0.0796(18) C3 0.120(2) 0.152(3) 0.077(3) -0.061(3) -0.051(3) 0.1196(18) C4 0.081(2) 0.152(3) 0.069(3) -0.040(3) -0.019(3) 0.091(2) C5 0.0650(17) 0.084(2) 0.065(3) -0.013(2) -0.005(2) 0.0678(13) C6 0.0349(15) 0.091(2) 0.080(3) -0.042(2) -0.016(2) 0.0464(14) C7 0.057(2) 0.139(4) 0.085(4) -0.030(4) -0.027(3) 0.064(2) C8 0.034(2) 0.097(4) 0.121(5) -0.026(4) -0.010(3) 0.029(2) C9 0.043(2) 0.073(3) 0.123(5) -0.001(3) -0.009(3) 0.028(2) C10 0.0496(19) 0.070(2) 0.094(4) -0.008(3) -0.008(3) 0.0450(16) C11 0.0248(17) 0.0235(17) 0.080(3) 0.000(2) -0.012(2) 0.0084(13) C12 0.0242(15) 0.0330(18) 0.092(4) -0.005(2) -0.010(2) 0.0167(12) C13 0.0349(17) 0.0324(18) 0.047(2) -0.0040(19) 0.0020(19) 0.0129(14) C14 0.031(2) 0.051(2) 0.068(3) 0.000(2) 0.004(2) 0.0087(18) C15 0.0278(19) 0.069(3) 0.078(3) 0.002(3) 0.006(2) 0.0195(18) C16 0.0305(16) 0.053(2) 0.063(3) 0.000(2) -0.0014(19) 0.0238(14) C17 0.0316(15) 0.0387(17) 0.059(3) -0.0116(17) -0.0061(17) 0.0230(12) C18 0.0320(15) 0.0383(16) 0.052(3) -0.0021(17) -0.0002(18) 0.0252(12) C19 0.0572(18) 0.066(2) 0.049(3) -0.0064(19) -0.009(2) 0.0491(14) C20 0.063(2) 0.055(2) 0.051(3) 0.013(2) 0.001(2) 0.0395(16) C21 0.066(2) 0.0473(19) 0.056(3) 0.0137(18) 0.011(2) 0.0353(17) C22 0.0420(18) 0.0498(19) 0.049(2) 0.0095(19) 0.0016(18) 0.0279(14) C23 0.0134(14) 0.0272(16) 0.035(2) -0.0146(15) -0.0041(14) 0.0040(11) C24 0.0349(17) 0.0290(17) 0.038(2) 0.0009(16) 0.0067(17) 0.0117(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N11 1.863(4) 10_665 ? Co1 N11 1.863(4) . ? Co1 N1 1.922(4) 10_665 ? Co1 N1 1.922(4) . ? Co1 N2 1.928(3) . ? Co1 N2 1.928(3) 10_665 ? Co2 N23 1.879(3) 8_766 ? Co2 N23 1.879(3) . ? Co2 N5 1.919(3) 8_766 ? Co2 N5 1.919(3) . ? Co2 N4 1.949(4) 8_766 ? Co2 N4 1.949(4) . ? Fe1 C11 1.902(5) . ? Fe1 C11 1.902(5) 5_665 ? Fe1 C11 1.902(5) 3_655 ? Fe1 C12 1.918(5) . ? Fe1 C12 1.918(5) 3_655 ? Fe1 C12 1.918(5) 5_665 ? Fe2 C23 1.901(4) 3_645 ? Fe2 C23 1.901(4) 5_765 ? Fe2 C23 1.901(4) . ? Fe2 C24 1.914(5) 5_765 ? Fe2 C24 1.914(5) . ? Fe2 C24 1.914(5) 3_645 ? Fe1A Fe3A 0.526(12) . ? Fe1A Fe2A 0.856(4) . ? Fe1A C1A 1.690(12) 12 ? Fe1A C1A 1.690(12) 10_775 ? Fe1A C1A 1.690(12) 11_755 ? Fe1A Fe1A 1.711(7) 10_775 ? Fe1A C1A 1.974(12) 5_775 ? Fe1A C1A 1.974(12) . ? Fe1A C1A 1.974(12) 3_755 ? Fe1A C2A 2.053(15) . ? Fe1A C2A 2.053(15) 5_775 ? Fe1A C2A 2.053(15) 3_755 ? Fe2A Fe1A 0.856(4) 10_775 ? Fe2A Fe3A 1.381(12) . ? Fe2A Fe3A 1.381(12) 10_775 ? Fe2A C1A 1.626(12) 12 ? Fe2A C1A 1.626(12) 5_775 ? Fe2A C1A 1.626(12) 10_775 ? Fe2A C1A 1.626(12) . ? Fe2A C1A 1.626(12) 3_755 ? Fe2A C1A 1.626(12) 11_755 ? O8S O11S 1.676(13) 7_556 ? O11S O8S 1.676(13) 7_556 ? N1 C1 1.344(6) . ? N1 C5 1.347(5) . ? N2 C6 1.349(6) . ? N2 C10 1.359(7) . ? N4 C22 1.343(5) . ? N4 C18 1.347(5) . ? N5 C17 1.333(6) . ? N5 C13 1.339(5) . ? N11 C11 1.164(6) . ? N12 C12 1.138(6) . ? N23 C23 1.169(5) . ? N24 C24 1.166(6) . ? N1A C1A 1.142(19) . ? N1A C2A 1.80(2) 12 ? N1A C1A 1.85(2) 11_755 ? N2A C2A 1.19(2) . ? C1 C2 1.403(8) . ? C2 C3 1.417(7) . ? C3 C4 1.325(8) . ? C4 C5 1.381(8) . ? C5 C6 1.416(7) . ? C6 C7 1.392(6) . ? C7 C8 1.400(10) . ? C8 C9 1.370(9) . ? C9 C10 1.367(6) . ? C13 C14 1.354(6) . ? C14 C15 1.410(8) . ? C15 C16 1.362(6) . ? C16 C17 1.401(5) . ? C17 C18 1.448(5) . ? C18 C19 1.418(7) . ? C19 C20 1.364(6) . ? C20 C21 1.347(7) . ? C21 C22 1.376(7) . ? C1A C1A 0.98(3) 11_755 ? C1A Fe1A 1.690(12) 10_775 ? C1A N1A 1.85(2) 11_755 ? C1A Fe3A 1.927(14) 10_775 ? C1A C2A 2.00(2) 12 ? C1A Fe3A 2.323(15) . ? C2A Fe3A 1.782(16) . ? C2A N1A 1.80(2) 12 ? C2A C1A 2.00(2) 12 ? Fe3A C2A 1.782(16) 5_775 ? Fe3A C2A 1.782(16) 3_755 ? Fe3A C1A 1.927(14) 12 ? Fe3A C1A 1.927(14) 10_775 ? Fe3A C1A 1.927(14) 11_755 ? Fe3A Fe1A 2.237(13) 10_775 ? Fe3A C1A 2.323(15) 5_775 ? Fe3A C1A 2.323(15) 3_755 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Co1 N11 90.9(2) 10_665 . ? N11 Co1 N1 88.65(17) 10_665 10_665 ? N11 Co1 N1 177.46(13) . 10_665 ? N11 Co1 N1 177.46(13) 10_665 . ? N11 Co1 N1 88.65(17) . . ? N1 Co1 N1 91.9(2) 10_665 . ? N11 Co1 N2 94.70(15) 10_665 . ? N11 Co1 N2 89.06(15) . . ? N1 Co1 N2 93.47(16) 10_665 . ? N1 Co1 N2 82.80(16) . . ? N11 Co1 N2 89.06(15) 10_665 10_665 ? N11 Co1 N2 94.70(15) . 10_665 ? N1 Co1 N2 82.80(16) 10_665 10_665 ? N1 Co1 N2 93.47(16) . 10_665 ? N2 Co1 N2 174.7(3) . 10_665 ? N23 Co2 N23 88.54(19) 8_766 . ? N23 Co2 N5 94.54(13) 8_766 8_766 ? N23 Co2 N5 88.78(12) . 8_766 ? N23 Co2 N5 88.78(12) 8_766 . ? N23 Co2 N5 94.54(13) . . ? N5 Co2 N5 175.4(2) 8_766 . ? N23 Co2 N4 177.21(11) 8_766 8_766 ? N23 Co2 N4 90.61(13) . 8_766 ? N5 Co2 N4 82.78(13) 8_766 8_766 ? N5 Co2 N4 93.94(12) . 8_766 ? N23 Co2 N4 90.61(13) 8_766 . ? N23 Co2 N4 177.21(11) . . ? N5 Co2 N4 93.94(12) 8_766 . ? N5 Co2 N4 82.78(13) . . ? N4 Co2 N4 90.4(2) 8_766 . ? C11 Fe1 C11 87.3(2) . 5_665 ? C11 Fe1 C11 87.3(2) . 3_655 ? C11 Fe1 C11 87.3(2) 5_665 3_655 ? C11 Fe1 C12 88.0(2) . . ? C11 Fe1 C12 94.58(17) 5_665 . ? C11 Fe1 C12 174.81(18) 3_655 . ? C11 Fe1 C12 94.58(17) . 3_655 ? C11 Fe1 C12 174.81(17) 5_665 3_655 ? C11 Fe1 C12 88.0(2) 3_655 3_655 ? C12 Fe1 C12 90.3(2) . 3_655 ? C11 Fe1 C12 174.81(17) . 5_665 ? C11 Fe1 C12 88.0(2) 5_665 5_665 ? C11 Fe1 C12 94.58(17) 3_655 5_665 ? C12 Fe1 C12 90.3(2) . 5_665 ? C12 Fe1 C12 90.3(2) 3_655 5_665 ? C23 Fe2 C23 92.22(15) 3_645 5_765 ? C23 Fe2 C23 92.22(15) 3_645 . ? C23 Fe2 C23 92.22(15) 5_765 . ? C23 Fe2 C24 176.93(15) 3_645 5_765 ? C23 Fe2 C24 86.56(17) 5_765 5_765 ? C23 Fe2 C24 90.64(14) . 5_765 ? C23 Fe2 C24 90.64(14) 3_645 . ? C23 Fe2 C24 176.93(15) 5_765 . ? C23 Fe2 C24 86.56(17) . . ? C24 Fe2 C24 90.64(18) 5_765 . ? C23 Fe2 C24 86.56(17) 3_645 3_645 ? C23 Fe2 C24 90.64(14) 5_765 3_645 ? C23 Fe2 C24 176.93(15) . 3_645 ? C24 Fe2 C24 90.64(18) 5_765 3_645 ? C24 Fe2 C24 90.64(19) . 3_645 ? Fe3A Fe1A Fe2A 180.000(4) . . ? Fe3A Fe1A C1A 109.0(5) . 12 ? Fe2A Fe1A C1A 71.0(5) . 12 ? Fe3A Fe1A C1A 109.0(5) . 10_775 ? Fe2A Fe1A C1A 71.0(5) . 10_775 ? C1A Fe1A C1A 109.9(5) 12 10_775 ? Fe3A Fe1A C1A 109.0(5) . 11_755 ? Fe2A Fe1A C1A 71.0(5) . 11_755 ? C1A Fe1A C1A 109.9(5) 12 11_755 ? C1A Fe1A C1A 109.9(5) 10_775 11_755 ? Fe3A Fe1A Fe1A 180.000(4) . 10_775 ? Fe2A Fe1A Fe1A 0.000(1) . 10_775 ? C1A Fe1A Fe1A 71.0(5) 12 10_775 ? C1A Fe1A Fe1A 71.0(5) 10_775 10_775 ? C1A Fe1A Fe1A 71.0(5) 11_755 10_775 ? Fe3A Fe1A C1A 126.0(4) . 5_775 ? Fe2A Fe1A C1A 54.0(4) . 5_775 ? C1A Fe1A C1A 29.6(9) 12 5_775 ? C1A Fe1A C1A 80.8(9) 10_775 5_775 ? C1A Fe1A C1A 117.0(5) 11_755 5_775 ? Fe1A Fe1A C1A 54.0(4) 10_775 5_775 ? Fe3A Fe1A C1A 126.0(4) . . ? Fe2A Fe1A C1A 54.0(4) . . ? C1A Fe1A C1A 80.8(9) 12 . ? C1A Fe1A C1A 117.0(5) 10_775 . ? C1A Fe1A C1A 29.6(9) 11_755 . ? Fe1A Fe1A C1A 54.0(4) 10_775 . ? C1A Fe1A C1A 89.0(5) 5_775 . ? Fe3A Fe1A C1A 126.0(4) . 3_755 ? Fe2A Fe1A C1A 54.0(4) . 3_755 ? C1A Fe1A C1A 117.0(5) 12 3_755 ? C1A Fe1A C1A 29.6(9) 10_775 3_755 ? C1A Fe1A C1A 80.8(9) 11_755 3_755 ? Fe1A Fe1A C1A 54.0(4) 10_775 3_755 ? C1A Fe1A C1A 89.0(5) 5_775 3_755 ? C1A Fe1A C1A 89.0(5) . 3_755 ? Fe3A Fe1A C2A 52.5(4) . . ? Fe2A Fe1A C2A 127.5(4) . . ? C1A Fe1A C2A 63.8(6) 12 . ? C1A Fe1A C2A 148.9(6) 10_775 . ? C1A Fe1A C2A 100.4(7) 11_755 . ? Fe1A Fe1A C2A 127.5(4) 10_775 . ? C1A Fe1A C2A 91.6(6) 5_775 . ? C1A Fe1A C2A 92.7(5) . . ? C1A Fe1A C2A 178.3(6) 3_755 . ? Fe3A Fe1A C2A 52.5(4) . 5_775 ? Fe2A Fe1A C2A 127.5(4) . 5_775 ? C1A Fe1A C2A 100.4(7) 12 5_775 ? C1A Fe1A C2A 63.8(6) 10_775 5_775 ? C1A Fe1A C2A 148.9(6) 11_755 5_775 ? Fe1A Fe1A C2A 127.5(4) 10_775 5_775 ? C1A Fe1A C2A 92.7(5) 5_775 5_775 ? C1A Fe1A C2A 178.3(6) . 5_775 ? C1A Fe1A C2A 91.6(6) 3_755 5_775 ? C2A Fe1A C2A 86.8(6) . 5_775 ? Fe3A Fe1A C2A 52.5(4) . 3_755 ? Fe2A Fe1A C2A 127.5(4) . 3_755 ? C1A Fe1A C2A 148.9(6) 12 3_755 ? C1A Fe1A C2A 100.4(7) 10_775 3_755 ? C1A Fe1A C2A 63.8(6) 11_755 3_755 ? Fe1A Fe1A C2A 127.5(4) 10_775 3_755 ? C1A Fe1A C2A 178.3(6) 5_775 3_755 ? C1A Fe1A C2A 91.6(6) . 3_755 ? C1A Fe1A C2A 92.7(5) 3_755 3_755 ? C2A Fe1A C2A 86.8(6) . 3_755 ? C2A Fe1A C2A 86.8(6) 5_775 3_755 ? Fe1A Fe2A Fe1A 180.000(2) . 10_775 ? Fe1A Fe2A Fe3A 0.000(1) . . ? Fe1A Fe2A Fe3A 180.000(4) 10_775 . ? Fe1A Fe2A Fe3A 180.000(4) . 10_775 ? Fe1A Fe2A Fe3A 0.000(1) 10_775 10_775 ? Fe3A Fe2A Fe3A 180.000(4) . 10_775 ? Fe1A Fe2A C1A 79.2(5) . 12 ? Fe1A Fe2A C1A 100.8(5) 10_775 12 ? Fe3A Fe2A C1A 79.2(5) . 12 ? Fe3A Fe2A C1A 100.8(5) 10_775 12 ? Fe1A Fe2A C1A 100.8(5) . 5_775 ? Fe1A Fe2A C1A 79.2(5) 10_775 5_775 ? Fe3A Fe2A C1A 100.8(5) . 5_775 ? Fe3A Fe2A C1A 79.2(5) 10_775 5_775 ? C1A Fe2A C1A 35.0(10) 12 5_775 ? Fe1A Fe2A C1A 79.2(5) . 10_775 ? Fe1A Fe2A C1A 100.8(5) 10_775 10_775 ? Fe3A Fe2A C1A 79.2(5) . 10_775 ? Fe3A Fe2A C1A 100.8(5) 10_775 10_775 ? C1A Fe2A C1A 116.6(3) 12 10_775 ? C1A Fe2A C1A 94.3(11) 5_775 10_775 ? Fe1A Fe2A C1A 100.8(5) . . ? Fe1A Fe2A C1A 79.2(5) 10_775 . ? Fe3A Fe2A C1A 100.8(5) . . ? Fe3A Fe2A C1A 79.2(5) 10_775 . ? C1A Fe2A C1A 94.3(11) 12 . ? C1A Fe2A C1A 116.6(3) 5_775 . ? C1A Fe2A C1A 148.3(10) 10_775 . ? Fe1A Fe2A C1A 100.8(5) . 3_755 ? Fe1A Fe2A C1A 79.2(5) 10_775 3_755 ? Fe3A Fe2A C1A 100.8(5) . 3_755 ? Fe3A Fe2A C1A 79.2(5) 10_775 3_755 ? C1A Fe2A C1A 148.3(11) 12 3_755 ? C1A Fe2A C1A 116.6(3) 5_775 3_755 ? C1A Fe2A C1A 35.0(10) 10_775 3_755 ? C1A Fe2A C1A 116.6(3) . 3_755 ? Fe1A Fe2A C1A 79.2(5) . 11_755 ? Fe1A Fe2A C1A 100.8(5) 10_775 11_755 ? Fe3A Fe2A C1A 79.2(5) . 11_755 ? Fe3A Fe2A C1A 100.8(5) 10_775 11_755 ? C1A Fe2A C1A 116.6(3) 12 11_755 ? C1A Fe2A C1A 148.3(11) 5_775 11_755 ? C1A Fe2A C1A 116.6(3) 10_775 11_755 ? C1A Fe2A C1A 35.0(10) . 11_755 ? C1A Fe2A C1A 94.3(10) 3_755 11_755 ? C1 N1 C5 120.1(4) . . ? C1 N1 Co1 125.6(3) . . ? C5 N1 Co1 114.3(3) . . ? C6 N2 C10 120.1(4) . . ? C6 N2 Co1 113.1(3) . . ? C10 N2 Co1 126.8(3) . . ? C22 N4 C18 119.4(4) . . ? C22 N4 Co2 127.2(3) . . ? C18 N4 Co2 113.4(3) . . ? C17 N5 C13 118.7(3) . . ? C17 N5 Co2 114.8(2) . . ? C13 N5 Co2 126.4(3) . . ? C11 N11 Co1 164.9(3) . . ? C23 N23 Co2 161.9(3) . . ? C1A N1A C2A 82.4(13) . 12 ? C1A N1A C1A 26.7(10) . 11_755 ? C2A N1A C1A 104.4(10) 12 11_755 ? N1 C1 C2 121.0(4) . . ? C1 C2 C3 117.4(5) . . ? C4 C3 C2 119.9(5) . . ? C3 C4 C5 120.9(5) . . ? N1 C5 C4 120.7(5) . . ? N1 C5 C6 114.0(4) . . ? C4 C5 C6 125.2(4) . . ? N2 C6 C7 119.7(5) . . ? N2 C6 C5 115.6(3) . . ? C7 C6 C5 124.7(5) . . ? C6 C7 C8 119.0(5) . . ? C9 C8 C7 120.7(5) . . ? C10 C9 C8 117.7(6) . . ? N2 C10 C9 122.8(5) . . ? N11 C11 Fe1 171.7(3) . . ? N12 C12 Fe1 178.7(5) . . ? N5 C13 C14 123.5(5) . . ? C13 C14 C15 117.4(4) . . ? C16 C15 C14 120.4(4) . . ? C15 C16 C17 117.6(5) . . ? N5 C17 C16 122.2(4) . . ? N5 C17 C18 114.6(3) . . ? C16 C17 C18 123.2(4) . . ? N4 C18 C19 119.7(3) . . ? N4 C18 C17 114.3(4) . . ? C19 C18 C17 125.9(3) . . ? C20 C19 C18 119.4(4) . . ? C21 C20 C19 119.9(5) . . ? C20 C21 C22 119.8(4) . . ? N4 C22 C21 121.9(4) . . ? N23 C23 Fe2 172.4(3) . . ? N24 C24 Fe2 175.2(4) . . ? C1A C1A N1A 121.6(15) 11_755 . ? C1A C1A Fe2A 72.5(5) 11_755 . ? N1A C1A Fe2A 154.6(14) . . ? C1A C1A Fe1A 91.5(8) 11_755 10_775 ? N1A C1A Fe1A 124.7(13) . 10_775 ? Fe2A C1A Fe1A 29.8(2) . 10_775 ? C1A C1A N1A 31.7(9) 11_755 11_755 ? N1A C1A N1A 98.1(17) . 11_755 ? Fe2A C1A N1A 101.8(8) . 11_755 ? Fe1A C1A N1A 123.2(9) 10_775 11_755 ? C1A C1A Fe3A 101.1(11) 11_755 10_775 ? N1A C1A Fe3A 109.8(12) . 10_775 ? Fe2A C1A Fe3A 44.8(4) . 10_775 ? Fe1A C1A Fe3A 15.0(3) 10_775 10_775 ? N1A C1A Fe3A 132.0(9) 11_755 10_775 ? C1A C1A Fe1A 58.8(7) 11_755 . ? N1A C1A Fe1A 179.5(17) . . ? Fe2A C1A Fe1A 25.2(2) . . ? Fe1A C1A Fe1A 55.0(4) 10_775 . ? N1A C1A Fe1A 82.4(7) 11_755 . ? Fe3A C1A Fe1A 70.0(5) 10_775 . ? C1A C1A C2A 149.7(19) 11_755 12 ? N1A C1A C2A 63.2(12) . 12 ? Fe2A C1A C2A 93.8(8) . 12 ? Fe1A C1A C2A 67.0(7) 10_775 12 ? N1A C1A C2A 158.1(11) 11_755 12 ? Fe3A C1A C2A 53.9(6) 10_775 12 ? Fe1A C1A C2A 116.4(8) . 12 ? C1A C1A Fe3A 54.5(9) 11_755 . ? N1A C1A Fe3A 169.7(13) . . ? Fe2A C1A Fe3A 35.8(3) . . ? Fe1A C1A Fe3A 65.6(5) 10_775 . ? N1A C1A Fe3A 74.4(7) 11_755 . ? Fe3A C1A Fe3A 80.5(6) 10_775 . ? Fe1A C1A Fe3A 10.6(2) . . ? C2A C1A Fe3A 125.6(8) 12 . ? N2A C2A Fe3A 175.1(13) . . ? N2A C2A N1A 90.0(13) . 12 ? Fe3A C2A N1A 90.7(8) . 12 ? N2A C2A C1A 121.2(14) . 12 ? Fe3A C2A C1A 60.9(6) . 12 ? N1A C2A C1A 34.4(6) 12 12 ? N2A C2A Fe1A 170.0(14) . . ? Fe3A C2A Fe1A 13.5(4) . . ? N1A C2A Fe1A 81.4(7) 12 . ? C1A C2A Fe1A 49.2(5) 12 . ? Fe1A Fe3A Fe2A 0.000(1) . . ? Fe1A Fe3A C2A 114.0(6) . . ? Fe2A Fe3A C2A 114.0(6) . . ? Fe1A Fe3A C2A 114.0(6) . 5_775 ? Fe2A Fe3A C2A 114.0(6) . 5_775 ? C2A Fe3A C2A 104.6(7) . 5_775 ? Fe1A Fe3A C2A 114.0(6) . 3_755 ? Fe2A Fe3A C2A 114.0(6) . 3_755 ? C2A Fe3A C2A 104.6(7) . 3_755 ? C2A Fe3A C2A 104.6(7) 5_775 3_755 ? Fe1A Fe3A C1A 56.0(5) . 12 ? Fe2A Fe3A C1A 56.0(5) . 12 ? C2A Fe3A C1A 65.2(6) . 12 ? C2A Fe3A C1A 102.1(6) 5_775 12 ? C2A Fe3A C1A 153.1(7) 3_755 12 ? Fe1A Fe3A C1A 56.0(5) . 10_775 ? Fe2A Fe3A C1A 56.0(5) . 10_775 ? C2A Fe3A C1A 153.1(7) . 10_775 ? C2A Fe3A C1A 65.2(6) 5_775 10_775 ? C2A Fe3A C1A 102.1(7) 3_755 10_775 ? C1A Fe3A C1A 91.8(7) 12 10_775 ? Fe1A Fe3A C1A 56.0(5) . 11_755 ? Fe2A Fe3A C1A 56.0(5) . 11_755 ? C2A Fe3A C1A 102.1(7) . 11_755 ? C2A Fe3A C1A 153.1(7) 5_775 11_755 ? C2A Fe3A C1A 65.2(6) 3_755 11_755 ? C1A Fe3A C1A 91.8(7) 12 11_755 ? C1A Fe3A C1A 91.8(7) 10_775 11_755 ? Fe1A Fe3A Fe1A 0.000(2) . 10_775 ? Fe2A Fe3A Fe1A 0.0 . 10_775 ? C2A Fe3A Fe1A 114.0(6) . 10_775 ? C2A Fe3A Fe1A 114.0(6) 5_775 10_775 ? C2A Fe3A Fe1A 114.0(6) 3_755 10_775 ? C1A Fe3A Fe1A 56.0(5) 12 10_775 ? C1A Fe3A Fe1A 56.0(5) 10_775 10_775 ? C1A Fe3A Fe1A 56.0(5) 11_755 10_775 ? Fe1A Fe3A C1A 43.5(4) . 5_775 ? Fe2A Fe3A C1A 43.5(4) . 5_775 ? C2A Fe3A C1A 88.4(7) . 5_775 ? C2A Fe3A C1A 89.4(6) 5_775 5_775 ? C2A Fe3A C1A 157.4(8) 3_755 5_775 ? C1A Fe3A C1A 24.4(7) 12 5_775 ? C1A Fe3A C1A 67.5(8) 10_775 5_775 ? C1A Fe3A C1A 94.4(6) 11_755 5_775 ? Fe1A Fe3A C1A 43.5(4) 10_775 5_775 ? Fe1A Fe3A C1A 43.5(4) . . ? Fe2A Fe3A C1A 43.5(4) . . ? C2A Fe3A C1A 89.4(6) . . ? C2A Fe3A C1A 157.4(8) 5_775 . ? C2A Fe3A C1A 88.4(7) 3_755 . ? C1A Fe3A C1A 67.5(8) 12 . ? C1A Fe3A C1A 94.4(6) 10_775 . ? C1A Fe3A C1A 24.4(7) 11_755 . ? Fe1A Fe3A C1A 43.5(4) 10_775 . ? C1A Fe3A C1A 73.1(6) 5_775 . ? Fe1A Fe3A C1A 43.5(4) . 3_755 ? Fe2A Fe3A C1A 43.5(4) . 3_755 ? C2A Fe3A C1A 157.4(8) . 3_755 ? C2A Fe3A C1A 88.4(7) 5_775 3_755 ? C2A Fe3A C1A 89.4(6) 3_755 3_755 ? C1A Fe3A C1A 94.4(6) 12 3_755 ? C1A Fe3A C1A 24.4(7) 10_775 3_755 ? C1A Fe3A C1A 67.5(8) 11_755 3_755 ? Fe1A Fe3A C1A 43.5(4) 10_775 3_755 ? C1A Fe3A C1A 73.1(6) 5_775 3_755 ? C1A Fe3A C1A 73.1(6) . 3_755 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.741 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.121