data_CoFetmphen_110K #============================================================================== # 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 the Discrete Cyanide-bridged Complex: {[Co(tmphen)2]3[Fe(CN)6]2}.' ; 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 ; 'Galan-Mascaros, Jose-Ramon' ; Instituto de Ciencia Molecular Universidad de Valencia Spain ; '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 ; ? ; _chemical_name_common 'final110K' _chemical_formula_moiety ; {[Co(tmphen)2]3[Fe(CN)6]2}.13H2O ; _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_CoFetmphen_220K #============================================================================== # 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 'Inorganic Chemistry' _publ_requested_coeditor_name ? _publ_contact_letter ; ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; 'A Charge Transfer Induced Spin Transition in the Discrete Cyanide-bridged Complex: {[Co(tmphen)2]3[Fe(CN)6]2}.' ; 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 ; 'Galan-Mascaros, Jose-Ramon' ; Instituto de Ciencia Molecular Universidad de Valencia Spain ; '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 ; ? ; _chemical_name_common 'final220K' _chemical_melting_point ? _chemical_formula_moiety ; {[Co(tmphen)2]3[Fe(CN)6]2}.9H2O ; _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