_publ_contact_author ; 'Annie K. Powell' ; _publ_contact_author_email powell@aoc.uni-karlsruhe.de _publ_contact_author_phone '+44 721 608 2135' _publ_requested_journal 'Inorg. Chem.' _publ_section_title ; Odd-numbered Fe(III) Complexes: Synthesis, Molecular Structure, Reactivity, and Magnetic Properties ; loop_ _publ_author_name _publ_author_address 'Ako M. Ayuk' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Oliver Waldmann' ; Department of Chemistry and Biochemistry University of Berne Freiestrasse 3 CH-3012 Berne Switzerland ; 'Valeriu Mereacre' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Ian J. Hewitt' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Frederik Kl\"ower' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Christopher E. Anson' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Hans U. G\"udel' ; Department of Chemistry and Biochemistry University of Berne Freiestrasse 3 CH-3012 Berne Switzerland ; 'Annie K. Powell' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; ########################################################################### data_ako224 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H126 Fe7 N3 O33' _chemical_formula_weight 1844.62 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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 3 1 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, z+1/2' 'x-y, -y, z+1/2' '-x, -x+y, z+1/2' _cell_length_a 15.5804(8) _cell_length_b 15.5804(8) _cell_length_c 20.8694(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4387.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11090 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 27.96 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour brown _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1942 _exptl_absorpt_coefficient_mu 1.202 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.699 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16786 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5060 _reflns_number_gt 4823 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_data_reduction 'SAINT+ 6.0 (Bruker AXS Inc., 2000)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _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^)+(0.0608P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(14) _refine_ls_number_reflns 5060 _refine_ls_number_parameters 326 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.000 _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 Fe1 Fe 0.3333 0.6667 0.10611(4) 0.01896(17) Uani 1 3 d S . . Fe2 Fe 0.11407(3) 0.54118(3) 0.08966(2) 0.02121(12) Uani 1 1 d . . . Fe3 Fe 0.22631(3) 0.45407(3) 0.00468(2) 0.02094(12) Uani 1 1 d . . . O1 O 0.23153(16) 0.55917(16) 0.05055(12) 0.0207(5) Uani 1 1 d . . . N1 N 0.0142(2) 0.5594(2) 0.15845(14) 0.0255(6) Uani 1 1 d . . . C1 C 0.0661(3) 0.5767(3) 0.22028(16) 0.0271(7) Uani 1 1 d . . . H1A H 0.0551 0.5130 0.2378 0.032 Uiso 1 1 calc R . . H1B H 0.0391 0.6053 0.2512 0.032 Uiso 1 1 calc R . . C2 C 0.1770(3) 0.6477(3) 0.21121(17) 0.0295(8) Uani 1 1 d . . . H2A H 0.1895 0.7156 0.2034 0.035 Uiso 1 1 calc R . . H2B H 0.2134 0.6487 0.2504 0.035 Uiso 1 1 calc R . . O2 O 0.21005(16) 0.61586(17) 0.15908(11) 0.0232(5) Uani 1 1 d . . . C3 C 0.0106(3) 0.6490(3) 0.13628(17) 0.0273(7) Uani 1 1 d . . . H3A H 0.0627 0.7087 0.1583 0.033 Uiso 1 1 calc R . . H3B H -0.0545 0.6418 0.1472 0.033 Uiso 1 1 calc R . . C4 C 0.0264(3) 0.6607(3) 0.06469(17) 0.0273(8) Uani 1 1 d . . . H4A H -0.0304 0.6057 0.0422 0.033 Uiso 1 1 calc R . . H4B H 0.0319 0.7239 0.0505 0.033 Uiso 1 1 calc R . . O3 O 0.11658(16) 0.65994(17) 0.04990(12) 0.0229(5) Uani 1 1 d . . . C5 C -0.0868(3) 0.4703(3) 0.16056(19) 0.0312(8) Uani 1 1 d . . . H5A H -0.0793 0.4109 0.1587 0.037 Uiso 1 1 calc R . . H5B H -0.1224 0.4703 0.1212 0.037 Uiso 1 1 calc R . . C6 C -0.1523(3) 0.4587(3) 0.2174(2) 0.0373(9) Uani 1 1 d . . . H6A H -0.2145 0.3942 0.2142 0.045 Uiso 1 1 calc R . . H6B H -0.1181 0.4582 0.2573 0.045 Uiso 1 1 calc R . . O4 O -0.1757(2) 0.5353(2) 0.22124(14) 0.0402(7) Uani 1 1 d . . . H4 H -0.1624 0.5603 0.2581 0.060 Uiso 1 1 calc R . . O5 O 0.01038(17) 0.45667(17) 0.02428(11) 0.0261(5) Uani 1 1 d . . . O6 O 0.10444(17) 0.43738(18) -0.04883(12) 0.0275(5) Uani 1 1 d . . . C7 C 0.0250(2) 0.4327(2) -0.03111(16) 0.0229(7) Uani 1 1 d . . . C8 C -0.0618(3) 0.3962(3) -0.07836(17) 0.0286(8) Uani 1 1 d . . . C9 C -0.0427(3) 0.3506(3) -0.13837(18) 0.0364(9) Uani 1 1 d . . . H9A H -0.0987 0.3282 -0.1680 0.055 Uiso 1 1 calc R . . H9B H -0.0352 0.2941 -0.1258 0.055 Uiso 1 1 calc R . . H9C H 0.0181 0.4006 -0.1596 0.055 Uiso 1 1 calc R . . C10 C -0.0711(4) 0.4853(3) -0.0978(2) 0.0422(10) Uani 1 1 d . . . H10A H -0.1258 0.4644 -0.1283 0.063 Uiso 1 1 calc R . . H10B H -0.0092 0.5352 -0.1178 0.063 Uiso 1 1 calc R . . H10C H -0.0843 0.5137 -0.0597 0.063 Uiso 1 1 calc R . . C11 C -0.1566(3) 0.3178(3) -0.0450(2) 0.0460(11) Uani 1 1 d . . . H11A H -0.2125 0.2938 -0.0748 0.069 Uiso 1 1 calc R . . H11B H -0.1698 0.3473 -0.0074 0.069 Uiso 1 1 calc R . . H11C H -0.1482 0.2623 -0.0314 0.069 Uiso 1 1 calc R . . O7 O 0.07246(17) 0.40829(17) 0.13430(11) 0.0268(5) Uani 1 1 d . . . O8 O 0.12821(18) 0.34235(17) 0.06124(12) 0.0254(5) Uani 1 1 d . . . C12 C 0.0769(2) 0.3368(2) 0.10987(16) 0.0236(7) Uani 1 1 d . . . C13 C 0.0120(3) 0.2338(3) 0.13837(19) 0.0308(8) Uani 1 1 d . . . C14 C 0.0633(3) 0.1714(3) 0.1338(2) 0.0423(10) Uani 1 1 d . . . H14A H 0.1241 0.2023 0.1595 0.063 Uiso 1 1 calc R . . H14B H 0.0799 0.1676 0.0889 0.063 Uiso 1 1 calc R . . H14C H 0.0186 0.1044 0.1499 0.063 Uiso 1 1 calc R . . C15 C -0.0159(5) 0.2402(4) 0.2084(3) 0.0730(18) Uani 1 1 d . . . H15A H 0.0442 0.2718 0.2347 0.110 Uiso 1 1 calc R . . H15B H -0.0607 0.1734 0.2246 0.110 Uiso 1 1 calc R . . H15C H -0.0491 0.2796 0.2103 0.110 Uiso 1 1 calc R . . C16 C -0.0825(3) 0.1839(3) 0.0971(3) 0.0614(15) Uani 1 1 d . . . H16A H -0.0649 0.1792 0.0527 0.092 Uiso 1 1 calc R . . H16B H -0.1155 0.2234 0.0988 0.092 Uiso 1 1 calc R . . H16C H -0.1274 0.1173 0.1137 0.092 Uiso 1 1 calc R . . O9 O 0.21811(17) 0.34519(17) -0.05268(11) 0.0249(5) Uani 1 1 d . . . O10 O 0.27899(19) 0.40871(18) -0.14897(12) 0.0360(6) Uani 1 1 d . . . C17 C 0.2366(2) 0.3376(3) -0.11043(18) 0.0274(8) Uani 1 1 d . . . C18 C 0.2034(3) 0.2302(3) -0.13188(19) 0.0323(8) Uani 1 1 d . . . C19 C 0.0913(3) 0.1726(3) -0.1294(2) 0.0462(10) Uani 1 1 d . . . H19A H 0.0647 0.2005 -0.1604 0.069 Uiso 1 1 calc R . . H19B H 0.0691 0.1769 -0.0862 0.069 Uiso 1 1 calc R . . H19C H 0.0676 0.1030 -0.1400 0.069 Uiso 1 1 calc R . . C20 C 0.2398(5) 0.2266(4) -0.1990(3) 0.0728(18) Uani 1 1 d . . . H20A H 0.2132 0.2551 -0.2296 0.109 Uiso 1 1 calc R . . H20B H 0.2173 0.1577 -0.2107 0.109 Uiso 1 1 calc R . . H20C H 0.3124 0.2649 -0.2000 0.109 Uiso 1 1 calc R . . C21 C 0.2453(4) 0.1860(3) -0.0842(3) 0.0575(14) Uani 1 1 d . . . H21A H 0.2250 0.1178 -0.0968 0.086 Uiso 1 1 calc R . . H21B H 0.2201 0.1859 -0.0412 0.086 Uiso 1 1 calc R . . H21C H 0.3179 0.2258 -0.0841 0.086 Uiso 1 1 calc R . . O11 O 0.30879(18) 0.54915(17) -0.06993(12) 0.0258(5) Uani 1 1 d D . . H111 H 0.307(3) 0.509(3) -0.1043(16) 0.039 Uiso 1 1 d D . . H112 H 0.360(2) 0.597(2) -0.0621(18) 0.039 Uiso 1 1 d D . . 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 Fe1 0.0184(2) 0.0184(2) 0.0200(4) 0.000 0.000 0.00921(12) Fe2 0.0188(2) 0.0190(2) 0.0252(3) -0.00035(19) 0.00102(18) 0.00892(19) Fe3 0.0208(2) 0.0194(2) 0.0231(2) -0.0008(2) -0.00013(18) 0.0104(2) O1 0.0194(11) 0.0173(11) 0.0243(12) -0.0025(9) -0.0002(9) 0.0084(9) N1 0.0251(15) 0.0249(15) 0.0286(16) 0.0023(12) 0.0058(12) 0.0141(12) C1 0.0317(19) 0.0309(19) 0.0198(17) 0.0025(14) 0.0062(14) 0.0165(16) C2 0.0285(19) 0.0337(19) 0.0258(18) -0.0051(15) -0.0008(15) 0.0153(16) O2 0.0198(11) 0.0245(12) 0.0232(12) -0.0010(10) 0.0004(9) 0.0095(10) C3 0.0279(17) 0.0229(17) 0.0335(19) -0.0020(14) 0.0030(15) 0.0145(15) C4 0.0250(17) 0.0280(18) 0.032(2) 0.0020(15) 0.0029(15) 0.0157(15) O3 0.0185(11) 0.0219(12) 0.0297(13) 0.0039(10) 0.0021(9) 0.0112(10) C5 0.0308(19) 0.0291(18) 0.036(2) 0.0015(15) 0.0050(16) 0.0167(16) C6 0.0270(18) 0.037(2) 0.044(2) 0.0036(17) 0.0080(17) 0.0129(17) O4 0.0412(16) 0.0465(17) 0.0409(17) 0.0008(13) 0.0048(13) 0.0281(14) O5 0.0208(12) 0.0265(12) 0.0277(13) -0.0058(10) -0.0054(10) 0.0093(10) O6 0.0245(12) 0.0320(13) 0.0271(13) -0.0036(11) -0.0053(10) 0.0149(11) C7 0.0264(18) 0.0149(15) 0.0267(18) 0.0013(13) 0.0001(14) 0.0098(14) C8 0.0261(18) 0.0260(18) 0.032(2) -0.0034(15) -0.0049(15) 0.0116(15) C9 0.038(2) 0.038(2) 0.035(2) -0.0096(17) -0.0088(17) 0.0204(18) C10 0.053(3) 0.043(2) 0.040(2) -0.0087(18) -0.016(2) 0.031(2) C11 0.031(2) 0.048(3) 0.041(2) -0.005(2) -0.0081(18) 0.0060(19) O7 0.0276(13) 0.0221(12) 0.0287(13) 0.0020(10) 0.0040(10) 0.0110(10) O8 0.0244(12) 0.0183(11) 0.0295(14) 0.0013(10) 0.0036(10) 0.0077(10) C12 0.0213(16) 0.0222(17) 0.0241(17) 0.0002(14) -0.0017(14) 0.0085(14) C13 0.0307(19) 0.0261(19) 0.035(2) 0.0050(15) 0.0060(16) 0.0136(16) C14 0.039(2) 0.027(2) 0.064(3) 0.0161(19) 0.009(2) 0.0187(17) C15 0.115(5) 0.046(3) 0.057(3) 0.025(2) 0.045(3) 0.039(3) C16 0.028(2) 0.034(2) 0.111(4) 0.019(3) -0.004(3) 0.0070(18) O9 0.0278(12) 0.0222(12) 0.0261(14) -0.0047(10) -0.0016(10) 0.0136(10) O10 0.0396(15) 0.0276(14) 0.0342(15) 0.0015(11) 0.0067(12) 0.0117(12) C17 0.0201(16) 0.0263(18) 0.036(2) -0.0047(16) -0.0048(15) 0.0116(15) C18 0.0343(19) 0.0246(19) 0.037(2) -0.0098(15) 0.0007(16) 0.0143(16) C19 0.041(2) 0.026(2) 0.064(3) -0.0059(19) -0.006(2) 0.0118(18) C20 0.083(4) 0.039(3) 0.071(4) -0.020(2) 0.030(3) 0.011(3) C21 0.054(3) 0.033(2) 0.094(4) -0.024(2) -0.030(3) 0.028(2) O11 0.0238(12) 0.0201(12) 0.0287(13) -0.0016(10) 0.0025(10) 0.0074(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 Fe1 O1 2.002(2) 2_665 ? Fe1 O1 2.002(2) 3_565 ? Fe1 O1 2.002(2) . ? Fe1 O2 2.004(2) . ? Fe1 O2 2.004(2) 2_665 ? Fe1 O2 2.004(2) 3_565 ? Fe2 O1 1.892(2) . ? Fe2 O2 1.987(2) . ? Fe2 O3 2.010(2) . ? Fe2 O5 2.019(2) . ? Fe2 O7 2.057(2) . ? Fe2 N1 2.237(3) . ? Fe3 O1 1.863(2) . ? Fe3 O3 1.991(2) 2_665 ? Fe3 O8 2.025(2) . ? Fe3 O9 2.027(2) . ? Fe3 O11 2.090(2) . ? Fe3 O6 2.104(2) . ? N1 C1 1.474(5) . ? N1 C5 1.490(5) . ? N1 C3 1.499(4) . ? C1 C2 1.529(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.396(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.510(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.445(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O3 Fe3 1.991(2) 3_565 ? C5 C6 1.516(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.413(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O4 H4 0.8400 . ? O5 C7 1.270(4) . ? O6 C7 1.258(4) . ? C7 C8 1.535(5) . ? C8 C10 1.520(5) . ? C8 C11 1.535(5) . ? C8 C9 1.541(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? O7 C12 1.258(4) . ? O8 C12 1.268(4) . ? C12 C13 1.526(5) . ? C13 C16 1.540(6) . ? C13 C14 1.541(5) . ? C13 C15 1.542(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O9 C17 1.258(4) . ? O10 C17 1.256(4) . ? C17 C18 1.550(5) . ? C18 C19 1.514(6) . ? C18 C20 1.523(6) . ? C18 C21 1.530(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? O11 H111 0.94(2) . ? O11 H112 0.79(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 O1 Fe1 O1 89.83(10) 2_665 3_565 ? O1 Fe1 O1 89.83(10) 2_665 . ? O1 Fe1 O1 89.82(10) 3_565 . ? O1 Fe1 O2 162.19(9) 2_665 . ? O1 Fe1 O2 102.65(9) 3_565 . ? O1 Fe1 O2 77.71(9) . . ? O1 Fe1 O2 77.71(9) 2_665 2_665 ? O1 Fe1 O2 162.19(9) 3_565 2_665 ? O1 Fe1 O2 102.65(9) . 2_665 ? O2 Fe1 O2 92.51(9) . 2_665 ? O1 Fe1 O2 102.65(9) 2_665 3_565 ? O1 Fe1 O2 77.71(9) 3_565 3_565 ? O1 Fe1 O2 162.19(9) . 3_565 ? O2 Fe1 O2 92.51(9) . 3_565 ? O2 Fe1 O2 92.51(9) 2_665 3_565 ? O1 Fe2 O2 80.72(10) . . ? O1 Fe2 O3 96.51(10) . . ? O2 Fe2 O3 95.70(10) . . ? O1 Fe2 O5 101.79(10) . . ? O2 Fe2 O5 175.42(10) . . ? O3 Fe2 O5 87.84(10) . . ? O1 Fe2 O7 98.00(9) . . ? O2 Fe2 O7 91.45(10) . . ? O3 Fe2 O7 164.69(10) . . ? O5 Fe2 O7 84.43(10) . . ? O1 Fe2 N1 160.14(10) . . ? O2 Fe2 N1 79.94(10) . . ? O3 Fe2 N1 80.95(10) . . ? O5 Fe2 N1 97.81(11) . . ? O7 Fe2 N1 87.01(10) . . ? O1 Fe3 O3 95.25(10) . 2_665 ? O1 Fe3 O8 97.96(10) . . ? O3 Fe3 O8 91.30(10) 2_665 . ? O1 Fe3 O9 174.61(10) . . ? O3 Fe3 O9 88.84(9) 2_665 . ? O8 Fe3 O9 85.42(9) . . ? O1 Fe3 O11 91.07(10) . . ? O3 Fe3 O11 96.50(10) 2_665 . ? O8 Fe3 O11 167.49(10) . . ? O9 Fe3 O11 84.97(10) . . ? O1 Fe3 O6 91.23(10) . . ? O3 Fe3 O6 173.51(9) 2_665 . ? O8 Fe3 O6 87.51(10) . . ? O9 Fe3 O6 84.71(9) . . ? O11 Fe3 O6 83.64(10) . . ? Fe3 O1 Fe2 118.52(11) . . ? Fe3 O1 Fe1 134.50(12) . . ? Fe2 O1 Fe1 100.20(11) . . ? C1 N1 C5 111.8(3) . . ? C1 N1 C3 111.9(3) . . ? C5 N1 C3 111.2(3) . . ? C1 N1 Fe2 103.4(2) . . ? C5 N1 Fe2 112.3(2) . . ? C3 N1 Fe2 105.8(2) . . ? N1 C1 C2 110.0(3) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? O2 C2 C1 108.9(3) . . ? O2 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? O2 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C2 O2 Fe2 118.2(2) . . ? C2 O2 Fe1 137.7(2) . . ? Fe2 O2 Fe1 96.96(10) . . ? N1 C3 C4 109.8(3) . . ? N1 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? N1 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? O3 C4 C3 108.1(3) . . ? O3 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? O3 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? C4 O3 Fe3 120.7(2) . 3_565 ? C4 O3 Fe2 110.38(19) . . ? Fe3 O3 Fe2 128.53(11) 3_565 . ? N1 C5 C6 117.9(3) . . ? N1 C5 H5A 107.8 . . ? C6 C5 H5A 107.8 . . ? N1 C5 H5B 107.8 . . ? C6 C5 H5B 107.8 . . ? H5A C5 H5B 107.2 . . ? O4 C6 C5 112.7(3) . . ? O4 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? O4 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C6 O4 H4 109.5 . . ? C7 O5 Fe2 127.1(2) . . ? C7 O6 Fe3 130.7(2) . . ? O6 C7 O5 124.5(3) . . ? O6 C7 C8 119.4(3) . . ? O5 C7 C8 116.0(3) . . ? C10 C8 C11 110.8(3) . . ? C10 C8 C7 107.5(3) . . ? C11 C8 C7 108.8(3) . . ? C10 C8 C9 109.4(3) . . ? C11 C8 C9 109.4(3) . . ? C7 C8 C9 110.8(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 O7 Fe2 125.3(2) . . ? C12 O8 Fe3 134.8(2) . . ? O7 C12 O8 125.2(3) . . ? O7 C12 C13 118.2(3) . . ? O8 C12 C13 116.5(3) . . ? C12 C13 C16 106.1(3) . . ? C12 C13 C14 111.1(3) . . ? C16 C13 C14 108.3(4) . . ? C12 C13 C15 111.2(3) . . ? C16 C13 C15 109.4(4) . . ? C14 C13 C15 110.6(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 O9 Fe3 136.2(2) . . ? O10 C17 O9 125.1(3) . . ? O10 C17 C18 120.7(3) . . ? O9 C17 C18 114.2(3) . . ? C19 C18 C20 110.5(4) . . ? C19 C18 C21 109.7(4) . . ? C20 C18 C21 109.3(4) . . ? C19 C18 C17 107.1(3) . . ? C20 C18 C17 112.1(3) . . ? C21 C18 C17 108.2(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Fe3 O11 H111 107(2) . . ? Fe3 O11 H112 119(3) . . ? H111 O11 H112 117(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O10 0.84 2.00 2.826(4) 166.7 5_565 O11 H111 O10 0.94(2) 1.68(3) 2.590(4) 161(4) . O11 H112 O11 0.79(2) 2.20(3) 2.898(4) 146(4) 2_665 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.899 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.064 ########################################################################### data_188cx _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69.5 H138 Cl Fe7 N3 O30' _chemical_formula_weight 1922.23 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 63.351(3) _cell_length_b 10.4329(5) _cell_length_c 31.4090(16) _cell_angle_alpha 90.00 _cell_angle_beta 115.078(1) _cell_angle_gamma 90.00 _cell_volume 18802.3(16) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15332 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.91 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8120 _exptl_absorpt_coefficient_mu 1.150 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46786 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0676 _diffrn_reflns_limit_h_min -83 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.99 _reflns_number_total 21285 _reflns_number_gt 14323 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_data_reduction 'SAINT+ 6.0 (Bruker AXS Inc., 2000)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _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^)+(0.0317P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21285 _refine_ls_number_parameters 1044 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.002 _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 Fe1 Fe 0.128590(6) 0.02464(3) 0.497538(12) 0.01608(8) Uani 1 1 d . . . Fe2 Fe 0.148751(6) 0.05751(3) 0.428192(12) 0.01664(8) Uani 1 1 d . . . Fe3 Fe 0.101832(6) 0.22606(3) 0.397004(12) 0.01713(8) Uani 1 1 d . . . Fe4 Fe 0.077359(6) 0.04977(3) 0.463955(12) 0.01791(8) Uani 1 1 d . . . Fe5 Fe 0.103696(6) 0.22230(3) 0.556922(12) 0.01809(8) Uani 1 1 d . . . Fe6 Fe 0.159095(6) 0.05976(3) 0.598927(12) 0.01790(8) Uani 1 1 d . . . Fe7 Fe 0.178261(6) 0.22945(3) 0.536661(12) 0.01735(8) Uani 1 1 d . . . O1 O 0.12597(3) 0.13588(14) 0.44340(5) 0.0168(4) Uani 1 1 d . . . O2 O 0.10464(3) 0.13160(15) 0.50686(5) 0.0171(4) Uani 1 1 d . . . O3 O 0.15410(3) 0.13836(15) 0.54150(5) 0.0171(4) Uani 1 1 d . . . N1 N 0.17642(4) -0.08075(18) 0.43102(7) 0.0181(5) Uani 1 1 d . . . C1 C 0.16821(4) -0.2054(2) 0.44132(8) 0.0204(6) Uani 1 1 d . . . H1A H 0.1811 -0.2683 0.4519 0.024 Uiso 1 1 calc R . . H1B H 0.1554 -0.2390 0.4124 0.024 Uiso 1 1 calc R . . C2 C 0.15963(4) -0.1881(2) 0.47939(9) 0.0214(6) Uani 1 1 d . . . H2A H 0.1509 -0.2650 0.4812 0.026 Uiso 1 1 calc R . . H2B H 0.1730 -0.1756 0.5103 0.026 Uiso 1 1 calc R . . O4 O 0.14502(3) -0.07969(15) 0.46766(5) 0.0178(4) Uani 1 1 d . . . C3 C 0.19824(4) -0.0358(2) 0.47026(8) 0.0208(6) Uani 1 1 d . . . H3A H 0.2118 -0.0602 0.4642 0.025 Uiso 1 1 calc R . . H3B H 0.2000 -0.0769 0.5000 0.025 Uiso 1 1 calc R . . C4 C 0.19746(4) 0.1078(2) 0.47468(9) 0.0209(6) Uani 1 1 d . . . H4A H 0.2113 0.1378 0.5025 0.025 Uiso 1 1 calc R . . H4B H 0.1974 0.1498 0.4464 0.025 Uiso 1 1 calc R . . O5 O 0.17664(3) 0.13950(15) 0.47958(5) 0.0189(4) Uani 1 1 d . . . C5 C 0.17881(5) -0.0850(2) 0.38576(9) 0.0225(6) Uani 1 1 d . . . H5A H 0.1854 -0.0021 0.3817 0.027 Uiso 1 1 calc R . . H5B H 0.1630 -0.0928 0.3598 0.027 Uiso 1 1 calc R . . C6 C 0.19387(5) -0.1921(2) 0.38068(9) 0.0256(6) Uani 1 1 d . . . H6A H 0.1863 -0.2755 0.3802 0.031 Uiso 1 1 calc R . . H6B H 0.2092 -0.1914 0.4083 0.031 Uiso 1 1 calc R . . C7 C 0.19772(5) -0.1795(3) 0.33608(10) 0.0353(7) Uani 1 1 d . . . H7A H 0.2055 -0.0965 0.3369 0.042 Uiso 1 1 calc R . . H7B H 0.2084 -0.2484 0.3358 0.042 Uiso 1 1 calc R . . C8 C 0.17551(6) -0.1869(3) 0.29077(10) 0.0477(9) Uani 1 1 d . . . H8A H 0.1793 -0.1774 0.2638 0.072 Uiso 1 1 calc R . . H8B H 0.1649 -0.1181 0.2903 0.072 Uiso 1 1 calc R . . H8C H 0.1680 -0.2701 0.2890 0.072 Uiso 1 1 calc R . . N2 N 0.05465(4) -0.09098(19) 0.41047(7) 0.0200(5) Uani 1 1 d . . . C9 C 0.06749(4) -0.2145(2) 0.42548(9) 0.0226(6) Uani 1 1 d . . . H9A H 0.0613 -0.2771 0.3994 0.027 Uiso 1 1 calc R . . H9B H 0.0652 -0.2500 0.4524 0.027 Uiso 1 1 calc R . . C10 C 0.09333(4) -0.1932(2) 0.43952(9) 0.0225(6) Uani 1 1 d . . . H10A H 0.1023 -0.2695 0.4563 0.027 Uiso 1 1 calc R . . H10B H 0.0962 -0.1788 0.4112 0.027 Uiso 1 1 calc R . . O6 O 0.10036(3) -0.08483(15) 0.46913(5) 0.0181(4) Uani 1 1 d . . . C11 C 0.05362(5) -0.0453(2) 0.36486(8) 0.0236(6) Uani 1 1 d . . . H11A H 0.0387 -0.0720 0.3390 0.028 Uiso 1 1 calc R . . H11B H 0.0665 -0.0838 0.3593 0.028 Uiso 1 1 calc R . . C12 C 0.05560(4) 0.0986(2) 0.36558(8) 0.0230(6) Uani 1 1 d . . . H12A H 0.0563 0.1293 0.3364 0.028 Uiso 1 1 calc R . . H12B H 0.0419 0.1380 0.3678 0.028 Uiso 1 1 calc R . . O7 O 0.07644(3) 0.13344(15) 0.40555(5) 0.0191(4) Uani 1 1 d . . . C13 C 0.03120(4) -0.0991(2) 0.41017(9) 0.0233(6) Uani 1 1 d . . . H13A H 0.0234 -0.0149 0.4001 0.028 Uiso 1 1 calc R . . H13B H 0.0332 -0.1140 0.4428 0.028 Uiso 1 1 calc R . . C14 C 0.01488(5) -0.2024(2) 0.37883(9) 0.0268(6) Uani 1 1 d . . . H14A H 0.0129 -0.1902 0.3461 0.032 Uiso 1 1 calc R . . H14B H 0.0219 -0.2878 0.3895 0.032 Uiso 1 1 calc R . . C15 C -0.00878(5) -0.1972(3) 0.38010(10) 0.0369(7) Uani 1 1 d . . . H15A H -0.0068 -0.2170 0.4124 0.044 Uiso 1 1 calc R . . H15B H -0.0150 -0.1091 0.3724 0.044 Uiso 1 1 calc R . . C16 C -0.02623(5) -0.2900(3) 0.34612(11) 0.0489(9) Uani 1 1 d . . . H16A H -0.0411 -0.2822 0.3484 0.073 Uiso 1 1 calc R . . H16B H -0.0204 -0.3778 0.3540 0.073 Uiso 1 1 calc R . . H16C H -0.0285 -0.2700 0.3140 0.073 Uiso 1 1 calc R . . N3 N 0.15595(4) -0.07717(19) 0.65076(7) 0.0209(5) Uani 1 1 d . . . C17 C 0.15161(5) -0.2029(2) 0.62594(8) 0.0228(6) Uani 1 1 d . . . H17A H 0.1453 -0.2648 0.6415 0.027 Uiso 1 1 calc R . . H17B H 0.1664 -0.2377 0.6273 0.027 Uiso 1 1 calc R . . C18 C 0.13423(5) -0.1853(2) 0.57478(8) 0.0231(6) Uani 1 1 d . . . H18A H 0.1337 -0.2636 0.5565 0.028 Uiso 1 1 calc R . . H18B H 0.1184 -0.1693 0.5729 0.028 Uiso 1 1 calc R . . O8 O 0.14157(3) -0.08002(15) 0.55640(5) 0.0186(4) Uani 1 1 d . . . C19 C 0.13554(5) -0.0336(2) 0.65881(9) 0.0249(6) Uani 1 1 d . . . H19A H 0.1380 -0.0545 0.6913 0.030 Uiso 1 1 calc R . . H19B H 0.1213 -0.0784 0.6369 0.030 Uiso 1 1 calc R . . C20 C 0.13248(5) 0.1093(2) 0.65104(8) 0.0246(6) Uani 1 1 d . . . H20A H 0.1179 0.1374 0.6525 0.030 Uiso 1 1 calc R . . H20B H 0.1457 0.1552 0.6757 0.030 Uiso 1 1 calc R . . O9 O 0.13164(3) 0.13747(15) 0.60588(5) 0.0195(4) Uani 1 1 d . . . C21 C 0.17796(5) -0.0775(2) 0.69490(8) 0.0261(6) Uani 1 1 d . B . H21A H 0.1902 -0.0190 0.6993 0.031 Uiso 1 1 calc R . . C22 C 0.18012(5) -0.1740(3) 0.73242(9) 0.0359(7) Uani 1 1 d . . . H22A H 0.1769 -0.2613 0.7189 0.043 Uiso 0.65 1 calc PR A 1 H22B H 0.1688 -0.1541 0.7456 0.043 Uiso 0.65 1 calc PR A 1 H22C H 0.1653 -0.1745 0.7348 0.043 Uiso 0.35 1 d PR A 2 H22D H 0.1817 -0.2574 0.7205 0.043 Uiso 0.35 1 d PR A 2 C23A C 0.20619(10) -0.1662(6) 0.77290(17) 0.0361(13) Uani 0.65 1 d P B 1 H23A H 0.2170 -0.2036 0.7610 0.043 Uiso 0.65 1 calc PR B 1 H23B H 0.2105 -0.0752 0.7806 0.043 Uiso 0.65 1 calc PR B 1 C24A C 0.20890(9) -0.2360(5) 0.81685(15) 0.0467(14) Uani 0.65 1 d P B 1 H24A H 0.2250 -0.2272 0.8407 0.070 Uiso 0.65 1 calc PR B 1 H24B H 0.2053 -0.3270 0.8097 0.070 Uiso 0.65 1 calc PR B 1 H24C H 0.1982 -0.1994 0.8288 0.070 Uiso 0.65 1 calc PR B 1 C23B C 0.19765(17) -0.1644(11) 0.7777(4) 0.029(3) Uiso 0.35 1 d P B 2 H23C H 0.1985 -0.2460 0.7944 0.034 Uiso 0.35 1 calc PR B 2 H23D H 0.1935 -0.0959 0.7946 0.034 Uiso 0.35 1 calc PR B 2 C24B C 0.22133(18) -0.1357(9) 0.7797(3) 0.046(3) Uiso 0.35 1 d P B 2 H24D H 0.2327 -0.1277 0.8126 0.069 Uiso 0.35 1 calc PR B 2 H24E H 0.2207 -0.0552 0.7632 0.069 Uiso 0.35 1 calc PR B 2 H24F H 0.2260 -0.2054 0.7647 0.069 Uiso 0.35 1 calc PR B 2 O10 O 0.12707(3) -0.03345(15) 0.36745(5) 0.0202(4) Uani 1 1 d . . . O11 O 0.09798(3) 0.11049(15) 0.34154(5) 0.0213(4) Uani 1 1 d . . . C25 C 0.10866(4) 0.0139(2) 0.33628(8) 0.0191(6) Uani 1 1 d . . . C26 C 0.09878(5) -0.0483(2) 0.28740(8) 0.0235(6) Uani 1 1 d . . . C27 C 0.10467(6) -0.1907(3) 0.29193(10) 0.0480(9) Uani 1 1 d . . . H27A H 0.0969 -0.2333 0.3091 0.072 Uiso 1 1 calc R . . H27B H 0.1216 -0.2017 0.3091 0.072 Uiso 1 1 calc R . . H27C H 0.0994 -0.2285 0.2605 0.072 Uiso 1 1 calc R . . C28 C 0.07267(5) -0.0291(3) 0.26178(10) 0.0405(8) Uani 1 1 d . . . H28A H 0.0650 -0.0726 0.2790 0.061 Uiso 1 1 calc R . . H28B H 0.0671 -0.0649 0.2300 0.061 Uiso 1 1 calc R . . H28C H 0.0691 0.0628 0.2598 0.061 Uiso 1 1 calc R . . C29 C 0.11103(6) 0.0185(3) 0.26054(10) 0.0428(8) Uani 1 1 d . . . H29A H 0.1054 -0.0175 0.2288 0.064 Uiso 1 1 calc R . . H29B H 0.1279 0.0051 0.2772 0.064 Uiso 1 1 calc R . . H29C H 0.1076 0.1105 0.2585 0.064 Uiso 1 1 calc R . . O12 O 0.15239(3) 0.18887(15) 0.38394(6) 0.0218(4) Uani 1 1 d . . . O13 O 0.12581(3) 0.33272(16) 0.38251(6) 0.0235(4) Uani 1 1 d . . . C30 C 0.14278(4) 0.2987(2) 0.37465(8) 0.0197(6) Uani 1 1 d . . . C31 C 0.15291(5) 0.3950(2) 0.35124(9) 0.0227(6) Uani 1 1 d . . . C32 C 0.14909(5) 0.3388(3) 0.30347(9) 0.0365(7) Uani 1 1 d . . . H32A H 0.1573 0.2568 0.3082 0.055 Uiso 1 1 calc R . . H32B H 0.1551 0.3984 0.2872 0.055 Uiso 1 1 calc R . . H32C H 0.1324 0.3251 0.2845 0.055 Uiso 1 1 calc R . . C33 C 0.14026(5) 0.5234(2) 0.34385(11) 0.0367(7) Uani 1 1 d . . . H33A H 0.1427 0.5594 0.3744 0.055 Uiso 1 1 calc R . . H33B H 0.1236 0.5105 0.3247 0.055 Uiso 1 1 calc R . . H33C H 0.1464 0.5827 0.3277 0.055 Uiso 1 1 calc R . . C34 C 0.17876(5) 0.4127(3) 0.38223(10) 0.0363(7) Uani 1 1 d . . . H34A H 0.1808 0.4490 0.4125 0.054 Uiso 1 1 calc R . . H34B H 0.1855 0.4710 0.3668 0.054 Uiso 1 1 calc R . . H34C H 0.1866 0.3295 0.3874 0.054 Uiso 1 1 calc R . . O14 O 0.06883(3) -0.04228(15) 0.51180(6) 0.0228(4) Uani 1 1 d . . . O15 O 0.08215(3) 0.10057(16) 0.57083(6) 0.0231(4) Uani 1 1 d . . . C35 C 0.07012(4) 0.0032(2) 0.55003(9) 0.0214(6) Uani 1 1 d . . . C36 C 0.05523(5) -0.0602(2) 0.57165(9) 0.0256(6) Uani 1 1 d . . . C37 C 0.03131(5) 0.0042(3) 0.54787(10) 0.0398(8) Uani 1 1 d . . . H37A H 0.0329 0.0960 0.5551 0.060 Uiso 1 1 calc R . . H37B H 0.0207 -0.0343 0.5595 0.060 Uiso 1 1 calc R . . H37C H 0.0251 -0.0079 0.5138 0.060 Uiso 1 1 calc R . . C38 C 0.05273(5) -0.2031(3) 0.56043(10) 0.0373(8) Uani 1 1 d . . . H38A H 0.0680 -0.2444 0.5756 0.056 Uiso 1 1 calc R . . H38B H 0.0465 -0.2152 0.5263 0.056 Uiso 1 1 calc R . . H38C H 0.0421 -0.2415 0.5721 0.056 Uiso 1 1 calc R . . C39 C 0.06553(5) -0.0379(3) 0.62473(9) 0.0354(7) Uani 1 1 d . . . H39A H 0.0669 0.0544 0.6311 0.053 Uiso 1 1 calc R . . H39B H 0.0810 -0.0778 0.6396 0.053 Uiso 1 1 calc R . . H39C H 0.0553 -0.0760 0.6375 0.053 Uiso 1 1 calc R . . O16 O 0.05228(3) 0.17620(16) 0.46031(6) 0.0238(4) Uani 1 1 d . . . O17 O 0.07405(3) 0.32289(16) 0.51238(6) 0.0242(4) Uani 1 1 d . . . C40 C 0.05547(4) 0.2861(2) 0.47964(9) 0.0216(6) Uani 1 1 d . C . C41 C 0.03470(5) 0.3782(2) 0.46085(10) 0.0284(6) Uani 1 1 d . . . C42A C 0.04018(10) 0.5039(5) 0.48635(19) 0.0426(14) Uiso 0.65 1 d P C 1 H42A H 0.0259 0.5411 0.4857 0.064 Uiso 0.65 1 calc PR C 1 H42B H 0.0469 0.5625 0.4710 0.064 Uiso 0.65 1 calc PR C 1 H42C H 0.0514 0.4902 0.5190 0.064 Uiso 0.65 1 calc PR C 1 C43A C 0.01394(10) 0.3162(5) 0.4621(2) 0.0563(15) Uiso 0.65 1 d P C 1 H43A H 0.0038 0.2840 0.4308 0.084 Uiso 0.65 1 calc PR C 1 H43B H 0.0054 0.3789 0.4720 0.084 Uiso 0.65 1 calc PR C 1 H43C H 0.0189 0.2447 0.4845 0.084 Uiso 0.65 1 calc PR C 1 C44A C 0.02956(10) 0.4061(5) 0.40813(17) 0.0497(14) Uiso 0.65 1 d P C 1 H44A H 0.0442 0.4272 0.4060 0.075 Uiso 0.65 1 calc PR C 1 H44B H 0.0187 0.4784 0.3965 0.075 Uiso 0.65 1 calc PR C 1 H44C H 0.0226 0.3300 0.3890 0.075 Uiso 0.65 1 calc PR C 1 C42B C 0.02093(16) 0.3419(9) 0.4948(3) 0.043(2) Uiso 0.35 1 d P C 2 H42D H 0.0324 0.3353 0.5277 0.065 Uiso 0.35 1 calc PR C 2 H42E H 0.0128 0.2600 0.4846 0.065 Uiso 0.35 1 calc PR C 2 H42F H 0.0096 0.4094 0.4919 0.065 Uiso 0.35 1 calc PR C 2 C43B C 0.04337(18) 0.5129(9) 0.4704(3) 0.038(2) Uiso 0.35 1 d P C 2 H43D H 0.0455 0.5377 0.5021 0.057 Uiso 0.35 1 calc PR C 2 H43E H 0.0320 0.5702 0.4473 0.057 Uiso 0.35 1 calc PR C 2 H43F H 0.0583 0.5192 0.4682 0.057 Uiso 0.35 1 calc PR C 2 C44B C 0.01834(17) 0.3518(9) 0.4128(3) 0.047(2) Uiso 0.35 1 d P C 2 H44D H 0.0255 0.3736 0.3915 0.071 Uiso 0.35 1 calc PR C 2 H44E H 0.0042 0.4034 0.4049 0.071 Uiso 0.35 1 calc PR C 2 H44F H 0.0142 0.2606 0.4096 0.071 Uiso 0.35 1 calc PR C 2 O18 O 0.19026(3) -0.02971(15) 0.61192(6) 0.0218(4) Uani 1 1 d . . . O19 O 0.20492(3) 0.11327(16) 0.57830(6) 0.0242(4) Uani 1 1 d . . . C45 C 0.20661(5) 0.0178(2) 0.60445(9) 0.0226(6) Uani 1 1 d . . . C46 C 0.23112(5) -0.0383(3) 0.63098(10) 0.0320(7) Uani 1 1 d . . . C47 C 0.24503(5) -0.0303(3) 0.60162(11) 0.0416(8) Uani 1 1 d . . . H47A H 0.2378 -0.0853 0.5739 0.062 Uiso 1 1 calc R . . H47B H 0.2610 -0.0590 0.6205 0.062 Uiso 1 1 calc R . . H47C H 0.2452 0.0585 0.5916 0.062 Uiso 1 1 calc R . . C48 C 0.24256(6) 0.0485(3) 0.67481(11) 0.0578(10) Uani 1 1 d . . . H48A H 0.2336 0.0432 0.6937 0.087 Uiso 1 1 calc R . . H48B H 0.2427 0.1374 0.6648 0.087 Uiso 1 1 calc R . . H48C H 0.2586 0.0199 0.6936 0.087 Uiso 1 1 calc R . . C49 C 0.22996(6) -0.1752(3) 0.64627(13) 0.0571(10) Uani 1 1 d . . . H49A H 0.2227 -0.2299 0.6185 0.086 Uiso 1 1 calc R . . H49B H 0.2207 -0.1778 0.6646 0.086 Uiso 1 1 calc R . . H49C H 0.2458 -0.2061 0.6657 0.086 Uiso 1 1 calc R . . O20 O 0.17950(3) 0.19250(16) 0.64547(5) 0.0228(4) Uani 1 1 d . . . O21 O 0.18359(3) 0.33607(16) 0.59657(6) 0.0248(4) Uani 1 1 d . . . C50 C 0.18545(4) 0.3007(2) 0.63643(9) 0.0221(6) Uani 1 1 d . D . C51 C 0.19549(5) 0.3966(2) 0.67727(9) 0.0301(7) Uani 1 1 d D . . C52A C 0.20518(8) 0.5136(3) 0.66384(13) 0.0460(10) Uani 0.86 1 d P D 1 H52A H 0.2179 0.4883 0.6556 0.069 Uiso 0.86 1 calc PR D 1 H52B H 0.2111 0.5734 0.6904 0.069 Uiso 0.86 1 calc PR D 1 H52C H 0.1928 0.5554 0.6368 0.069 Uiso 0.86 1 calc PR D 1 C53A C 0.17482(7) 0.4367(3) 0.68934(13) 0.0428(10) Uani 0.86 1 d P D 1 H53A H 0.1804 0.4987 0.7152 0.064 Uiso 0.86 1 calc PR D 1 H53B H 0.1687 0.3607 0.6988 0.064 Uiso 0.86 1 calc PR D 1 H53C H 0.1624 0.4756 0.6616 0.064 Uiso 0.86 1 calc PR D 1 C54A C 0.21385(7) 0.3270(3) 0.71966(12) 0.0498(11) Uani 0.86 1 d P D 1 H54A H 0.2269 0.3016 0.7125 0.075 Uiso 0.86 1 calc PR D 1 H54B H 0.2069 0.2506 0.7266 0.075 Uiso 0.86 1 calc PR D 1 H54C H 0.2195 0.3843 0.7470 0.075 Uiso 0.86 1 calc PR D 1 C52B C 0.2222(3) 0.400(2) 0.6867(8) 0.060(7) Uiso 0.14 1 d PD D 2 H52D H 0.2235 0.4219 0.6576 0.090 Uiso 0.14 1 calc PR D 2 H52E H 0.2292 0.3152 0.6975 0.090 Uiso 0.14 1 calc PR D 2 H52F H 0.2304 0.4639 0.7108 0.090 Uiso 0.14 1 calc PR D 2 C53B C 0.1940(4) 0.373(2) 0.7193(7) 0.060(7) Uiso 0.14 1 d PD D 2 H53D H 0.2002 0.2878 0.7308 0.089 Uiso 0.14 1 calc PR D 2 H53E H 0.1777 0.3781 0.7143 0.089 Uiso 0.14 1 calc PR D 2 H53F H 0.2031 0.4377 0.7425 0.089 Uiso 0.14 1 calc PR D 2 C54B C 0.1879(5) 0.5278(19) 0.6569(9) 0.076(10) Uiso 0.14 1 d PD D 2 H54D H 0.1894 0.5348 0.6271 0.114 Uiso 0.14 1 calc PR D 2 H54E H 0.1978 0.5925 0.6789 0.114 Uiso 0.14 1 calc PR D 2 H54F H 0.1717 0.5418 0.6513 0.114 Uiso 0.14 1 calc PR D 2 O22 O 0.07763(3) 0.33474(16) 0.34638(5) 0.0221(4) Uani 1 1 d . . . O23 O 0.07466(4) 0.51879(19) 0.37880(7) 0.0513(7) Uani 1 1 d . . . C55 C 0.06945(5) 0.4471(2) 0.34442(9) 0.0263(6) Uani 1 1 d . . . C56 C 0.05211(5) 0.4904(3) 0.29557(9) 0.0288(7) Uani 1 1 d . . . C57 C 0.06542(6) 0.4977(3) 0.26456(10) 0.0418(8) Uani 1 1 d . . . H57A H 0.0719 0.4133 0.2634 0.063 Uiso 1 1 calc R . . H57B H 0.0781 0.5604 0.2778 0.063 Uiso 1 1 calc R . . H57C H 0.0547 0.5241 0.2327 0.063 Uiso 1 1 calc R . . C58 C 0.04173(6) 0.6201(3) 0.29769(11) 0.0583(11) Uani 1 1 d . . . H58A H 0.0332 0.6137 0.3173 0.087 Uiso 1 1 calc R . . H58B H 0.0311 0.6468 0.2659 0.087 Uiso 1 1 calc R . . H58C H 0.0543 0.6833 0.3113 0.087 Uiso 1 1 calc R . . C59 C 0.03299(5) 0.3907(3) 0.27556(11) 0.0505(9) Uani 1 1 d . . . H59A H 0.0245 0.3853 0.2953 0.076 Uiso 1 1 calc R . . H59B H 0.0399 0.3071 0.2749 0.076 Uiso 1 1 calc R . . H59C H 0.0222 0.4152 0.2436 0.076 Uiso 1 1 calc R . . O24 O 0.10210(3) 0.33635(15) 0.60758(6) 0.0219(4) Uani 1 1 d . . . O25 O 0.11859(4) 0.52331(17) 0.60501(7) 0.0346(5) Uani 1 1 d . . . C60 C 0.10804(5) 0.4519(2) 0.62067(9) 0.0227(6) Uani 1 1 d . . . C61 C 0.10096(5) 0.4981(2) 0.65914(9) 0.0262(6) Uani 1 1 d . . . C62 C 0.10848(5) 0.6376(2) 0.67260(9) 0.0313(7) Uani 1 1 d . . . H62A H 0.1037 0.6653 0.6971 0.047 Uiso 1 1 calc R . . H62B H 0.1011 0.6925 0.6449 0.047 Uiso 1 1 calc R . . H62C H 0.1255 0.6441 0.6845 0.047 Uiso 1 1 calc R . . C63 C 0.07451(6) 0.4882(3) 0.64027(12) 0.0468(9) Uani 1 1 d . . . H63A H 0.0697 0.3990 0.6318 0.070 Uiso 1 1 calc R . . H63B H 0.0672 0.5425 0.6124 0.070 Uiso 1 1 calc R . . H63C H 0.0696 0.5166 0.6645 0.070 Uiso 1 1 calc R . . C64 C 0.11244(6) 0.4131(3) 0.70216(10) 0.0462(9) Uani 1 1 d . . . H64A H 0.1074 0.3242 0.6937 0.069 Uiso 1 1 calc R . . H64B H 0.1079 0.4418 0.7268 0.069 Uiso 1 1 calc R . . H64C H 0.1294 0.4186 0.7138 0.069 Uiso 1 1 calc R . . O26 O 0.20410(3) 0.34090(15) 0.53508(6) 0.0213(4) Uani 1 1 d . . . O27 O 0.18832(3) 0.52540(17) 0.50089(7) 0.0333(5) Uani 1 1 d . . . C65 C 0.20534(4) 0.4535(2) 0.52101(8) 0.0204(6) Uani 1 1 d . E . C66 C 0.22981(5) 0.4973(2) 0.52942(9) 0.0255(6) Uani 1 1 d . . . C67A C 0.24561(9) 0.4841(5) 0.58158(17) 0.0485(14) Uiso 0.65 1 d P E 1 H67A H 0.2405 0.5437 0.5995 0.073 Uiso 0.65 1 calc PR E 1 H67B H 0.2617 0.5040 0.5872 0.073 Uiso 0.65 1 calc PR E 1 H67C H 0.2448 0.3961 0.5917 0.073 Uiso 0.65 1 calc PR E 1 C68A C 0.23011(9) 0.6313(5) 0.51232(18) 0.0442(13) Uiso 0.65 1 d P E 1 H68A H 0.2251 0.6913 0.5302 0.066 Uiso 0.65 1 calc PR E 1 H68B H 0.2195 0.6370 0.4789 0.066 Uiso 0.65 1 calc PR E 1 H68C H 0.2460 0.6532 0.5168 0.066 Uiso 0.65 1 calc PR E 1 C69A C 0.23788(10) 0.4052(5) 0.50069(18) 0.0504(14) Uiso 0.65 1 d P E 1 H69A H 0.2325 0.3181 0.5025 0.076 Uiso 0.65 1 calc PR E 1 H69B H 0.2549 0.4061 0.5135 0.076 Uiso 0.65 1 calc PR E 1 H69C H 0.2313 0.4330 0.4678 0.076 Uiso 0.65 1 calc PR E 1 C67B C 0.24965(14) 0.4236(8) 0.5673(3) 0.032(2) Uiso 0.35 1 d P E 2 H67D H 0.2519 0.4546 0.5983 0.048 Uiso 0.35 1 calc PR E 2 H67E H 0.2640 0.4367 0.5632 0.048 Uiso 0.35 1 calc PR E 2 H67F H 0.2458 0.3321 0.5646 0.048 Uiso 0.35 1 calc PR E 2 C68B C 0.23232(19) 0.6398(9) 0.5417(4) 0.057(3) Uiso 0.35 1 d P E 2 H68D H 0.2243 0.6591 0.5616 0.085 Uiso 0.35 1 calc PR E 2 H68E H 0.2254 0.6905 0.5127 0.085 Uiso 0.35 1 calc PR E 2 H68F H 0.2489 0.6614 0.5586 0.085 Uiso 0.35 1 calc PR E 2 C69B C 0.2320(2) 0.4836(11) 0.4835(4) 0.071(3) Uiso 0.35 1 d P E 2 H69D H 0.2243 0.5560 0.4629 0.106 Uiso 0.35 1 calc PR E 2 H69E H 0.2246 0.4033 0.4682 0.106 Uiso 0.35 1 calc PR E 2 H69F H 0.2485 0.4825 0.4897 0.106 Uiso 0.35 1 calc PR E 2 O28 O 0.10444(3) 0.37570(17) 0.44262(6) 0.0222(4) Uani 1 1 d D . . H281 H 0.0941(5) 0.432(2) 0.4238(9) 0.033 Uiso 1 1 d D . . H282 H 0.1042(5) 0.372(3) 0.4663(8) 0.033 Uiso 1 1 d D . . O29 O 0.12215(3) 0.37321(17) 0.54406(6) 0.0213(4) Uani 1 1 d D . . H291 H 0.1234(5) 0.436(2) 0.5656(9) 0.032 Uiso 1 1 d D . . H292 H 0.1348(4) 0.360(3) 0.5436(10) 0.032 Uiso 1 1 d D . . O30 O 0.15580(3) 0.37814(17) 0.50069(6) 0.0212(4) Uani 1 1 d D . . H301 H 0.1651(5) 0.435(2) 0.4967(9) 0.032 Uiso 1 1 d D . . H302 H 0.1441(4) 0.371(3) 0.4770(8) 0.032 Uiso 1 1 d D . . Cl1A Cl -0.00511(8) -0.0778(3) 0.2541(3) 0.074(2) Uani 0.31 1 d PU . . Cl2A Cl 0.01169(8) 0.1121(5) 0.18683(17) 0.0916(18) Uani 0.31 1 d PU . . Cl1B Cl -0.01261(14) 0.0041(8) 0.2710(3) 0.107(2) Uiso 0.19 1 d PU . . Cl2B Cl 0.01288(15) 0.0772(8) 0.2035(3) 0.059(2) Uiso 0.19 1 d PU . . C91 C 0.0037(2) 0.0891(7) 0.2426(4) 0.079(3) Uiso 0.50 1 d P . . 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 Fe1 0.0166(2) 0.01668(18) 0.01568(18) -0.00079(14) 0.00754(15) -0.00138(15) Fe2 0.0177(2) 0.01633(18) 0.01703(18) 0.00126(14) 0.00843(15) 0.00122(15) Fe3 0.0176(2) 0.01592(17) 0.01731(18) -0.00037(14) 0.00681(15) 0.00112(15) Fe4 0.0171(2) 0.01808(19) 0.01946(18) -0.00403(14) 0.00860(15) -0.00190(15) Fe5 0.0208(2) 0.01649(18) 0.01851(18) -0.00316(14) 0.00983(16) -0.00217(15) Fe6 0.0205(2) 0.01687(18) 0.01613(18) 0.00047(14) 0.00753(15) -0.00296(15) Fe7 0.0175(2) 0.01595(17) 0.01798(18) 0.00147(14) 0.00691(15) -0.00209(15) O1 0.0147(9) 0.0187(9) 0.0164(8) 0.0004(7) 0.0060(7) 0.0012(7) O2 0.0153(9) 0.0196(9) 0.0169(9) -0.0045(7) 0.0071(7) -0.0030(7) O3 0.0166(9) 0.0187(9) 0.0150(8) 0.0010(7) 0.0058(7) -0.0024(7) N1 0.0197(12) 0.0166(11) 0.0190(11) 0.0014(8) 0.0091(9) -0.0011(9) C1 0.0227(15) 0.0163(13) 0.0241(13) 0.0022(10) 0.0118(11) 0.0025(11) C2 0.0221(15) 0.0166(13) 0.0265(14) 0.0048(10) 0.0113(12) 0.0032(11) O4 0.0199(10) 0.0156(9) 0.0200(9) 0.0025(7) 0.0104(8) 0.0034(7) C3 0.0140(13) 0.0251(14) 0.0228(13) 0.0019(11) 0.0075(11) 0.0034(11) C4 0.0166(14) 0.0252(14) 0.0212(13) -0.0003(11) 0.0082(11) 0.0004(11) O5 0.0163(10) 0.0193(9) 0.0228(9) -0.0010(7) 0.0098(8) -0.0009(7) C5 0.0270(16) 0.0222(14) 0.0230(14) 0.0036(11) 0.0153(12) 0.0013(11) C6 0.0262(16) 0.0255(14) 0.0293(15) -0.0008(11) 0.0159(12) 0.0020(12) C7 0.0414(19) 0.0374(17) 0.0411(18) -0.0005(14) 0.0310(16) 0.0061(14) C8 0.057(2) 0.064(2) 0.0327(17) 0.0002(16) 0.0287(17) 0.0058(18) N2 0.0179(12) 0.0205(11) 0.0224(11) -0.0033(9) 0.0093(9) -0.0025(9) C9 0.0234(15) 0.0175(13) 0.0281(14) -0.0066(11) 0.0122(12) -0.0037(11) C10 0.0247(15) 0.0195(13) 0.0230(14) -0.0061(11) 0.0099(12) -0.0016(11) O6 0.0182(10) 0.0149(8) 0.0219(9) -0.0054(7) 0.0092(8) -0.0024(7) C11 0.0201(15) 0.0293(15) 0.0205(13) -0.0074(11) 0.0079(11) -0.0035(12) C12 0.0186(15) 0.0272(14) 0.0201(13) -0.0024(11) 0.0052(11) -0.0012(11) O7 0.0166(10) 0.0197(9) 0.0184(9) -0.0031(7) 0.0049(7) -0.0022(7) C13 0.0195(15) 0.0234(14) 0.0285(15) -0.0061(11) 0.0115(12) -0.0027(11) C14 0.0243(16) 0.0277(15) 0.0298(15) -0.0088(12) 0.0129(12) -0.0041(12) C15 0.0287(17) 0.0404(18) 0.0458(18) -0.0153(14) 0.0200(15) -0.0118(14) C16 0.0285(19) 0.051(2) 0.068(2) -0.0170(18) 0.0213(17) -0.0183(16) N3 0.0250(13) 0.0185(11) 0.0204(11) 0.0023(9) 0.0107(10) -0.0006(9) C17 0.0312(16) 0.0180(13) 0.0222(14) 0.0016(10) 0.0143(12) -0.0025(11) C18 0.0272(16) 0.0186(13) 0.0264(14) 0.0000(11) 0.0142(12) -0.0064(11) O8 0.0227(10) 0.0167(9) 0.0173(9) 0.0021(7) 0.0094(8) -0.0044(7) C19 0.0289(16) 0.0292(15) 0.0224(14) 0.0028(11) 0.0165(12) -0.0010(12) C20 0.0307(17) 0.0259(14) 0.0201(13) -0.0018(11) 0.0134(12) 0.0003(12) O9 0.0239(10) 0.0202(9) 0.0151(9) -0.0001(7) 0.0090(8) -0.0018(8) C21 0.0280(16) 0.0251(14) 0.0186(13) 0.0032(11) 0.0034(12) -0.0071(12) C22 0.0352(18) 0.0465(19) 0.0283(16) 0.0155(14) 0.0157(14) 0.0087(15) C23A 0.032(3) 0.051(3) 0.029(3) 0.012(2) 0.016(3) 0.006(3) C24A 0.049(3) 0.051(3) 0.032(3) 0.012(2) 0.009(2) -0.001(3) O10 0.0204(10) 0.0206(9) 0.0188(9) -0.0012(7) 0.0074(8) 0.0018(8) O11 0.0246(10) 0.0194(9) 0.0196(9) -0.0016(7) 0.0092(8) 0.0041(8) C25 0.0232(15) 0.0176(13) 0.0185(13) 0.0004(10) 0.0110(11) -0.0023(11) C26 0.0280(16) 0.0258(14) 0.0165(13) -0.0037(11) 0.0094(12) 0.0017(12) C27 0.067(3) 0.0293(17) 0.0345(18) -0.0123(14) 0.0094(17) 0.0059(16) C28 0.0341(19) 0.054(2) 0.0262(16) -0.0143(14) 0.0057(14) -0.0013(15) C29 0.047(2) 0.062(2) 0.0231(15) -0.0028(14) 0.0183(15) -0.0109(17) O12 0.0262(11) 0.0202(9) 0.0215(9) 0.0037(7) 0.0127(8) 0.0029(8) O13 0.0238(11) 0.0213(9) 0.0278(10) 0.0036(8) 0.0132(8) 0.0026(8) C30 0.0221(15) 0.0205(14) 0.0130(12) 0.0001(10) 0.0039(11) -0.0029(11) C31 0.0260(16) 0.0210(14) 0.0232(14) 0.0029(11) 0.0125(12) 0.0005(11) C32 0.053(2) 0.0349(17) 0.0285(16) 0.0022(13) 0.0236(15) -0.0065(15) C33 0.044(2) 0.0236(15) 0.0488(19) 0.0099(13) 0.0261(16) 0.0015(14) C34 0.0338(18) 0.0342(17) 0.0419(18) 0.0070(13) 0.0168(15) -0.0069(14) O14 0.0280(11) 0.0219(9) 0.0234(9) -0.0061(8) 0.0155(8) -0.0061(8) O15 0.0272(11) 0.0214(9) 0.0248(10) -0.0057(7) 0.0148(8) -0.0066(8) C35 0.0210(15) 0.0200(14) 0.0240(14) 0.0004(11) 0.0104(12) 0.0015(11) C36 0.0299(16) 0.0261(14) 0.0245(14) -0.0025(11) 0.0153(12) -0.0055(12) C37 0.0320(18) 0.052(2) 0.0421(18) 0.0030(15) 0.0222(15) 0.0008(15) C38 0.048(2) 0.0323(17) 0.0406(17) -0.0053(13) 0.0273(16) -0.0154(15) C39 0.044(2) 0.0413(18) 0.0287(16) -0.0031(13) 0.0224(14) -0.0138(15) O16 0.0215(10) 0.0215(9) 0.0296(10) -0.0069(8) 0.0121(8) 0.0005(8) O17 0.0218(11) 0.0216(9) 0.0274(10) -0.0052(8) 0.0087(8) 0.0003(8) C40 0.0224(15) 0.0222(14) 0.0247(14) 0.0011(11) 0.0143(12) -0.0005(11) C41 0.0234(16) 0.0227(15) 0.0371(16) -0.0034(12) 0.0110(13) 0.0033(12) O18 0.0212(10) 0.0209(9) 0.0232(9) 0.0027(7) 0.0092(8) -0.0019(8) O19 0.0200(10) 0.0224(10) 0.0271(10) 0.0088(8) 0.0071(8) -0.0001(8) C45 0.0222(15) 0.0205(13) 0.0213(13) 0.0000(11) 0.0054(11) -0.0007(11) C46 0.0219(16) 0.0329(16) 0.0376(17) 0.0134(13) 0.0094(13) 0.0007(13) C47 0.0253(18) 0.0432(19) 0.058(2) 0.0169(16) 0.0193(16) 0.0102(14) C48 0.037(2) 0.071(3) 0.043(2) 0.0077(18) -0.0048(16) 0.0038(19) C49 0.036(2) 0.043(2) 0.095(3) 0.0414(19) 0.0300(19) 0.0175(16) O20 0.0269(11) 0.0205(9) 0.0188(9) -0.0009(7) 0.0075(8) -0.0064(8) O21 0.0331(12) 0.0204(9) 0.0195(9) -0.0008(7) 0.0099(8) -0.0066(8) C50 0.0178(14) 0.0225(14) 0.0232(14) -0.0028(11) 0.0058(11) -0.0021(11) C51 0.0384(19) 0.0225(14) 0.0228(14) -0.0054(11) 0.0066(13) -0.0097(13) C52A 0.066(3) 0.031(2) 0.043(2) -0.0162(17) 0.025(2) -0.027(2) C53A 0.065(3) 0.0290(19) 0.042(2) -0.0110(16) 0.030(2) -0.0085(19) C54A 0.055(3) 0.043(2) 0.029(2) -0.0090(17) -0.0040(18) -0.012(2) O22 0.0221(10) 0.0203(9) 0.0212(9) 0.0008(7) 0.0067(8) 0.0048(8) O23 0.0794(18) 0.0321(12) 0.0236(11) -0.0066(9) 0.0035(11) 0.0290(11) C55 0.0280(16) 0.0238(15) 0.0268(15) 0.0013(12) 0.0112(12) 0.0052(12) C56 0.0314(17) 0.0279(15) 0.0230(14) 0.0004(12) 0.0075(13) 0.0112(13) C57 0.046(2) 0.0451(19) 0.0303(17) 0.0092(14) 0.0124(15) 0.0114(16) C58 0.076(3) 0.054(2) 0.0313(18) 0.0068(16) 0.0100(18) 0.043(2) C59 0.0291(19) 0.067(2) 0.0389(19) 0.0108(17) -0.0017(15) 0.0037(17) O24 0.0302(11) 0.0174(9) 0.0210(9) -0.0051(7) 0.0137(8) -0.0041(8) O25 0.0560(14) 0.0236(10) 0.0396(11) -0.0092(9) 0.0350(11) -0.0148(10) C60 0.0306(16) 0.0198(14) 0.0196(13) -0.0019(11) 0.0123(12) -0.0036(12) C61 0.0411(18) 0.0188(14) 0.0270(14) -0.0066(11) 0.0225(13) -0.0076(12) C62 0.048(2) 0.0242(15) 0.0280(15) -0.0066(12) 0.0222(14) -0.0040(13) C63 0.060(2) 0.0389(19) 0.065(2) -0.0206(16) 0.049(2) -0.0180(17) C64 0.095(3) 0.0255(16) 0.0327(17) -0.0015(13) 0.0414(19) -0.0020(17) O26 0.0194(10) 0.0175(9) 0.0274(10) 0.0045(7) 0.0103(8) -0.0034(7) O27 0.0219(11) 0.0237(10) 0.0515(13) 0.0149(9) 0.0127(9) 0.0014(8) C65 0.0225(15) 0.0198(14) 0.0193(13) 0.0017(10) 0.0092(11) -0.0016(11) C66 0.0228(16) 0.0200(14) 0.0321(15) 0.0057(11) 0.0099(12) -0.0035(11) O28 0.0281(11) 0.0208(10) 0.0166(9) -0.0004(8) 0.0085(9) 0.0034(8) O29 0.0254(11) 0.0205(10) 0.0225(10) -0.0036(7) 0.0146(9) -0.0017(8) O30 0.0185(11) 0.0199(10) 0.0234(10) 0.0024(8) 0.0072(8) -0.0025(8) Cl1A 0.045(4) 0.0619(16) 0.057(3) 0.018(2) -0.036(3) -0.0135(17) Cl2A 0.057(3) 0.107(4) 0.069(3) -0.031(3) -0.013(2) 0.015(2) _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 Fe1 O6 1.9865(16) . ? Fe1 O4 1.9944(16) . ? Fe1 O8 1.9994(15) . ? Fe1 O2 2.0023(16) . ? Fe1 O1 2.0066(16) . ? Fe1 O3 2.0085(16) . ? Fe1 Fe6 2.9653(5) . ? Fe1 Fe4 2.9686(5) . ? Fe1 Fe2 2.9751(5) . ? Fe2 O1 1.8878(16) . ? Fe2 O4 1.9722(16) . ? Fe2 O5 2.0101(16) . ? Fe2 O12 2.0336(16) . ? Fe2 O10 2.0507(16) . ? Fe2 N1 2.243(2) . ? Fe3 O1 1.8597(15) . ? Fe3 O7 1.9895(17) . ? Fe3 O22 2.0244(16) . ? Fe3 O11 2.0465(16) . ? Fe3 O28 2.0776(18) . ? Fe3 O13 2.0832(18) . ? Fe4 O2 1.8863(16) . ? Fe4 O6 1.9801(16) . ? Fe4 O7 2.0102(16) . ? Fe4 O16 2.0304(17) . ? Fe4 O14 2.0398(17) . ? Fe4 N2 2.236(2) . ? Fe5 O2 1.8577(16) . ? Fe5 O9 1.9935(16) . ? Fe5 O24 2.0233(16) . ? Fe5 O15 2.0427(17) . ? Fe5 O17 2.0875(17) . ? Fe5 O29 2.0997(18) . ? Fe6 O3 1.8819(15) . ? Fe6 O8 1.9715(16) . ? Fe6 O9 2.0130(17) . ? Fe6 O20 2.0308(16) . ? Fe6 O18 2.0624(18) . ? Fe6 N3 2.238(2) . ? Fe7 O3 1.8621(16) . ? Fe7 O5 1.9874(16) . ? Fe7 O26 2.0254(17) . ? Fe7 O19 2.0396(17) . ? Fe7 O30 2.0844(18) . ? Fe7 O21 2.0865(17) . ? N1 C3 1.485(3) . ? N1 C1 1.487(3) . ? N1 C5 1.493(3) . ? C1 C2 1.520(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O4 1.408(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.508(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O5 1.430(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.521(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.526(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.521(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? N2 C13 1.484(3) . ? N2 C11 1.485(3) . ? N2 C9 1.490(3) . ? C9 C10 1.521(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O6 1.411(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.506(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O7 1.431(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.529(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.517(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.516(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? N3 C19 1.490(3) . ? N3 C17 1.491(3) . ? N3 C21 1.493(3) . ? C17 C18 1.526(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O8 1.408(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.510(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O9 1.427(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.511(3) . ? C21 H21A 0.9500 . ? C22 C23B 1.388(11) . ? C22 C23A 1.604(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22 H22C 0.9702 . ? C22 H22D 0.9699 . ? C23A C24A 1.505(6) . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C24A H24C 0.9800 . ? C23B C24B 1.505(12) . ? C23B H23C 0.9900 . ? C23B H23D 0.9900 . ? C24B H24D 0.9800 . ? C24B H24E 0.9800 . ? C24B H24F 0.9800 . ? O10 C25 1.263(3) . ? O11 C25 1.263(3) . ? C25 C26 1.535(3) . ? C26 C28 1.515(4) . ? C26 C27 1.523(4) . ? C26 C29 1.534(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? O12 C30 1.272(3) . ? O13 C30 1.252(3) . ? C30 C31 1.537(3) . ? C31 C34 1.521(4) . ? C31 C33 1.528(4) . ? C31 C32 1.532(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O14 C35 1.261(3) . ? O15 C35 1.272(3) . ? C35 C36 1.527(4) . ? C36 C38 1.524(4) . ? C36 C39 1.529(3) . ? C36 C37 1.532(4) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? O16 C40 1.273(3) . ? O17 C40 1.251(3) . ? C40 C41 1.531(3) . ? C41 C44B 1.449(9) . ? C41 C43A 1.482(6) . ? C41 C43B 1.492(9) . ? C41 C42A 1.498(6) . ? C41 C44A 1.574(5) . ? C41 C42B 1.682(9) . ? C42A H42A 0.9800 . ? C42A H42B 0.9800 . ? C42A H42C 0.9800 . ? C43A H43A 0.9800 . ? C43A H43B 0.9800 . ? C43A H43C 0.9800 . ? C44A H44A 0.9800 . ? C44A H44B 0.9800 . ? C44A H44C 0.9800 . ? C42B H42D 0.9800 . ? C42B H42E 0.9800 . ? C42B H42F 0.9800 . ? C43B H43D 0.9800 . ? C43B H43E 0.9800 . ? C43B H43F 0.9800 . ? C44B H44D 0.9800 . ? C44B H44E 0.9800 . ? C44B H44F 0.9800 . ? O18 C45 1.257(3) . ? O19 C45 1.266(3) . ? C45 C46 1.533(4) . ? C46 C49 1.518(4) . ? C46 C47 1.524(4) . ? C46 C48 1.547(4) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? O20 C50 1.260(3) . ? O21 C50 1.262(3) . ? C50 C51 1.536(3) . ? C51 C53B 1.384(14) . ? C51 C54B 1.501(15) . ? C51 C52A 1.505(4) . ? C51 C54A 1.530(4) . ? C51 C53A 1.567(5) . ? C51 C52B 1.590(14) . ? C52A H52A 0.9800 . ? C52A H52B 0.9800 . ? C52A H52C 0.9800 . ? C53A H53A 0.9800 . ? C53A H53B 0.9800 . ? C53A H53C 0.9800 . ? C54A H54A 0.9800 . ? C54A H54B 0.9800 . ? C54A H54C 0.9800 . ? C52B H52D 0.9800 . ? C52B H52E 0.9800 . ? C52B H52F 0.9800 . ? C53B H53D 0.9800 . ? C53B H53E 0.9800 . ? C53B H53F 0.9800 . ? C54B H54D 0.9800 . ? C54B H54E 0.9800 . ? C54B H54F 0.9800 . ? O22 C55 1.272(3) . ? O23 C55 1.238(3) . ? C55 C56 1.528(4) . ? C56 C59 1.516(4) . ? C56 C58 1.518(4) . ? C56 C57 1.537(4) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? O24 C60 1.277(3) . ? O25 C60 1.234(3) . ? C60 C61 1.534(3) . ? C61 C64 1.519(4) . ? C61 C63 1.525(4) . ? C61 C62 1.534(3) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? O26 C65 1.269(3) . ? O27 C65 1.244(3) . ? C65 C66 1.528(4) . ? C66 C68A 1.501(5) . ? C66 C69B 1.513(11) . ? C66 C67A 1.522(5) . ? C66 C67B 1.522(8) . ? C66 C68B 1.528(10) . ? C66 C69A 1.546(6) . ? C67A H67A 0.9800 . ? C67A H67B 0.9800 . ? C67A H67C 0.9800 . ? C68A H68A 0.9800 . ? C68A H68B 0.9800 . ? C68A H68C 0.9800 . ? C69A H69A 0.9800 . ? C69A H69B 0.9800 . ? C69A H69C 0.9800 . ? C67B H67D 0.9800 . ? C67B H67E 0.9800 . ? C67B H67F 0.9800 . ? C68B H68D 0.9800 . ? C68B H68E 0.9800 . ? C68B H68F 0.9800 . ? C69B H69D 0.9800 . ? C69B H69E 0.9800 . ? C69B H69F 0.9800 . ? O28 H281 0.89(2) . ? O28 H282 0.75(2) . ? O29 H291 0.92(2) . ? O29 H292 0.82(2) . ? O30 H301 0.88(2) . ? O30 H302 0.80(2) . ? Cl1A Cl1A 0.791(11) 2 ? Cl1A Cl1B 1.206(9) . ? Cl1A C91 1.745(8) 2 ? Cl1A Cl1B 1.834(11) 2 ? Cl1A C91 1.908(8) . ? Cl1A Cl2B 2.278(9) 2 ? Cl2A Cl2B 0.615(9) . ? Cl2A Cl1B 1.720(10) 2 ? Cl2A C91 2.036(11) . ? Cl1B Cl2B 1.111(9) 2 ? Cl1B C91 1.223(10) 2 ? Cl1B Cl2A 1.720(10) 2 ? Cl1B Cl1A 1.834(11) 2 ? Cl1B C91 1.850(12) . ? Cl1B Cl1B 2.467(18) 2 ? Cl2B Cl1B 1.111(9) 2 ? Cl2B C91 1.574(12) . ? Cl2B Cl1A 2.278(9) 2 ? C91 C91 0.782(18) 2 ? C91 Cl1B 1.224(10) 2 ? C91 Cl1A 1.745(8) 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 O6 Fe1 O4 91.43(7) . . ? O6 Fe1 O8 92.31(7) . . ? O4 Fe1 O8 92.58(7) . . ? O6 Fe1 O2 78.02(6) . . ? O4 Fe1 O2 162.17(6) . . ? O8 Fe1 O2 102.07(7) . . ? O6 Fe1 O1 102.51(6) . . ? O4 Fe1 O1 77.82(6) . . ? O8 Fe1 O1 162.42(7) . . ? O2 Fe1 O1 90.34(6) . . ? O6 Fe1 O3 163.18(7) . . ? O4 Fe1 O3 102.57(7) . . ? O8 Fe1 O3 77.95(6) . . ? O2 Fe1 O3 90.51(7) . . ? O1 Fe1 O3 89.68(6) . . ? O6 Fe1 Fe6 127.32(5) . . ? O4 Fe1 Fe6 109.89(5) . . ? O8 Fe1 Fe6 41.33(5) . . ? O2 Fe1 Fe6 87.90(4) . . ? O1 Fe1 Fe6 128.37(5) . . ? O3 Fe1 Fe6 38.78(4) . . ? O6 Fe1 Fe4 41.47(5) . . ? O4 Fe1 Fe4 126.24(5) . . ? O8 Fe1 Fe4 109.62(5) . . ? O2 Fe1 Fe4 38.81(4) . . ? O1 Fe1 Fe4 87.85(5) . . ? O3 Fe1 Fe4 129.19(5) . . ? Fe6 Fe1 Fe4 119.168(15) . . ? O6 Fe1 Fe2 108.76(5) . . ? O4 Fe1 Fe2 41.12(5) . . ? O8 Fe1 Fe2 127.16(5) . . ? O2 Fe1 Fe2 129.04(5) . . ? O1 Fe1 Fe2 38.73(5) . . ? O3 Fe1 Fe2 88.01(5) . . ? Fe6 Fe1 Fe2 119.037(16) . . ? Fe4 Fe1 Fe2 118.271(15) . . ? O1 Fe2 O4 81.21(7) . . ? O1 Fe2 O5 96.80(7) . . ? O4 Fe2 O5 95.90(7) . . ? O1 Fe2 O12 101.62(7) . . ? O4 Fe2 O12 175.76(7) . . ? O5 Fe2 O12 86.92(7) . . ? O1 Fe2 O10 98.82(7) . . ? O4 Fe2 O10 92.14(7) . . ? O5 Fe2 O10 163.35(7) . . ? O12 Fe2 O10 84.34(7) . . ? O1 Fe2 N1 159.57(7) . . ? O4 Fe2 N1 78.93(7) . . ? O5 Fe2 N1 80.54(7) . . ? O12 Fe2 N1 98.47(7) . . ? O10 Fe2 N1 86.76(7) . . ? O1 Fe2 Fe1 41.69(5) . . ? O4 Fe2 Fe1 41.69(5) . . ? O5 Fe2 Fe1 88.00(5) . . ? O12 Fe2 Fe1 141.85(5) . . ? O10 Fe2 Fe1 107.55(5) . . ? N1 Fe2 Fe1 117.89(5) . . ? O1 Fe3 O7 95.27(7) . . ? O1 Fe3 O22 175.12(7) . . ? O7 Fe3 O22 89.51(7) . . ? O1 Fe3 O11 97.51(7) . . ? O7 Fe3 O11 90.98(7) . . ? O22 Fe3 O11 83.34(7) . . ? O1 Fe3 O28 92.36(7) . . ? O7 Fe3 O28 95.99(7) . . ? O22 Fe3 O28 86.17(7) . . ? O11 Fe3 O28 167.34(7) . . ? O1 Fe3 O13 90.45(7) . . ? O7 Fe3 O13 174.27(7) . . ? O22 Fe3 O13 84.77(7) . . ? O11 Fe3 O13 87.91(7) . . ? O28 Fe3 O13 84.10(7) . . ? O2 Fe4 O6 80.95(7) . . ? O2 Fe4 O7 96.82(7) . . ? O6 Fe4 O7 96.80(7) . . ? O2 Fe4 O16 101.79(7) . . ? O6 Fe4 O16 175.08(7) . . ? O7 Fe4 O16 86.97(7) . . ? O2 Fe4 O14 97.78(7) . . ? O6 Fe4 O14 91.21(7) . . ? O7 Fe4 O14 164.29(7) . . ? O16 Fe4 O14 84.39(7) . . ? O2 Fe4 N2 159.55(7) . . ? O6 Fe4 N2 79.20(7) . . ? O7 Fe4 N2 80.74(7) . . ? O16 Fe4 N2 98.36(7) . . ? O14 Fe4 N2 87.56(7) . . ? O2 Fe4 Fe1 41.70(5) . . ? O6 Fe4 Fe1 41.63(5) . . ? O7 Fe4 Fe1 88.10(5) . . ? O16 Fe4 Fe1 142.08(5) . . ? O14 Fe4 Fe1 106.72(5) . . ? N2 Fe4 Fe1 117.86(6) . . ? O2 Fe5 O9 95.17(7) . . ? O2 Fe5 O24 174.50(7) . . ? O9 Fe5 O24 88.77(7) . . ? O2 Fe5 O15 97.39(7) . . ? O9 Fe5 O15 90.83(7) . . ? O24 Fe5 O15 86.37(7) . . ? O2 Fe5 O17 91.80(7) . . ? O9 Fe5 O17 173.02(7) . . ? O24 Fe5 O17 84.30(7) . . ? O15 Fe5 O17 87.88(7) . . ? O2 Fe5 O29 89.93(7) . . ? O9 Fe5 O29 95.54(7) . . ? O24 Fe5 O29 85.86(7) . . ? O15 Fe5 O29 169.84(7) . . ? O17 Fe5 O29 84.84(7) . . ? O3 Fe6 O8 81.68(7) . . ? O3 Fe6 O9 97.26(7) . . ? O8 Fe6 O9 96.14(7) . . ? O3 Fe6 O20 100.95(7) . . ? O8 Fe6 O20 174.91(7) . . ? O9 Fe6 O20 87.88(7) . . ? O3 Fe6 O18 98.33(7) . . ? O8 Fe6 O18 90.94(7) . . ? O9 Fe6 O18 163.66(7) . . ? O20 Fe6 O18 84.39(7) . . ? O3 Fe6 N3 160.89(7) . . ? O8 Fe6 N3 79.77(7) . . ? O9 Fe6 N3 80.25(7) . . ? O20 Fe6 N3 97.90(7) . . ? O18 Fe6 N3 86.57(7) . . ? O3 Fe6 Fe1 41.95(5) . . ? O8 Fe6 Fe1 42.05(4) . . ? O9 Fe6 Fe1 88.08(5) . . ? O20 Fe6 Fe1 141.59(5) . . ? O18 Fe6 Fe1 106.86(5) . . ? N3 Fe6 Fe1 118.95(5) . . ? O3 Fe7 O5 95.89(7) . . ? O3 Fe7 O26 174.81(7) . . ? O5 Fe7 O26 88.99(7) . . ? O3 Fe7 O19 97.49(7) . . ? O5 Fe7 O19 90.57(7) . . ? O26 Fe7 O19 84.18(7) . . ? O3 Fe7 O30 91.61(7) . . ? O5 Fe7 O30 95.75(7) . . ? O26 Fe7 O30 86.14(7) . . ? O19 Fe7 O30 168.35(7) . . ? O3 Fe7 O21 91.31(7) . . ? O5 Fe7 O21 172.78(7) . . ? O26 Fe7 O21 83.83(7) . . ? O19 Fe7 O21 87.99(7) . . ? O30 Fe7 O21 84.52(7) . . ? Fe3 O1 Fe2 118.93(8) . . ? Fe3 O1 Fe1 134.57(9) . . ? Fe2 O1 Fe1 99.58(7) . . ? Fe5 O2 Fe4 119.13(9) . . ? Fe5 O2 Fe1 134.90(8) . . ? Fe4 O2 Fe1 99.49(7) . . ? Fe7 O3 Fe6 119.37(8) . . ? Fe7 O3 Fe1 134.03(8) . . ? Fe6 O3 Fe1 99.27(7) . . ? C3 N1 C1 112.59(18) . . ? C3 N1 C5 111.43(19) . . ? C1 N1 C5 111.54(18) . . ? C3 N1 Fe2 105.48(14) . . ? C1 N1 Fe2 103.40(14) . . ? C5 N1 Fe2 111.98(14) . . ? N1 C1 C2 109.99(19) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? O4 C2 C1 107.71(19) . . ? O4 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? O4 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? C2 O4 Fe2 120.48(14) . . ? C2 O4 Fe1 137.01(14) . . ? Fe2 O4 Fe1 97.19(7) . . ? N1 C3 C4 109.56(19) . . ? N1 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? N1 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? O5 C4 C3 107.9(2) . . ? O5 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? O5 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? C4 O5 Fe7 120.58(14) . . ? C4 O5 Fe2 110.63(14) . . ? Fe7 O5 Fe2 128.11(9) . . ? N1 C5 C6 116.3(2) . . ? N1 C5 H5A 108.2 . . ? C6 C5 H5A 108.2 . . ? N1 C5 H5B 108.2 . . ? C6 C5 H5B 108.2 . . ? H5A C5 H5B 107.4 . . ? C5 C6 C7 112.6(2) . . ? C5 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C6 114.2(2) . . ? C8 C7 H7A 108.7 . . ? C6 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? C6 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C13 N2 C11 112.18(19) . . ? C13 N2 C9 111.32(19) . . ? C11 N2 C9 112.21(19) . . ? C13 N2 Fe4 111.45(14) . . ? C11 N2 Fe4 105.37(14) . . ? C9 N2 Fe4 103.85(14) . . ? N2 C9 C10 110.0(2) . . ? N2 C9 H9A 109.7 . . ? C10 C9 H9A 109.7 . . ? N2 C9 H9B 109.7 . . ? C10 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? O6 C10 C9 108.0(2) . . ? O6 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? O6 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C10 O6 Fe4 119.90(14) . . ? C10 O6 Fe1 136.84(15) . . ? Fe4 O6 Fe1 96.90(7) . . ? N2 C11 C12 109.7(2) . . ? N2 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? N2 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? O7 C12 C11 107.83(19) . . ? O7 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? O7 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? H12A C12 H12B 108.5 . . ? C12 O7 Fe3 120.22(15) . . ? C12 O7 Fe4 110.45(14) . . ? Fe3 O7 Fe4 128.45(8) . . ? N2 C13 C14 116.5(2) . . ? N2 C13 H13A 108.2 . . ? C14 C13 H13A 108.2 . . ? N2 C13 H13B 108.2 . . ? C14 C13 H13B 108.2 . . ? H13A C13 H13B 107.3 . . ? C15 C14 C13 111.4(2) . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C14 113.1(2) . . ? C16 C15 H15A 109.0 . . ? C14 C15 H15A 109.0 . . ? C16 C15 H15B 109.0 . . ? C14 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 N3 C17 112.1(2) . . ? C19 N3 C21 112.3(2) . . ? C17 N3 C21 112.11(19) . . ? C19 N3 Fe6 106.25(14) . . ? C17 N3 Fe6 103.58(14) . . ? C21 N3 Fe6 109.93(15) . . ? N3 C17 C18 109.60(19) . . ? N3 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? N3 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? O8 C18 C17 108.0(2) . . ? O8 C18 H18A 110.1 . . ? C17 C18 H18A 110.1 . . ? O8 C18 H18B 110.1 . . ? C17 C18 H18B 110.1 . . ? H18A C18 H18B 108.4 . . ? C18 O8 Fe6 119.23(14) . . ? C18 O8 Fe1 136.65(15) . . ? Fe6 O8 Fe1 96.62(7) . . ? N3 C19 C20 109.6(2) . . ? N3 C19 H19A 109.8 . . ? C20 C19 H19A 109.8 . . ? N3 C19 H19B 109.8 . . ? C20 C19 H19B 109.8 . . ? H19A C19 H19B 108.2 . . ? O9 C20 C19 108.2(2) . . ? O9 C20 H20A 110.1 . . ? C19 C20 H20A 110.1 . . ? O9 C20 H20B 110.1 . . ? C19 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? C20 O9 Fe5 120.33(15) . . ? C20 O9 Fe6 110.78(14) . . ? Fe5 O9 Fe6 128.37(8) . . ? N3 C21 C22 117.8(2) . . ? N3 C21 H21A 121.1 . . ? C22 C21 H21A 121.1 . . ? C23B C22 C21 121.3(5) . . ? C23B C22 C23A 22.5(4) . . ? C21 C22 C23A 107.9(3) . . ? C23B C22 H22A 115.9 . . ? C21 C22 H22A 110.1 . . ? C23A C22 H22A 110.1 . . ? C23B C22 H22B 88.0 . . ? C21 C22 H22B 110.1 . . ? C23A C22 H22B 110.1 . . ? H22A C22 H22B 108.4 . . ? C23B C22 H22C 107.5 . . ? C21 C22 H22C 107.0 . . ? C23A C22 H22C 130.0 . . ? H22A C22 H22C 89.8 . . ? H22B C22 H22C 22.3 . . ? C23B C22 H22D 107.0 . . ? C21 C22 H22D 106.6 . . ? C23A C22 H22D 96.4 . . ? H22A C22 H22D 17.1 . . ? H22B C22 H22D 124.1 . . ? H22C C22 H22D 106.6 . . ? C24A C23A C22 112.4(4) . . ? C24A C23A H23A 109.1 . . ? C22 C23A H23A 109.1 . . ? C24A C23A H23B 109.1 . . ? C22 C23A H23B 109.1 . . ? H23A C23A H23B 107.8 . . ? C23A C24A H24A 109.5 . . ? C23A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C23A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? C22 C23B C24B 114.1(8) . . ? C22 C23B H23C 108.7 . . ? C24B C23B H23C 108.7 . . ? C22 C23B H23D 108.7 . . ? C24B C23B H23D 108.7 . . ? H23C C23B H23D 107.6 . . ? C23B C24B H24D 109.5 . . ? C23B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C23B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C25 O10 Fe2 125.07(15) . . ? C25 O11 Fe3 134.77(16) . . ? O10 C25 O11 125.5(2) . . ? O10 C25 C26 117.5(2) . . ? O11 C25 C26 117.0(2) . . ? C28 C26 C27 110.4(2) . . ? C28 C26 C29 109.9(2) . . ? C27 C26 C29 109.5(2) . . ? C28 C26 C25 111.5(2) . . ? C27 C26 C25 109.8(2) . . ? C29 C26 C25 105.7(2) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C30 O12 Fe2 125.57(16) . . ? C30 O13 Fe3 131.17(16) . . ? O13 C30 O12 125.3(2) . . ? O13 C30 C31 118.5(2) . . ? O12 C30 C31 116.2(2) . . ? C34 C31 C33 110.1(2) . . ? C34 C31 C32 110.7(2) . . ? C33 C31 C32 109.4(2) . . ? C34 C31 C30 109.2(2) . . ? C33 C31 C30 110.3(2) . . ? C32 C31 C30 107.1(2) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C35 O14 Fe4 126.44(16) . . ? C35 O15 Fe5 134.11(16) . . ? O14 C35 O15 124.9(2) . . ? O14 C35 C36 117.2(2) . . ? O15 C35 C36 117.8(2) . . ? C38 C36 C35 110.1(2) . . ? C38 C36 C39 110.8(2) . . ? C35 C36 C39 111.1(2) . . ? C38 C36 C37 109.4(2) . . ? C35 C36 C37 105.2(2) . . ? C39 C36 C37 110.0(2) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C40 O16 Fe4 126.61(16) . . ? C40 O17 Fe5 131.50(16) . . ? O17 C40 O16 124.9(2) . . ? O17 C40 C41 118.7(2) . . ? O16 C40 C41 116.4(2) . . ? C44B C41 C43A 72.2(5) . . ? C44B C41 C43B 115.4(6) . . ? C43A C41 C43B 131.4(5) . . ? C44B C41 C42A 128.6(5) . . ? C43A C41 C42A 112.0(4) . . ? C43B C41 C42A 24.0(4) . . ? C44B C41 C40 113.6(4) . . ? C43A C41 C40 110.1(3) . . ? C43B C41 C40 109.3(4) . . ? C42A C41 C40 112.1(3) . . ? C44B C41 C44A 37.1(4) . . ? C43A C41 C44A 108.6(3) . . ? C43B C41 C44A 86.1(5) . . ? C42A C41 C44A 107.4(3) . . ? C40 C41 C44A 106.4(3) . . ? C44B C41 C42B 106.4(5) . . ? C43A C41 C42B 34.9(3) . . ? C43B C41 C42B 109.2(5) . . ? C42A C41 C42B 85.6(4) . . ? C40 C41 C42B 101.9(4) . . ? C44A C41 C42B 141.0(4) . . ? C41 C42A H42A 109.5 . . ? C41 C42A H42B 109.5 . . ? H42A C42A H42B 109.5 . . ? C41 C42A H42C 109.5 . . ? H42A C42A H42C 109.5 . . ? H42B C42A H42C 109.5 . . ? C41 C43A H43A 109.5 . . ? C41 C43A H43B 109.5 . . ? H43A C43A H43B 109.5 . . ? C41 C43A H43C 109.5 . . ? H43A C43A H43C 109.5 . . ? H43B C43A H43C 109.5 . . ? C41 C44A H44A 109.5 . . ? C41 C44A H44B 109.5 . . ? H44A C44A H44B 109.5 . . ? C41 C44A H44C 109.5 . . ? H44A C44A H44C 109.5 . . ? H44B C44A H44C 109.5 . . ? C41 C42B H42D 109.5 . . ? C41 C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C41 C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? C41 C43B H43D 109.5 . . ? C41 C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? C41 C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? C41 C44B H44D 109.5 . . ? C41 C44B H44E 109.5 . . ? H44D C44B H44E 109.5 . . ? C41 C44B H44F 109.5 . . ? H44D C44B H44F 109.5 . . ? H44E C44B H44F 109.5 . . ? C45 O18 Fe6 125.44(16) . . ? C45 O19 Fe7 134.63(17) . . ? O18 C45 O19 125.6(2) . . ? O18 C45 C46 118.2(2) . . ? O19 C45 C46 116.1(2) . . ? C49 C46 C47 111.2(3) . . ? C49 C46 C45 110.9(2) . . ? C47 C46 C45 111.2(2) . . ? C49 C46 C48 109.6(3) . . ? C47 C46 C48 109.5(3) . . ? C45 C46 C48 104.1(2) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C50 O20 Fe6 127.49(15) . . ? C50 O21 Fe7 130.56(16) . . ? O20 C50 O21 125.1(2) . . ? O20 C50 C51 116.9(2) . . ? O21 C50 C51 118.0(2) . . ? C53B C51 C54B 115.4(13) . . ? C52A C51 C54A 112.3(3) . . ? C53B C51 C50 120.7(11) . . ? C54B C51 C50 107.1(11) . . ? C52A C51 C50 111.6(2) . . ? C54A C51 C50 108.1(2) . . ? C52A C51 C53A 109.5(3) . . ? C54A C51 C53A 108.7(3) . . ? C50 C51 C53A 106.4(2) . . ? C53B C51 C52B 108.8(11) . . ? C54B C51 C52B 100.6(11) . . ? C50 C51 C52B 101.5(9) . . ? C51 C52A H52A 109.5 . . ? C51 C52A H52B 109.5 . . ? H52A C52A H52B 109.5 . . ? C51 C52A H52C 109.5 . . ? H52A C52A H52C 109.5 . . ? H52B C52A H52C 109.5 . . ? C51 C53A H53A 109.5 . . ? C51 C53A H53B 109.5 . . ? H53A C53A H53B 109.5 . . ? C51 C53A H53C 109.5 . . ? H53A C53A H53C 109.5 . . ? H53B C53A H53C 109.5 . . ? C51 C54A H54A 109.5 . . ? C51 C54A H54B 109.5 . . ? H54A C54A H54B 109.5 . . ? C51 C54A H54C 109.5 . . ? H54A C54A H54C 109.5 . . ? H54B C54A H54C 109.5 . . ? C51 C52B H52D 109.5 . . ? C51 C52B H52E 109.5 . . ? H52D C52B H52E 109.5 . . ? C51 C52B H52F 109.5 . . ? H52D C52B H52F 109.5 . . ? H52E C52B H52F 109.5 . . ? C51 C53B H53D 109.5 . . ? C51 C53B H53E 109.5 . . ? H53D C53B H53E 109.5 . . ? C51 C53B H53F 109.5 . . ? H53D C53B H53F 109.5 . . ? H53E C53B H53F 109.5 . . ? C51 C54B H54D 109.5 . . ? C51 C54B H54E 109.5 . . ? H54D C54B H54E 109.5 . . ? C51 C54B H54F 109.5 . . ? H54D C54B H54F 109.5 . . ? H54E C54B H54F 109.5 . . ? C55 O22 Fe3 135.33(16) . . ? O23 C55 O22 124.2(2) . . ? O23 C55 C56 120.6(2) . . ? O22 C55 C56 115.2(2) . . ? C59 C56 C58 110.1(3) . . ? C59 C56 C55 108.7(2) . . ? C58 C56 C55 111.1(2) . . ? C59 C56 C57 109.1(2) . . ? C58 C56 C57 110.4(3) . . ? C55 C56 C57 107.3(2) . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C56 C59 H59A 109.5 . . ? C56 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C56 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C60 O24 Fe5 134.56(17) . . ? O25 C60 O24 125.2(2) . . ? O25 C60 C61 120.8(2) . . ? O24 C60 C61 113.9(2) . . ? C64 C61 C63 109.8(2) . . ? C64 C61 C62 109.4(2) . . ? C63 C61 C62 109.5(2) . . ? C64 C61 C60 109.1(2) . . ? C63 C61 C60 108.2(2) . . ? C62 C61 C60 110.8(2) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C65 O26 Fe7 135.22(16) . . ? O27 C65 O26 124.5(2) . . ? O27 C65 C66 120.3(2) . . ? O26 C65 C66 115.1(2) . . ? C68A C66 C67A 111.5(3) . . ? C69B C66 C67B 108.5(6) . . ? C68A C66 C65 112.5(3) . . ? C69B C66 C65 107.7(5) . . ? C67A C66 C65 108.4(3) . . ? C67B C66 C65 115.2(4) . . ? C69B C66 C68B 106.9(6) . . ? C67B C66 C68B 109.4(5) . . ? C65 C66 C68B 108.9(5) . . ? C68A C66 C69A 108.2(3) . . ? C67A C66 C69A 110.1(3) . . ? C65 C66 C69A 106.0(3) . . ? C68B C66 C69A 136.6(5) . . ? C66 C67A H67A 109.5 . . ? C66 C67A H67B 109.5 . . ? H67A C67A H67B 109.5 . . ? C66 C67A H67C 109.5 . . ? H67A C67A H67C 109.5 . . ? H67B C67A H67C 109.5 . . ? C66 C68A H68A 109.5 . . ? C66 C68A H68B 109.5 . . ? H68A C68A H68B 109.5 . . ? C66 C68A H68C 109.5 . . ? H68A C68A H68C 109.5 . . ? H68B C68A H68C 109.5 . . ? C66 C69A H69A 109.5 . . ? C66 C69A H69B 109.5 . . ? H69A C69A H69B 109.5 . . ? C66 C69A H69C 109.5 . . ? H69A C69A H69C 109.5 . . ? H69B C69A H69C 109.5 . . ? C66 C67B H67D 109.5 . . ? C66 C67B H67E 109.5 . . ? H67D C67B H67E 109.5 . . ? C66 C67B H67F 109.5 . . ? H67D C67B H67F 109.5 . . ? H67E C67B H67F 109.5 . . ? C66 C68B H68D 109.5 . . ? C66 C68B H68E 109.5 . . ? H68D C68B H68E 109.5 . . ? C66 C68B H68F 109.5 . . ? H68D C68B H68F 109.5 . . ? H68E C68B H68F 109.5 . . ? C66 C69B H69D 109.5 . . ? C66 C69B H69E 109.5 . . ? H69D C69B H69E 109.5 . . ? C66 C69B H69F 109.5 . . ? H69D C69B H69F 109.5 . . ? H69E C69B H69F 109.5 . . ? Fe3 O28 H281 102.5(17) . . ? Fe3 O28 H282 128(2) . . ? H281 O28 H282 112(3) . . ? Fe5 O29 H291 105.8(17) . . ? Fe5 O29 H292 120(2) . . ? H291 O29 H292 111(3) . . ? Fe7 O30 H301 103.5(18) . . ? Fe7 O30 H302 125(2) . . ? H301 O30 H302 110(3) . . ? Cl2B C91 Cl1B 143.7(7) . . ? Cl2B C91 Cl1A 108.0(6) . . ? Cl1A C91 Cl2A 98.2(5) 2 . ? Cl1B C91 Cl2A 149.9(6) . . ? Cl1A C91 Cl2A 118.0(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O28 H281 O23 0.89(2) 1.69(2) 2.569(3) 168(3) . O28 H282 O29 0.75(2) 2.21(2) 2.895(2) 151(3) . O29 H291 O25 0.92(2) 1.67(2) 2.556(2) 162(3) . O29 H292 O30 0.82(2) 2.27(2) 2.977(3) 145(3) . O30 H301 O27 0.88(2) 1.70(2) 2.568(3) 165(3) . O30 H302 O28 0.80(2) 2.27(3) 2.981(3) 147(3) . _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.078 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.074 ########################################################################### data_283 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H126 Fe7 N3 O30' _chemical_formula_weight 1940.74 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 10.6609(5) _cell_length_b 31.5950(14) _cell_length_c 27.2343(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.120(1) _cell_angle_gamma 90.00 _cell_volume 9173.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20102 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.92 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4076 _exptl_absorpt_coefficient_mu 1.151 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.747 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46053 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.01 _reflns_number_total 20567 _reflns_number_gt 14887 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_data_reduction 'SAINT+ 6.0 (Bruker AXS Inc., 2000)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _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^)+(0.0815P)^2^+1.0523P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20567 _refine_ls_number_parameters 1087 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1380 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.004 _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 Fe1 Fe 0.26150(4) -0.136116(13) 0.250393(14) 0.01720(10) Uani 1 1 d . . . Fe2 Fe 0.24204(4) -0.132782(13) 0.359226(15) 0.01828(10) Uani 1 1 d . . . Fe3 Fe 0.07279(4) -0.058771(13) 0.309137(15) 0.01842(10) Uani 1 1 d D . . Fe4 Fe 0.23341(4) -0.055740(14) 0.194694(15) 0.02013(10) Uani 1 1 d . . . Fe5 Fe 0.06694(4) -0.130722(14) 0.144501(15) 0.02122(10) Uani 1 1 d . . . Fe6 Fe 0.22705(4) -0.218269(13) 0.199232(15) 0.01996(10) Uani 1 1 d . . . Fe7 Fe 0.07198(4) -0.216867(13) 0.302597(15) 0.01975(10) Uani 1 1 d D . . O1 O 0.16079(18) -0.10961(6) 0.30361(7) 0.0186(4) Uani 1 1 d . . . O2 O 0.15435(18) -0.10931(6) 0.19868(7) 0.0208(4) Uani 1 1 d . . . O3 O 0.15366(18) -0.18802(6) 0.25179(7) 0.0194(4) Uani 1 1 d . . . N1 N 0.3915(2) -0.17023(8) 0.40530(9) 0.0233(5) Uani 1 1 d . . . C1 C 0.5049(3) -0.16738(11) 0.37308(11) 0.0259(7) Uani 1 1 d . . . H1A H 0.5658 -0.1896 0.3826 0.031 Uiso 1 1 calc R . . H1B H 0.5456 -0.1395 0.3777 0.031 Uiso 1 1 calc R . . C2 C 0.4693(3) -0.17293(11) 0.31969(11) 0.0267(7) Uani 1 1 d . . . H2A H 0.5423 -0.1669 0.2984 0.032 Uiso 1 1 calc R . . H2B H 0.4417 -0.2024 0.3136 0.032 Uiso 1 1 calc R . . O4 O 0.37074(18) -0.14447(6) 0.30914(7) 0.0191(4) Uani 1 1 d . . . C3 C 0.3414(3) -0.21492(10) 0.40690(12) 0.0298(7) Uani 1 1 d . . . H3A H 0.3813 -0.2319 0.3807 0.036 Uiso 1 1 calc R . . H3B H 0.3630 -0.2280 0.4389 0.036 Uiso 1 1 calc R . . C4 C 0.2011(3) -0.21533(10) 0.40007(11) 0.0260(7) Uani 1 1 d . . . H4A H 0.1709 -0.2448 0.3963 0.031 Uiso 1 1 calc R . . H4B H 0.1597 -0.2027 0.4291 0.031 Uiso 1 1 calc R . . O5 O 0.17157(19) -0.19130(6) 0.35687(7) 0.0222(4) Uani 1 1 d . . . C5 C 0.4172(3) -0.15551(10) 0.45517(11) 0.0252(7) Uani 1 1 d . . . C6 C 0.3193(4) -0.14063(13) 0.48368(13) 0.0391(9) Uani 1 1 d . . . H6 H 0.2365 -0.1400 0.4707 0.047 Uiso 1 1 calc R . . C7 C 0.3420(4) -0.12666(13) 0.53137(13) 0.0446(10) Uani 1 1 d . . . H7 H 0.2746 -0.1160 0.5505 0.054 Uiso 1 1 calc R . . C8 C 0.4596(4) -0.12801(13) 0.55099(13) 0.0453(10) Uani 1 1 d . . . H8 H 0.4744 -0.1184 0.5835 0.054 Uiso 1 1 calc R . . C9 C 0.5544(4) -0.14311(17) 0.52371(14) 0.0568(13) Uani 1 1 d . . . H9 H 0.6364 -0.1441 0.5374 0.068 Uiso 1 1 calc R . . C10 C 0.5353(4) -0.15749(14) 0.47544(13) 0.0430(9) Uani 1 1 d . . . H10 H 0.6034 -0.1685 0.4570 0.052 Uiso 1 1 calc R . . N2 N 0.3816(2) -0.00194(8) 0.20960(10) 0.0249(6) Uani 1 1 d . . . C11 C 0.3344(3) 0.01974(10) 0.25525(12) 0.0283(7) Uani 1 1 d . . . H11A H 0.3558 0.0502 0.2540 0.034 Uiso 1 1 calc R . . H11B H 0.3757 0.0073 0.2845 0.034 Uiso 1 1 calc R . . C12 C 0.1936(3) 0.01461(9) 0.25953(11) 0.0239(6) Uani 1 1 d . . . H12A H 0.1643 0.0259 0.2914 0.029 Uiso 1 1 calc R . . H12B H 0.1509 0.0303 0.2329 0.029 Uiso 1 1 calc R . . O6 O 0.16600(18) -0.02950(6) 0.25592(7) 0.0219(4) Uani 1 1 d . . . C13 C 0.4972(3) -0.02727(10) 0.21992(13) 0.0301(7) Uani 1 1 d . . . H13A H 0.5592 -0.0094 0.2373 0.036 Uiso 1 1 calc R . . H13B H 0.5349 -0.0366 0.1885 0.036 Uiso 1 1 calc R . . C14 C 0.4668(3) -0.06536(10) 0.25090(13) 0.0280(7) Uani 1 1 d . . . H14A H 0.5414 -0.0839 0.2538 0.034 Uiso 1 1 calc R . . H14B H 0.4418 -0.0563 0.2843 0.034 Uiso 1 1 calc R . . O7 O 0.36743(18) -0.08760(6) 0.22816(7) 0.0213(4) Uani 1 1 d . . . C15 C 0.4027(3) 0.02980(10) 0.17102(12) 0.0284(7) Uani 1 1 d . . . C16 C 0.3029(3) 0.04295(11) 0.14267(13) 0.0335(8) Uani 1 1 d . . . H16 H 0.2225 0.0307 0.1474 0.040 Uiso 1 1 calc R . . C17 C 0.3194(4) 0.07418(12) 0.10694(13) 0.0400(9) Uani 1 1 d . . . H17 H 0.2505 0.0828 0.0872 0.048 Uiso 1 1 calc R . . C18 C 0.4339(4) 0.09236(13) 0.10034(15) 0.0472(10) Uani 1 1 d . . . H18 H 0.4450 0.1138 0.0763 0.057 Uiso 1 1 calc R . . C19 C 0.5329(4) 0.07945(14) 0.12858(19) 0.0610(13) Uani 1 1 d . . . H19 H 0.6131 0.0920 0.1239 0.073 Uiso 1 1 calc R . . C20 C 0.5177(4) 0.04809(13) 0.16423(17) 0.0489(10) Uani 1 1 d . . . H20 H 0.5871 0.0395 0.1837 0.059 Uiso 1 1 calc R . . N3 N 0.3692(2) -0.23658(8) 0.13639(9) 0.0262(6) Uani 1 1 d . . . C21 C 0.3169(3) -0.21602(11) 0.09088(11) 0.0318(8) Uani 1 1 d . . . H21A H 0.3623 -0.1892 0.0845 0.038 Uiso 1 1 calc R . . H21B H 0.3300 -0.2350 0.0624 0.038 Uiso 1 1 calc R . . C22 C 0.1792(3) -0.20694(11) 0.09635(11) 0.0305(7) Uani 1 1 d . . . H22A H 0.1499 -0.1890 0.0688 0.037 Uiso 1 1 calc R . . H22B H 0.1312 -0.2338 0.0957 0.037 Uiso 1 1 calc R . . O8 O 0.1591(2) -0.18559(7) 0.14192(7) 0.0241(5) Uani 1 1 d . . . C23 C 0.4853(3) -0.21485(10) 0.15322(12) 0.0285(7) Uani 1 1 d . . . H23A H 0.5432 -0.2115 0.1251 0.034 Uiso 1 1 calc R . . H23B H 0.5277 -0.2325 0.1783 0.034 Uiso 1 1 calc R . . C24 C 0.4560(3) -0.17168(11) 0.17484(12) 0.0291(7) Uani 1 1 d . . . H24A H 0.5326 -0.1592 0.1895 0.035 Uiso 1 1 calc R . . H24B H 0.4249 -0.1524 0.1489 0.035 Uiso 1 1 calc R . . O9 O 0.36318(18) -0.17721(6) 0.21128(7) 0.0212(4) Uani 1 1 d . . . C25 C 0.3880(3) -0.28181(10) 0.12778(11) 0.0290(7) Uani 1 1 d . . . C26 C 0.2877(3) -0.30916(11) 0.12950(12) 0.0333(8) Uani 1 1 d . . . H26 H 0.2065 -0.2983 0.1362 0.040 Uiso 1 1 calc R . . C27 C 0.3024(4) -0.35199(12) 0.12167(13) 0.0366(8) Uani 1 1 d . . . H27 H 0.2320 -0.3703 0.1236 0.044 Uiso 1 1 calc R . . C28 C 0.4187(4) -0.36808(12) 0.11106(14) 0.0415(9) Uani 1 1 d . . . H28 H 0.4294 -0.3976 0.1059 0.050 Uiso 1 1 calc R . . C29 C 0.5198(4) -0.34109(13) 0.10790(16) 0.0490(10) Uani 1 1 d . . . H29 H 0.6001 -0.3521 0.0998 0.059 Uiso 1 1 calc R . . C30 C 0.5058(4) -0.29802(12) 0.11640(14) 0.0402(9) Uani 1 1 d . . . H30 H 0.5763 -0.2797 0.1145 0.048 Uiso 1 1 calc R . . O10 O 0.1064(2) -0.11952(7) 0.40932(7) 0.0262(5) Uani 1 1 d . . . O11 O -0.03427(19) -0.08165(7) 0.36638(7) 0.0250(5) Uani 1 1 d . . . C31 C 0.0007(3) -0.10168(10) 0.40389(11) 0.0229(6) Uani 1 1 d . . . C32 C -0.0892(3) -0.10353(11) 0.44788(12) 0.0294(7) Uani 1 1 d . . . C33 C -0.2196(3) -0.08829(14) 0.43264(14) 0.0446(10) Uani 1 1 d . . . H33A H -0.2759 -0.0893 0.4610 0.067 Uiso 1 1 calc R . . H33B H -0.2524 -0.1066 0.4066 0.067 Uiso 1 1 calc R . . H33C H -0.2142 -0.0591 0.4206 0.067 Uiso 1 1 calc R . . C34 C -0.0952(4) -0.14855(12) 0.46834(14) 0.0408(9) Uani 1 1 d . . . H34A H -0.1525 -0.1493 0.4964 0.061 Uiso 1 1 calc R . . H34B H -0.0113 -0.1574 0.4789 0.061 Uiso 1 1 calc R . . H34C H -0.1258 -0.1678 0.4428 0.061 Uiso 1 1 calc R . . C35 C -0.0352(4) -0.07382(13) 0.48712(13) 0.0440(9) Uani 1 1 d . . . H35A H -0.0900 -0.0739 0.5159 0.066 Uiso 1 1 calc R . . H35B H -0.0297 -0.0450 0.4738 0.066 Uiso 1 1 calc R . . H35C H 0.0487 -0.0835 0.4966 0.066 Uiso 1 1 calc R . . O12 O 0.32827(19) -0.08023(7) 0.38464(8) 0.0242(5) Uani 1 1 d . . . O13 O 0.18747(19) -0.03142(7) 0.36062(8) 0.0242(5) Uani 1 1 d . . . C36 C 0.2829(3) -0.04329(10) 0.38450(11) 0.0238(6) Uani 1 1 d . . . C37 C 0.3442(3) -0.01059(11) 0.41843(12) 0.0299(7) Uani 1 1 d . . . C38 C 0.2708(4) -0.01338(14) 0.46725(13) 0.0464(10) Uani 1 1 d . . . H38A H 0.2784 -0.0420 0.4808 0.070 Uiso 1 1 calc R . . H38B H 0.1821 -0.0070 0.4612 0.070 Uiso 1 1 calc R . . H38C H 0.3052 0.0071 0.4907 0.070 Uiso 1 1 calc R . . C39 C 0.3301(4) 0.03360(11) 0.39807(14) 0.0396(9) Uani 1 1 d . . . H39A H 0.3699 0.0539 0.4204 0.059 Uiso 1 1 calc R . . H39B H 0.2408 0.0404 0.3947 0.059 Uiso 1 1 calc R . . H39C H 0.3704 0.0352 0.3658 0.059 Uiso 1 1 calc R . . C40 C 0.4822(4) -0.02181(14) 0.42701(17) 0.0521(11) Uani 1 1 d . . . H40A H 0.4883 -0.0506 0.4401 0.078 Uiso 1 1 calc R . . H40B H 0.5189 -0.0019 0.4505 0.078 Uiso 1 1 calc R . . H40C H 0.5278 -0.0201 0.3959 0.078 Uiso 1 1 calc R . . O14 O 0.0930(2) -0.02496(7) 0.15850(8) 0.0279(5) Uani 1 1 d . . . O15 O -0.0431(2) -0.07691(7) 0.14023(8) 0.0292(5) Uani 1 1 d . . . C41 C -0.0113(3) -0.03857(11) 0.14260(11) 0.0261(7) Uani 1 1 d . . . C42 C -0.1037(3) -0.00470(12) 0.12404(14) 0.0381(9) Uani 1 1 d . . . C43 C -0.2283(3) -0.02469(13) 0.11127(16) 0.0482(10) Uani 1 1 d . . . H43A H -0.2861 -0.0028 0.0994 0.072 Uiso 1 1 calc R . . H43B H -0.2635 -0.0382 0.1406 0.072 Uiso 1 1 calc R . . H43C H -0.2160 -0.0460 0.0856 0.072 Uiso 1 1 calc R . . C44 C -0.0436(5) 0.0137(2) 0.0771(2) 0.093(2) Uani 1 1 d . . . H44A H 0.0373 0.0266 0.0854 0.139 Uiso 1 1 calc R . . H44B H -0.0993 0.0353 0.0631 0.139 Uiso 1 1 calc R . . H44C H -0.0309 -0.0090 0.0531 0.139 Uiso 1 1 calc R . . C45 C -0.1174(4) 0.02917(15) 0.1626(2) 0.0747(17) Uani 1 1 d . . . H45A H -0.0350 0.0414 0.1700 0.112 Uiso 1 1 calc R . . H45B H -0.1527 0.0167 0.1925 0.112 Uiso 1 1 calc R . . H45C H -0.1735 0.0514 0.1505 0.112 Uiso 1 1 calc R . . O16 O 0.3158(2) -0.06040(7) 0.12844(8) 0.0275(5) Uani 1 1 d . . . O17 O 0.1814(2) -0.10533(7) 0.09223(8) 0.0288(5) Uani 1 1 d . . . C46 C 0.2734(3) -0.08006(11) 0.09175(11) 0.0273(7) Uani 1 1 d . A . C47 C 0.3371(3) -0.07140(12) 0.04202(13) 0.0366(8) Uani 1 1 d . . . C48A C 0.2755(10) -0.0995(4) 0.0015(4) 0.049(3) Uani 0.59 1 d P A 1 H48A H 0.2833 -0.1294 0.0106 0.073 Uiso 0.59 1 calc PR A 1 H48B H 0.3179 -0.0946 -0.0299 0.073 Uiso 0.59 1 calc PR A 1 H48C H 0.1866 -0.0921 -0.0017 0.073 Uiso 0.59 1 calc PR A 1 C49A C 0.3287(8) -0.0268(4) 0.0286(4) 0.047(2) Uani 0.59 1 d P A 1 H49A H 0.3701 -0.0223 -0.0030 0.070 Uiso 0.59 1 calc PR A 1 H49B H 0.3701 -0.0096 0.0539 0.070 Uiso 0.59 1 calc PR A 1 H49C H 0.2403 -0.0186 0.0261 0.070 Uiso 0.59 1 calc PR A 1 C50A C 0.4745(7) -0.0861(3) 0.0469(3) 0.062(2) Uani 0.59 1 d P A 1 H50A H 0.4765 -0.1163 0.0554 0.094 Uiso 0.59 1 calc PR A 1 H50B H 0.5164 -0.0698 0.0727 0.094 Uiso 0.59 1 calc PR A 1 H50C H 0.5180 -0.0818 0.0156 0.094 Uiso 0.59 1 calc PR A 1 C48B C 0.3313(13) -0.1070(6) 0.0100(6) 0.050(4) Uani 0.41 1 d P A 2 H48D H 0.3729 -0.1002 -0.0210 0.074 Uiso 0.41 1 calc PR A 2 H48E H 0.2434 -0.1143 0.0037 0.074 Uiso 0.41 1 calc PR A 2 H48F H 0.3737 -0.1312 0.0255 0.074 Uiso 0.41 1 calc PR A 2 C49B C 0.2625(14) -0.0290(6) 0.0247(6) 0.060(4) Uani 0.41 1 d P A 2 H49D H 0.2732 -0.0068 0.0495 0.090 Uiso 0.41 1 calc PR A 2 H49E H 0.1731 -0.0355 0.0210 0.090 Uiso 0.41 1 calc PR A 2 H49F H 0.2961 -0.0192 -0.0067 0.090 Uiso 0.41 1 calc PR A 2 C50B C 0.4739(11) -0.0547(5) 0.0515(4) 0.062(4) Uani 0.41 1 d P A 2 H50D H 0.4710 -0.0305 0.0738 0.093 Uiso 0.41 1 calc PR A 2 H50E H 0.5115 -0.0460 0.0203 0.093 Uiso 0.41 1 calc PR A 2 H50F H 0.5245 -0.0773 0.0662 0.093 Uiso 0.41 1 calc PR A 2 O18 O 0.0828(2) -0.25942(7) 0.18838(8) 0.0281(5) Uani 1 1 d . . . O19 O -0.0410(2) -0.24776(7) 0.25318(8) 0.0309(5) Uani 1 1 d . . . C51 C -0.0165(3) -0.26478(10) 0.21233(13) 0.0290(7) Uani 1 1 d . B . C52 C -0.1128(3) -0.29566(12) 0.19145(16) 0.0425(9) Uani 1 1 d . . . C53A C -0.2374(6) -0.2918(3) 0.2164(3) 0.0443(17) Uani 0.73 1 d P B 1 H53D H -0.2676 -0.2626 0.2136 0.066 Uiso 0.73 1 calc PR B 1 H53E H -0.2283 -0.2993 0.2511 0.066 Uiso 0.73 1 calc PR B 1 H53F H -0.2976 -0.3110 0.2008 0.066 Uiso 0.73 1 calc PR B 1 C54A C -0.1280(5) -0.2854(2) 0.13424(19) 0.0455(14) Uani 0.73 1 d P B 1 H54D H -0.0451 -0.2846 0.1188 0.068 Uiso 0.73 1 calc PR B 1 H54E H -0.1692 -0.2579 0.1302 0.068 Uiso 0.73 1 calc PR B 1 H54F H -0.1791 -0.3075 0.1186 0.068 Uiso 0.73 1 calc PR B 1 C55A C -0.0583(5) -0.33962(17) 0.1969(3) 0.0575(17) Uani 0.73 1 d P B 1 H55D H 0.0172 -0.3421 0.1766 0.086 Uiso 0.73 1 calc PR B 1 H55E H -0.1203 -0.3606 0.1862 0.086 Uiso 0.73 1 calc PR B 1 H55F H -0.0365 -0.3447 0.2314 0.086 Uiso 0.73 1 calc PR B 1 C53B C -0.247(2) -0.2768(7) 0.2056(9) 0.056(8) Uiso 0.27 1 d P B 2 H53A H -0.2491 -0.2710 0.2409 0.084 Uiso 0.27 1 calc PR B 2 H53B H -0.3120 -0.2974 0.1971 0.084 Uiso 0.27 1 calc PR B 2 H53C H -0.2609 -0.2505 0.1873 0.084 Uiso 0.27 1 calc PR B 2 C54B C -0.103(2) -0.3104(8) 0.1490(8) 0.078(6) Uiso 0.27 1 d P B 2 H54A H -0.1710 -0.3305 0.1429 0.117 Uiso 0.27 1 calc PR B 2 H54B H -0.0220 -0.3250 0.1459 0.117 Uiso 0.27 1 calc PR B 2 H54C H -0.1073 -0.2874 0.1251 0.117 Uiso 0.27 1 calc PR B 2 C55B C -0.107(2) -0.3361(7) 0.2357(8) 0.081(6) Uiso 0.27 1 d P B 2 H55A H -0.1078 -0.3235 0.2686 0.121 Uiso 0.27 1 calc PR B 2 H55B H -0.0297 -0.3525 0.2314 0.121 Uiso 0.27 1 calc PR B 2 H55C H -0.1796 -0.3547 0.2317 0.121 Uiso 0.27 1 calc PR B 2 O20 O 0.3113(2) -0.26497(7) 0.23709(7) 0.0244(5) Uani 1 1 d . . . O21 O 0.1870(2) -0.26877(7) 0.30333(8) 0.0267(5) Uani 1 1 d . . . C56 C 0.2755(3) -0.28206(10) 0.27671(11) 0.0242(6) Uani 1 1 d . . . C57 C 0.3404(3) -0.32327(10) 0.29213(12) 0.0302(7) Uani 1 1 d . . . C58 C 0.3492(4) -0.32646(12) 0.34765(13) 0.0395(9) Uani 1 1 d . . . H58A H 0.3908 -0.3530 0.3567 0.059 Uiso 1 1 calc R . . H58B H 0.2647 -0.3259 0.3617 0.059 Uiso 1 1 calc R . . H58C H 0.3978 -0.3025 0.3604 0.059 Uiso 1 1 calc R . . C59 C 0.2560(5) -0.35922(12) 0.27344(17) 0.0556(12) Uani 1 1 d . . . H59A H 0.2491 -0.3576 0.2376 0.083 Uiso 1 1 calc R . . H59B H 0.1724 -0.3565 0.2881 0.083 Uiso 1 1 calc R . . H59C H 0.2925 -0.3865 0.2827 0.083 Uiso 1 1 calc R . . C60 C 0.4701(4) -0.32665(14) 0.26860(17) 0.0559(12) Uani 1 1 d . . . H60A H 0.4620 -0.3243 0.2329 0.084 Uiso 1 1 calc R . . H60B H 0.5076 -0.3540 0.2770 0.084 Uiso 1 1 calc R . . H60C H 0.5238 -0.3038 0.2809 0.084 Uiso 1 1 calc R . . O22 O -0.03793(19) -0.00737(7) 0.31506(8) 0.0232(4) Uani 1 1 d . . . O23 O -0.2200(2) -0.02195(9) 0.27882(12) 0.0512(8) Uani 1 1 d . . . C61 C -0.1509(3) 0.00061(11) 0.30458(13) 0.0318(8) Uani 1 1 d . . . C62 C -0.2015(3) 0.04198(12) 0.32657(16) 0.0403(9) Uani 1 1 d . . . C63 C -0.1319(4) 0.07815(12) 0.30151(17) 0.0498(10) Uani 1 1 d . . . H63A H -0.1621 0.1052 0.3144 0.075 Uiso 1 1 calc R . . H63B H -0.1470 0.0770 0.2660 0.075 Uiso 1 1 calc R . . H63C H -0.0418 0.0755 0.3080 0.075 Uiso 1 1 calc R . . C64 C -0.1727(5) 0.04186(14) 0.38183(17) 0.0596(13) Uani 1 1 d . . . H64A H -0.2176 0.0185 0.3976 0.089 Uiso 1 1 calc R . . H64B H -0.1998 0.0687 0.3963 0.089 Uiso 1 1 calc R . . H64C H -0.0822 0.0383 0.3869 0.089 Uiso 1 1 calc R . . C65 C -0.3432(4) 0.04569(15) 0.3176(2) 0.0722(16) Uani 1 1 d . . . H65A H -0.3864 0.0221 0.3337 0.108 Uiso 1 1 calc R . . H65B H -0.3601 0.0448 0.2822 0.108 Uiso 1 1 calc R . . H65C H -0.3737 0.0725 0.3311 0.108 Uiso 1 1 calc R . . O24 O -0.0413(2) -0.15090(7) 0.08844(8) 0.0271(5) Uani 1 1 d . . . O25 O -0.2125(2) -0.18019(11) 0.12006(9) 0.0585(9) Uani 1 1 d . . . C66 C -0.1462(3) -0.16946(13) 0.08466(12) 0.0370(8) Uani 1 1 d . C . C67 C -0.1914(4) -0.17763(16) 0.03163(13) 0.0493(11) Uani 1 1 d . . . C68A C -0.0790(6) -0.1968(2) 0.0013(2) 0.0396(15) Uiso 0.59 1 d P C 1 H68A H -0.0060 -0.1780 0.0041 0.059 Uiso 0.59 1 calc PR C 1 H68B H -0.1034 -0.1993 -0.0332 0.059 Uiso 0.59 1 calc PR C 1 H68C H -0.0576 -0.2248 0.0143 0.059 Uiso 0.59 1 calc PR C 1 C69A C -0.2083(7) -0.1333(2) 0.0074(3) 0.0532(18) Uiso 0.59 1 d P C 1 H69A H -0.1307 -0.1170 0.0111 0.080 Uiso 0.59 1 calc PR C 1 H69B H -0.2773 -0.1183 0.0235 0.080 Uiso 0.59 1 calc PR C 1 H69C H -0.2275 -0.1368 -0.0275 0.080 Uiso 0.59 1 calc PR C 1 C70A C -0.3012(8) -0.2016(3) 0.0274(3) 0.065(2) Uiso 0.59 1 d P C 1 H70A H -0.3226 -0.2050 -0.0074 0.097 Uiso 0.59 1 calc PR C 1 H70B H -0.3699 -0.1870 0.0443 0.097 Uiso 0.59 1 calc PR C 1 H70C H -0.2881 -0.2295 0.0423 0.097 Uiso 0.59 1 calc PR C 1 C68B C -0.1052(13) -0.1735(5) -0.0041(5) 0.079(4) Uiso 0.41 1 d P C 2 H68D H -0.1442 -0.1792 -0.0360 0.119 Uiso 0.41 1 calc PR C 2 H68E H -0.0368 -0.1937 0.0016 0.119 Uiso 0.41 1 calc PR C 2 H68F H -0.0717 -0.1446 -0.0037 0.119 Uiso 0.41 1 calc PR C 2 C69B C -0.3150(14) -0.1509(5) 0.0267(6) 0.092(5) Uiso 0.41 1 d P C 2 H69D H -0.3675 -0.1554 0.0557 0.138 Uiso 0.41 1 calc PR C 2 H69E H -0.3610 -0.1598 -0.0028 0.138 Uiso 0.41 1 calc PR C 2 H69F H -0.2937 -0.1208 0.0240 0.138 Uiso 0.41 1 calc PR C 2 C70B C -0.2554(10) -0.2256(3) 0.0305(4) 0.049(2) Uiso 0.41 1 d P C 2 H70D H -0.3181 -0.2279 0.0566 0.073 Uiso 0.41 1 calc PR C 2 H70E H -0.1900 -0.2470 0.0356 0.073 Uiso 0.41 1 calc PR C 2 H70F H -0.2958 -0.2303 -0.0014 0.073 Uiso 0.41 1 calc PR C 2 O26 O -0.03237(19) -0.24764(7) 0.35327(8) 0.0257(5) Uani 1 1 d . . . O27 O -0.2081(2) -0.21081(8) 0.36566(10) 0.0431(7) Uani 1 1 d . . . C71 C -0.1394(3) -0.24222(10) 0.37285(12) 0.0287(7) Uani 1 1 d . D . C72 C -0.1819(3) -0.27791(11) 0.40743(14) 0.0374(8) Uani 1 1 d . . . C73A C -0.2843(7) -0.2610(2) 0.4452(3) 0.0395(16) Uiso 0.59 1 d P D 1 H73A H -0.3568 -0.2500 0.4270 0.059 Uiso 0.59 1 calc PR D 1 H73B H -0.2480 -0.2384 0.4652 0.059 Uiso 0.59 1 calc PR D 1 H73C H -0.3113 -0.2843 0.4665 0.059 Uiso 0.59 1 calc PR D 1 C74A C -0.0751(8) -0.2943(3) 0.4367(3) 0.051(2) Uiso 0.59 1 d P D 1 H74A H -0.1047 -0.3169 0.4585 0.076 Uiso 0.59 1 calc PR D 1 H74B H -0.0393 -0.2714 0.4564 0.076 Uiso 0.59 1 calc PR D 1 H74C H -0.0109 -0.3056 0.4146 0.076 Uiso 0.59 1 calc PR D 1 C75A C -0.2264(11) -0.3135(4) 0.3775(4) 0.059(3) Uiso 0.59 1 d P D 1 H75A H -0.2976 -0.3043 0.3574 0.088 Uiso 0.59 1 calc PR D 1 H75B H -0.2529 -0.3367 0.3991 0.088 Uiso 0.59 1 calc PR D 1 H75C H -0.1585 -0.3233 0.3562 0.088 Uiso 0.59 1 calc PR D 1 C73B C -0.3067(10) -0.2696(3) 0.4287(4) 0.043(3) Uiso 0.41 1 d P D 2 H73D H -0.3024 -0.2445 0.4498 0.064 Uiso 0.41 1 calc PR D 2 H73E H -0.3331 -0.2941 0.4482 0.064 Uiso 0.41 1 calc PR D 2 H73F H -0.3673 -0.2647 0.4022 0.064 Uiso 0.41 1 calc PR D 2 C74B C -0.0725(9) -0.2839(4) 0.4474(4) 0.031(2) Uiso 0.41 1 d P D 2 H74D H 0.0066 -0.2902 0.4306 0.047 Uiso 0.41 1 calc PR D 2 H74E H -0.0940 -0.3073 0.4694 0.047 Uiso 0.41 1 calc PR D 2 H74F H -0.0632 -0.2577 0.4665 0.047 Uiso 0.41 1 calc PR D 2 C75B C -0.1961(16) -0.3191(5) 0.3736(6) 0.057(4) Uiso 0.41 1 d P D 2 H75D H -0.1154 -0.3255 0.3581 0.085 Uiso 0.41 1 calc PR D 2 H75E H -0.2592 -0.3138 0.3481 0.085 Uiso 0.41 1 calc PR D 2 H75F H -0.2225 -0.3431 0.3938 0.085 Uiso 0.41 1 calc PR D 2 O28 O -0.0692(2) -0.08344(7) 0.26440(8) 0.0244(5) Uani 1 1 d D . . H281 H -0.127(3) -0.0632(11) 0.2625(14) 0.037 Uiso 1 1 d D . . H282 H -0.067(3) -0.1045(8) 0.2742(13) 0.037 Uiso 1 1 d D . . O29 O -0.0739(2) -0.15394(8) 0.19110(8) 0.0270(5) Uani 1 1 d D . . H291 H -0.135(3) -0.1652(12) 0.1714(13) 0.040 Uiso 1 1 d D . . H292 H -0.058(4) -0.1357(11) 0.2099(13) 0.040 Uiso 1 1 d D . . O30 O -0.0697(2) -0.17147(7) 0.30320(8) 0.0254(5) Uani 1 1 d D . . H301 H -0.125(3) -0.1763(12) 0.3239(12) 0.038 Uiso 1 1 d D . . H302 H -0.070(3) -0.1634(11) 0.2791(9) 0.038 Uiso 1 1 d D . . 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 Fe1 0.0183(2) 0.0174(2) 0.0160(2) -0.00010(16) -0.00115(16) 0.00046(15) Fe2 0.0193(2) 0.0199(2) 0.0156(2) -0.00077(16) -0.00176(16) 0.00240(16) Fe3 0.0176(2) 0.0187(2) 0.0190(2) -0.00048(16) -0.00074(16) 0.00150(16) Fe4 0.0206(2) 0.0206(2) 0.0192(2) 0.00207(16) -0.00008(17) 0.00188(16) Fe5 0.0215(2) 0.0255(2) 0.0166(2) -0.00135(17) -0.00285(16) 0.00314(17) Fe6 0.0222(2) 0.0202(2) 0.0176(2) -0.00270(16) -0.00123(17) 0.00136(16) Fe7 0.0189(2) 0.0199(2) 0.0205(2) 0.00053(17) -0.00039(17) -0.00078(16) O1 0.0192(10) 0.0202(10) 0.0164(9) -0.0008(8) -0.0009(8) 0.0029(8) O2 0.0232(11) 0.0210(11) 0.0180(10) 0.0011(8) -0.0035(8) -0.0002(8) O3 0.0190(10) 0.0205(10) 0.0188(10) -0.0019(8) -0.0004(8) -0.0012(8) N1 0.0255(14) 0.0230(13) 0.0212(13) 0.0003(10) -0.0043(10) 0.0021(10) C1 0.0201(15) 0.0328(18) 0.0247(16) 0.0007(13) -0.0038(12) 0.0081(13) C2 0.0237(16) 0.0304(17) 0.0258(16) -0.0024(13) -0.0044(13) 0.0087(13) O4 0.0184(10) 0.0209(11) 0.0180(10) -0.0012(8) -0.0005(8) 0.0029(8) C3 0.0333(18) 0.0254(17) 0.0307(17) 0.0024(14) -0.0082(14) 0.0011(13) C4 0.0323(18) 0.0245(16) 0.0212(15) 0.0039(13) -0.0028(13) 0.0005(13) O5 0.0239(11) 0.0225(11) 0.0201(10) 0.0033(8) -0.0032(8) -0.0020(8) C5 0.0294(17) 0.0254(16) 0.0208(15) 0.0013(12) -0.0049(13) -0.0024(13) C6 0.038(2) 0.055(2) 0.0250(17) -0.0041(16) -0.0092(15) 0.0097(17) C7 0.056(3) 0.052(3) 0.0258(18) -0.0034(17) 0.0002(17) 0.0128(19) C8 0.058(3) 0.059(3) 0.0193(17) -0.0039(16) -0.0052(17) -0.021(2) C9 0.035(2) 0.108(4) 0.0264(19) -0.002(2) -0.0101(17) -0.017(2) C10 0.034(2) 0.070(3) 0.0254(18) -0.0020(18) -0.0040(15) -0.0024(18) N2 0.0231(14) 0.0213(13) 0.0303(14) 0.0045(11) 0.0038(11) 0.0011(10) C11 0.0310(18) 0.0221(16) 0.0318(17) 0.0018(13) -0.0002(14) -0.0012(13) C12 0.0281(16) 0.0167(15) 0.0268(16) -0.0009(12) 0.0013(13) 0.0002(12) O6 0.0238(11) 0.0185(10) 0.0234(11) 0.0003(8) 0.0022(9) -0.0012(8) C13 0.0238(17) 0.0262(17) 0.0402(19) 0.0048(14) 0.0003(14) -0.0010(13) C14 0.0216(16) 0.0250(16) 0.0373(18) 0.0038(14) -0.0063(14) -0.0004(12) O7 0.0199(10) 0.0207(11) 0.0232(10) 0.0020(8) -0.0010(8) 0.0010(8) C15 0.0325(18) 0.0230(16) 0.0298(17) 0.0059(13) 0.0091(14) 0.0031(13) C16 0.040(2) 0.0271(18) 0.0334(18) 0.0059(14) 0.0026(15) -0.0058(15) C17 0.057(2) 0.031(2) 0.0324(19) 0.0077(15) 0.0039(17) 0.0047(17) C18 0.056(3) 0.035(2) 0.051(2) 0.0153(18) 0.026(2) 0.0087(18) C19 0.043(3) 0.049(3) 0.091(4) 0.034(3) 0.022(2) -0.0011(19) C20 0.034(2) 0.048(2) 0.065(3) 0.023(2) 0.0079(19) 0.0018(17) N3 0.0302(15) 0.0260(14) 0.0224(13) -0.0027(11) 0.0001(11) 0.0052(11) C21 0.044(2) 0.0322(19) 0.0193(15) 0.0005(13) 0.0000(14) 0.0082(15) C22 0.0382(19) 0.0354(19) 0.0178(15) -0.0051(13) -0.0053(13) 0.0092(15) O8 0.0268(12) 0.0267(12) 0.0187(10) -0.0040(9) -0.0020(9) 0.0056(9) C23 0.0259(17) 0.0302(18) 0.0293(17) -0.0047(14) 0.0060(13) 0.0023(13) C24 0.0281(17) 0.0330(18) 0.0264(16) -0.0045(14) 0.0151(13) -0.0001(13) O9 0.0204(10) 0.0220(11) 0.0214(10) -0.0015(8) 0.0030(8) 0.0008(8) C25 0.0399(19) 0.0280(17) 0.0192(15) -0.0055(13) -0.0025(13) 0.0083(14) C26 0.0349(19) 0.0338(19) 0.0313(18) -0.0096(15) 0.0012(15) 0.0050(15) C27 0.041(2) 0.035(2) 0.0334(19) -0.0066(15) -0.0073(16) 0.0027(15) C28 0.053(2) 0.033(2) 0.039(2) -0.0111(16) -0.0097(18) 0.0129(17) C29 0.042(2) 0.041(2) 0.064(3) -0.014(2) 0.000(2) 0.0158(18) C30 0.038(2) 0.036(2) 0.047(2) -0.0103(17) 0.0012(17) 0.0047(16) O10 0.0254(12) 0.0345(13) 0.0186(10) 0.0007(9) 0.0009(9) 0.0058(9) O11 0.0210(11) 0.0317(12) 0.0223(11) 0.0038(9) 0.0029(9) 0.0014(9) C31 0.0233(16) 0.0248(16) 0.0207(15) -0.0029(12) 0.0019(12) 0.0001(12) C32 0.0263(17) 0.0360(19) 0.0258(16) 0.0044(14) 0.0052(13) 0.0054(14) C33 0.0280(19) 0.064(3) 0.042(2) 0.0145(19) 0.0108(16) 0.0122(17) C34 0.047(2) 0.038(2) 0.037(2) 0.0089(16) 0.0139(17) -0.0008(17) C35 0.047(2) 0.056(3) 0.0295(19) -0.0094(17) 0.0098(17) 0.0011(19) O12 0.0229(11) 0.0247(11) 0.0248(11) -0.0049(9) -0.0043(9) 0.0040(9) O13 0.0228(11) 0.0245(11) 0.0252(11) -0.0034(9) -0.0055(9) 0.0031(9) C36 0.0210(15) 0.0256(16) 0.0246(15) -0.0014(13) 0.0004(12) -0.0002(12) C37 0.0296(18) 0.0273(17) 0.0326(18) -0.0087(14) -0.0071(14) 0.0011(13) C38 0.062(3) 0.047(2) 0.0295(19) -0.0143(17) -0.0040(18) -0.0051(19) C39 0.047(2) 0.0274(19) 0.044(2) -0.0085(16) -0.0115(17) -0.0052(16) C40 0.033(2) 0.047(2) 0.076(3) -0.027(2) -0.019(2) 0.0008(17) O14 0.0259(12) 0.0285(12) 0.0294(12) 0.0068(10) -0.0035(9) 0.0030(9) O15 0.0256(12) 0.0325(13) 0.0295(12) -0.0007(10) -0.0065(9) 0.0051(9) C41 0.0250(17) 0.0325(18) 0.0206(15) 0.0023(13) 0.0026(13) 0.0068(13) C42 0.0256(18) 0.039(2) 0.049(2) 0.0138(17) -0.0021(16) 0.0092(15) C43 0.031(2) 0.053(3) 0.061(3) 0.008(2) -0.0162(18) 0.0130(18) C44 0.049(3) 0.135(6) 0.094(4) 0.089(4) -0.003(3) 0.015(3) C45 0.051(3) 0.041(3) 0.133(5) -0.023(3) -0.028(3) 0.019(2) O16 0.0300(12) 0.0314(13) 0.0212(11) 0.0030(9) 0.0029(9) -0.0006(9) O17 0.0330(13) 0.0335(13) 0.0198(11) 0.0009(9) 0.0009(9) 0.0001(10) C46 0.0257(17) 0.0337(18) 0.0224(16) 0.0033(13) 0.0026(13) 0.0083(13) C47 0.037(2) 0.047(2) 0.0254(17) 0.0077(16) 0.0069(15) 0.0024(16) C48A 0.080(8) 0.047(5) 0.019(4) -0.009(3) 0.019(5) -0.003(6) C49A 0.057(6) 0.050(5) 0.034(4) 0.009(3) 0.015(5) 0.003(5) C50A 0.039(4) 0.096(7) 0.053(5) 0.020(5) 0.017(4) 0.023(5) C48B 0.047(9) 0.068(10) 0.034(8) -0.004(6) 0.017(6) -0.008(7) C49B 0.077(10) 0.072(9) 0.031(6) 0.026(6) 0.014(8) 0.020(10) C50B 0.047(7) 0.098(11) 0.040(6) -0.016(7) 0.021(5) -0.026(7) O18 0.0274(12) 0.0282(12) 0.0289(12) -0.0074(10) -0.0011(10) -0.0022(9) O19 0.0256(12) 0.0360(13) 0.0313(12) -0.0088(10) 0.0016(10) -0.0079(10) C51 0.0253(17) 0.0225(16) 0.0391(19) -0.0031(14) -0.0078(14) 0.0010(13) C52 0.0283(19) 0.040(2) 0.059(2) -0.0206(19) -0.0102(17) -0.0061(16) C53A 0.031(3) 0.056(5) 0.045(4) -0.021(4) 0.001(3) -0.022(3) C54A 0.041(3) 0.060(4) 0.035(3) -0.023(3) -0.011(2) -0.009(3) C55A 0.047(3) 0.029(3) 0.097(5) -0.015(3) -0.010(3) -0.016(2) O20 0.0296(12) 0.0206(11) 0.0229(11) -0.0002(9) -0.0005(9) 0.0029(9) O21 0.0269(12) 0.0245(12) 0.0286(11) 0.0042(9) 0.0040(9) 0.0041(9) C56 0.0243(16) 0.0215(15) 0.0269(16) -0.0012(13) -0.0033(13) -0.0026(12) C57 0.0368(19) 0.0214(16) 0.0324(17) 0.0060(14) 0.0035(15) 0.0063(13) C58 0.055(2) 0.032(2) 0.0312(19) 0.0060(15) -0.0062(17) 0.0124(17) C59 0.087(3) 0.023(2) 0.056(3) -0.0022(18) -0.024(2) -0.0001(19) C60 0.050(3) 0.055(3) 0.063(3) 0.025(2) 0.022(2) 0.030(2) O22 0.0193(11) 0.0232(11) 0.0271(11) -0.0027(9) -0.0017(9) 0.0032(8) O23 0.0283(14) 0.0402(16) 0.085(2) -0.0286(15) -0.0232(14) 0.0121(11) C61 0.0260(18) 0.0268(18) 0.043(2) -0.0015(15) 0.0028(15) 0.0041(13) C62 0.0259(18) 0.0293(19) 0.066(3) -0.0101(18) 0.0038(17) 0.0043(14) C63 0.049(2) 0.028(2) 0.072(3) -0.0052(19) 0.000(2) 0.0088(17) C64 0.075(3) 0.042(2) 0.062(3) -0.023(2) 0.031(2) -0.008(2) C65 0.034(2) 0.049(3) 0.134(5) -0.023(3) 0.002(3) 0.0121(19) O24 0.0264(12) 0.0345(13) 0.0205(11) -0.0028(9) -0.0042(9) 0.0029(10) O25 0.0359(16) 0.113(3) 0.0271(14) -0.0091(15) -0.0027(12) -0.0287(16) C66 0.0304(19) 0.057(2) 0.0232(17) -0.0046(16) -0.0042(14) 0.0029(17) C67 0.041(2) 0.081(3) 0.0262(19) -0.0072(19) -0.0105(16) -0.010(2) O26 0.0204(11) 0.0270(12) 0.0298(11) 0.0068(9) 0.0027(9) -0.0017(9) O27 0.0285(13) 0.0391(15) 0.0617(17) 0.0203(13) 0.0152(12) 0.0092(11) C71 0.0245(17) 0.0268(17) 0.0346(18) 0.0057(14) 0.0002(14) -0.0007(13) C72 0.0295(19) 0.0316(19) 0.051(2) 0.0164(17) 0.0090(16) 0.0004(14) O28 0.0227(11) 0.0224(12) 0.0282(12) -0.0025(9) -0.0027(9) 0.0035(9) O29 0.0243(12) 0.0373(14) 0.0193(11) -0.0056(9) -0.0021(9) -0.0007(10) O30 0.0243(12) 0.0245(12) 0.0275(12) 0.0072(10) 0.0032(10) 0.0018(9) _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 Fe1 O1 1.9901(19) . ? Fe1 O4 1.995(2) . ? Fe1 O7 1.999(2) . ? Fe1 O2 1.9996(19) . ? Fe1 O9 2.000(2) . ? Fe1 O3 2.003(2) . ? Fe1 Fe6 2.9684(6) . ? Fe1 Fe4 2.9728(6) . ? Fe1 Fe2 2.9736(6) . ? Fe2 O1 1.8909(19) . ? Fe2 O4 1.972(2) . ? Fe2 O5 1.997(2) . ? Fe2 O12 2.019(2) . ? Fe2 O10 2.034(2) . ? Fe2 N1 2.346(2) . ? Fe3 O1 1.866(2) . ? Fe3 O6 1.987(2) . ? Fe3 O22 2.014(2) . ? Fe3 O13 2.049(2) . ? Fe3 O11 2.065(2) . ? Fe3 O28 2.091(2) . ? Fe4 O2 1.894(2) . ? Fe4 O7 1.970(2) . ? Fe4 O6 1.997(2) . ? Fe4 O16 2.014(2) . ? Fe4 O14 2.038(2) . ? Fe4 N2 2.355(3) . ? Fe5 O2 1.8702(19) . ? Fe5 O8 1.994(2) . ? Fe5 O24 2.015(2) . ? Fe5 O17 2.041(2) . ? Fe5 O15 2.069(2) . ? Fe5 O29 2.100(2) . ? Fe6 O3 1.892(2) . ? Fe6 O9 1.974(2) . ? Fe6 O8 2.006(2) . ? Fe6 O20 2.011(2) . ? Fe6 O18 2.035(2) . ? Fe6 N3 2.360(3) . ? Fe7 O3 1.873(2) . ? Fe7 O5 1.989(2) . ? Fe7 O26 2.023(2) . ? Fe7 O21 2.048(2) . ? Fe7 O19 2.051(2) . ? Fe7 O30 2.083(2) . ? N1 C5 1.461(4) . ? N1 C1 1.498(4) . ? N1 C3 1.510(4) . ? C1 C2 1.512(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O4 1.412(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.507(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O5 1.435(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C10 1.375(5) . ? C5 C6 1.385(5) . ? C6 C7 1.393(5) . ? C6 H6 0.9500 . ? C7 C8 1.362(6) . ? C7 H7 0.9500 . ? C8 C9 1.343(6) . ? C8 H8 0.9500 . ? C9 C10 1.405(5) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? N2 C15 1.470(4) . ? N2 C13 1.495(4) . ? N2 C11 1.507(4) . ? C11 C12 1.514(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O6 1.428(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.505(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O7 1.413(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.368(5) . ? C15 C16 1.377(5) . ? C16 C17 1.397(5) . ? C16 H16 0.9500 . ? C17 C18 1.362(6) . ? C17 H17 0.9500 . ? C18 C19 1.367(6) . ? C18 H18 0.9500 . ? C19 C20 1.397(6) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? N3 C25 1.462(4) . ? N3 C23 1.487(4) . ? N3 C21 1.506(4) . ? C21 C22 1.503(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O8 1.429(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.518(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O9 1.413(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.376(5) . ? C25 C30 1.391(5) . ? C26 C27 1.379(5) . ? C26 H26 0.9500 . ? C27 C28 1.372(5) . ? C27 H27 0.9500 . ? C28 C29 1.377(6) . ? C28 H28 0.9500 . ? C29 C30 1.388(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? O10 C31 1.269(4) . ? O11 C31 1.258(4) . ? C31 C32 1.537(4) . ? C32 C33 1.528(5) . ? C32 C34 1.529(5) . ? C32 C35 1.534(5) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? O12 C36 1.263(4) . ? O13 C36 1.263(4) . ? C36 C37 1.532(4) . ? C37 C39 1.510(5) . ? C37 C40 1.531(5) . ? C37 C38 1.547(5) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? O14 C41 1.268(4) . ? O15 C41 1.260(4) . ? C41 C42 1.539(4) . ? C42 C45 1.507(6) . ? C42 C43 1.511(5) . ? C42 C44 1.545(6) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? O16 C46 1.260(4) . ? O17 C46 1.265(4) . ? C46 C47 1.541(4) . ? C47 C48B 1.425(19) . ? C47 C49A 1.457(11) . ? C47 C50A 1.543(8) . ? C47 C48A 1.560(11) . ? C47 C50B 1.571(11) . ? C47 C49B 1.626(16) . ? C48A H48A 0.9800 . ? C48A H48B 0.9800 . ? C48A H48C 0.9800 . ? C49A H49A 0.9800 . ? C49A H49B 0.9800 . ? C49A H49C 0.9800 . ? C50A H50A 0.9800 . ? C50A H50B 0.9800 . ? C50A H50C 0.9800 . ? C48B H48D 0.9800 . ? C48B H48E 0.9800 . ? C48B H48F 0.9800 . ? C49B H49D 0.9800 . ? C49B H49E 0.9800 . ? C49B H49F 0.9800 . ? C50B H50D 0.9800 . ? C50B H50E 0.9800 . ? C50B H50F 0.9800 . ? O18 C51 1.256(4) . ? O19 C51 1.264(4) . ? C51 C52 1.526(4) . ? C52 C54B 1.25(2) . ? C52 C53A 1.497(7) . ? C52 C55A 1.513(7) . ? C52 C53B 1.59(2) . ? C52 C54A 1.599(7) . ? C52 C55B 1.76(2) . ? C53A H53D 0.9800 . ? C53A H53E 0.9800 . ? C53A H53F 0.9800 . ? C54A H54D 0.9800 . ? C54A H54E 0.9800 . ? C54A H54F 0.9800 . ? C55A H55D 0.9800 . ? C55A H55E 0.9800 . ? C55A H55F 0.9800 . ? C53B H53A 0.9800 . ? C53B H53B 0.9800 . ? C53B H53C 0.9800 . ? C54B H54A 0.9800 . ? C54B H54B 0.9800 . ? C54B H54C 0.9800 . ? C55B H55A 0.9800 . ? C55B H55B 0.9800 . ? C55B H55C 0.9800 . ? O20 C56 1.266(4) . ? O21 C56 1.263(4) . ? C56 C57 1.533(4) . ? C57 C58 1.518(5) . ? C57 C60 1.528(5) . ? C57 C59 1.535(5) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? O22 C61 1.263(4) . ? O23 C61 1.241(4) . ? C61 C62 1.536(5) . ? C62 C63 1.524(6) . ? C62 C65 1.535(5) . ? C62 C64 1.535(6) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? O24 C66 1.267(4) . ? O25 C66 1.244(4) . ? C66 C67 1.543(5) . ? C67 C68B 1.346(14) . ? C67 C70A 1.398(9) . ? C67 C69A 1.557(9) . ? C67 C69B 1.571(16) . ? C67 C68A 1.577(8) . ? C67 C70B 1.663(11) . ? C68A H68A 0.9800 . ? C68A H68B 0.9800 . ? C68A H68C 0.9800 . ? C69A H69A 0.9800 . ? C69A H69B 0.9800 . ? C69A H69C 0.9800 . ? C70A H70A 0.9800 . ? C70A H70B 0.9800 . ? C70A H70C 0.9800 . ? C68B H68D 0.9800 . ? C68B H68E 0.9800 . ? C68B H68F 0.9800 . ? C69B H69D 0.9800 . ? C69B H69E 0.9800 . ? C69B H69F 0.9800 . ? C70B H70D 0.9800 . ? C70B H70E 0.9800 . ? C70B H70F 0.9800 . ? O26 C71 1.272(4) . ? O27 C71 1.249(4) . ? C71 C72 1.538(5) . ? C72 C75A 1.467(12) . ? C72 C73B 1.476(11) . ? C72 C74A 1.482(9) . ? C72 C73A 1.593(8) . ? C72 C75B 1.602(17) . ? C72 C74B 1.604(11) . ? C73A H73A 0.9800 . ? C73A H73B 0.9800 . ? C73A H73C 0.9800 . ? C74A H74A 0.9800 . ? C74A H74B 0.9800 . ? C74A H74C 0.9800 . ? C75A H75A 0.9800 . ? C75A H75B 0.9800 . ? C75A H75C 0.9800 . ? C73B H73D 0.9800 . ? C73B H73E 0.9800 . ? C73B H73F 0.9800 . ? C74B H74D 0.9800 . ? C74B H74E 0.9800 . ? C74B H74F 0.9800 . ? C75B H75D 0.9800 . ? C75B H75E 0.9800 . ? C75B H75F 0.9800 . ? O28 H281 0.89(3) . ? O28 H282 0.72(2) . ? O29 H291 0.91(3) . ? O29 H292 0.79(3) . ? O30 H301 0.83(3) . ? O30 H302 0.70(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 O1 Fe1 O4 77.67(8) . . ? O1 Fe1 O7 101.76(8) . . ? O4 Fe1 O7 90.87(8) . . ? O1 Fe1 O2 91.52(8) . . ? O4 Fe1 O2 162.31(8) . . ? O7 Fe1 O2 77.53(8) . . ? O1 Fe1 O9 162.71(8) . . ? O4 Fe1 O9 91.44(8) . . ? O7 Fe1 O9 91.68(8) . . ? O2 Fe1 O9 102.08(8) . . ? O1 Fe1 O3 91.15(8) . . ? O4 Fe1 O3 102.16(8) . . ? O7 Fe1 O3 163.40(8) . . ? O2 Fe1 O3 91.89(8) . . ? O9 Fe1 O3 77.90(8) . . ? O1 Fe1 Fe6 130.04(6) . . ? O4 Fe1 Fe6 109.41(6) . . ? O7 Fe1 Fe6 126.72(6) . . ? O2 Fe1 Fe6 88.27(6) . . ? O9 Fe1 Fe6 41.33(6) . . ? O3 Fe1 Fe6 38.98(6) . . ? O1 Fe1 Fe4 87.61(6) . . ? O4 Fe1 Fe4 125.48(6) . . ? O7 Fe1 Fe4 41.12(6) . . ? O2 Fe1 Fe4 38.93(6) . . ? O9 Fe1 Fe4 109.68(6) . . ? O3 Fe1 Fe4 130.68(6) . . ? Fe6 Fe1 Fe4 119.684(18) . . ? O1 Fe1 Fe2 38.77(5) . . ? O4 Fe1 Fe2 41.14(6) . . ? O7 Fe1 Fe2 108.39(6) . . ? O2 Fe1 Fe2 130.25(6) . . ? O9 Fe1 Fe2 126.37(6) . . ? O3 Fe1 Fe2 88.22(6) . . ? Fe6 Fe1 Fe2 119.344(18) . . ? Fe4 Fe1 Fe2 118.112(18) . . ? O1 Fe2 O4 80.60(8) . . ? O1 Fe2 O5 99.27(8) . . ? O4 Fe2 O5 93.82(9) . . ? O1 Fe2 O12 99.42(9) . . ? O4 Fe2 O12 94.25(8) . . ? O5 Fe2 O12 160.62(9) . . ? O1 Fe2 O10 97.61(8) . . ? O4 Fe2 O10 178.17(9) . . ? O5 Fe2 O10 86.81(9) . . ? O12 Fe2 O10 85.67(9) . . ? O1 Fe2 N1 158.93(9) . . ? O4 Fe2 N1 78.62(8) . . ? O5 Fe2 N1 78.77(9) . . ? O12 Fe2 N1 85.60(9) . . ? O10 Fe2 N1 103.19(9) . . ? O1 Fe2 Fe1 41.23(6) . . ? O4 Fe2 Fe1 41.73(6) . . ? O5 Fe2 Fe1 87.83(6) . . ? O12 Fe2 Fe1 109.76(6) . . ? O10 Fe2 Fe1 136.65(6) . . ? N1 Fe2 Fe1 117.81(6) . . ? O1 Fe3 O6 95.13(8) . . ? O1 Fe3 O22 174.30(9) . . ? O6 Fe3 O22 88.69(9) . . ? O1 Fe3 O13 96.83(8) . . ? O6 Fe3 O13 90.24(8) . . ? O22 Fe3 O13 87.37(8) . . ? O1 Fe3 O11 92.20(9) . . ? O6 Fe3 O11 172.58(9) . . ? O22 Fe3 O11 84.08(9) . . ? O13 Fe3 O11 87.76(9) . . ? O1 Fe3 O28 89.74(9) . . ? O6 Fe3 O28 96.37(9) . . ? O22 Fe3 O28 85.62(8) . . ? O13 Fe3 O28 170.25(9) . . ? O11 Fe3 O28 84.78(9) . . ? O2 Fe4 O7 80.75(8) . . ? O2 Fe4 O6 99.33(8) . . ? O7 Fe4 O6 95.03(8) . . ? O2 Fe4 O16 100.43(9) . . ? O7 Fe4 O16 93.44(9) . . ? O6 Fe4 O16 159.51(9) . . ? O2 Fe4 O14 97.34(9) . . ? O7 Fe4 O14 177.66(9) . . ? O6 Fe4 O14 86.59(9) . . ? O16 Fe4 O14 85.58(9) . . ? O2 Fe4 N2 158.98(9) . . ? O7 Fe4 N2 78.66(9) . . ? O6 Fe4 N2 78.40(9) . . ? O16 Fe4 N2 85.04(9) . . ? O14 Fe4 N2 103.34(9) . . ? O2 Fe4 Fe1 41.56(6) . . ? O7 Fe4 Fe1 41.85(6) . . ? O6 Fe4 Fe1 87.97(6) . . ? O16 Fe4 Fe1 110.55(7) . . ? O14 Fe4 Fe1 136.69(7) . . ? N2 Fe4 Fe1 117.50(6) . . ? O2 Fe5 O8 95.59(9) . . ? O2 Fe5 O24 174.70(9) . . ? O8 Fe5 O24 88.84(9) . . ? O2 Fe5 O17 96.34(9) . . ? O8 Fe5 O17 91.25(9) . . ? O24 Fe5 O17 86.45(9) . . ? O2 Fe5 O15 91.65(9) . . ? O8 Fe5 O15 172.72(9) . . ? O24 Fe5 O15 83.90(9) . . ? O17 Fe5 O15 88.71(9) . . ? O2 Fe5 O29 90.30(9) . . ? O8 Fe5 O29 94.05(9) . . ? O24 Fe5 O29 86.48(9) . . ? O17 Fe5 O29 171.07(9) . . ? O15 Fe5 O29 85.12(9) . . ? O3 Fe6 O9 81.22(8) . . ? O3 Fe6 O8 100.34(8) . . ? O9 Fe6 O8 93.16(9) . . ? O3 Fe6 O20 99.66(8) . . ? O9 Fe6 O20 93.99(9) . . ? O8 Fe6 O20 159.56(8) . . ? O3 Fe6 O18 96.84(9) . . ? O9 Fe6 O18 178.03(9) . . ? O8 Fe6 O18 86.82(9) . . ? O20 Fe6 O18 86.69(9) . . ? O3 Fe6 N3 159.98(9) . . ? O9 Fe6 N3 78.96(9) . . ? O8 Fe6 N3 78.06(9) . . ? O20 Fe6 N3 84.55(9) . . ? O18 Fe6 N3 102.95(9) . . ? O3 Fe6 Fe1 41.76(6) . . ? O9 Fe6 Fe1 42.01(6) . . ? O8 Fe6 Fe1 87.66(6) . . ? O20 Fe6 Fe1 110.26(6) . . ? O18 Fe6 Fe1 136.03(6) . . ? N3 Fe6 Fe1 118.40(7) . . ? O3 Fe7 O5 95.92(8) . . ? O3 Fe7 O26 174.14(9) . . ? O5 Fe7 O26 88.95(9) . . ? O3 Fe7 O21 96.76(9) . . ? O5 Fe7 O21 89.96(9) . . ? O26 Fe7 O21 86.48(9) . . ? O3 Fe7 O19 91.14(9) . . ? O5 Fe7 O19 172.92(9) . . ? O26 Fe7 O19 84.03(9) . . ? O21 Fe7 O19 88.63(9) . . ? O3 Fe7 O30 90.52(9) . . ? O5 Fe7 O30 95.77(9) . . ? O26 Fe7 O30 85.74(9) . . ? O21 Fe7 O30 170.24(9) . . ? O19 Fe7 O30 84.72(9) . . ? Fe3 O1 Fe2 119.87(10) . . ? Fe3 O1 Fe1 133.86(10) . . ? Fe2 O1 Fe1 99.99(9) . . ? Fe5 O2 Fe4 119.94(10) . . ? Fe5 O2 Fe1 133.28(11) . . ? Fe4 O2 Fe1 99.51(9) . . ? Fe7 O3 Fe6 120.45(11) . . ? Fe7 O3 Fe1 132.85(10) . . ? Fe6 O3 Fe1 99.26(9) . . ? C5 N1 C1 112.0(2) . . ? C5 N1 C3 109.7(2) . . ? C1 N1 C3 111.0(2) . . ? C5 N1 Fe2 117.56(19) . . ? C1 N1 Fe2 101.78(17) . . ? C3 N1 Fe2 104.30(17) . . ? N1 C1 C2 110.8(2) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? O4 C2 C1 107.9(2) . . ? O4 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? O4 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? C2 O4 Fe2 119.81(18) . . ? C2 O4 Fe1 132.87(18) . . ? Fe2 O4 Fe1 97.13(9) . . ? C4 C3 N1 110.8(3) . . ? C4 C3 H3A 109.5 . . ? N1 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? O5 C4 C3 108.2(3) . . ? O5 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? O5 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? C4 O5 Fe7 120.69(18) . . ? C4 O5 Fe2 112.44(17) . . ? Fe7 O5 Fe2 126.87(10) . . ? C10 C5 C6 118.8(3) . . ? C10 C5 N1 121.9(3) . . ? C6 C5 N1 119.3(3) . . ? C5 C6 C7 120.0(3) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C8 C7 C6 121.0(4) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C9 C8 C7 119.1(3) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 121.7(4) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C5 C10 C9 119.4(4) . . ? C5 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C15 N2 C13 111.8(2) . . ? C15 N2 C11 109.4(2) . . ? C13 N2 C11 111.4(3) . . ? C15 N2 Fe4 118.2(2) . . ? C13 N2 Fe4 101.43(18) . . ? C11 N2 Fe4 104.18(17) . . ? N2 C11 C12 110.4(3) . . ? N2 C11 H11A 109.6 . . ? C12 C11 H11A 109.6 . . ? N2 C11 H11B 109.6 . . ? C12 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? O6 C12 C11 107.7(2) . . ? O6 C12 H12A 110.2 . . ? C11 C12 H12A 110.2 . . ? O6 C12 H12B 110.2 . . ? C11 C12 H12B 110.2 . . ? H12A C12 H12B 108.5 . . ? C12 O6 Fe3 120.49(17) . . ? C12 O6 Fe4 112.83(17) . . ? Fe3 O6 Fe4 126.66(11) . . ? N2 C13 C14 110.8(3) . . ? N2 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? O7 C14 C13 108.3(3) . . ? O7 C14 H14A 110.0 . . ? C13 C14 H14A 110.0 . . ? O7 C14 H14B 110.0 . . ? C13 C14 H14B 110.0 . . ? H14A C14 H14B 108.4 . . ? C14 O7 Fe4 119.42(18) . . ? C14 O7 Fe1 132.24(19) . . ? Fe4 O7 Fe1 97.03(9) . . ? C20 C15 C16 119.2(3) . . ? C20 C15 N2 121.6(3) . . ? C16 C15 N2 119.2(3) . . ? C15 C16 C17 120.4(3) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 120.3(4) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 119.4(4) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C18 C19 C20 120.8(4) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C15 C20 C19 120.0(4) . . ? C15 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C25 N3 C23 112.7(3) . . ? C25 N3 C21 109.9(2) . . ? C23 N3 C21 111.2(3) . . ? C25 N3 Fe6 116.4(2) . . ? C23 N3 Fe6 101.46(18) . . ? C21 N3 Fe6 104.71(18) . . ? C22 C21 N3 111.1(3) . . ? C22 C21 H21A 109.4 . . ? N3 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? N3 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? O8 C22 C21 108.9(3) . . ? O8 C22 H22A 109.9 . . ? C21 C22 H22A 109.9 . . ? O8 C22 H22B 109.9 . . ? C21 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C22 O8 Fe5 121.05(18) . . ? C22 O8 Fe6 112.22(18) . . ? Fe5 O8 Fe6 126.68(10) . . ? N3 C23 C24 111.3(3) . . ? N3 C23 H23A 109.4 . . ? C24 C23 H23A 109.4 . . ? N3 C23 H23B 109.4 . . ? C24 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? O9 C24 C23 107.8(3) . . ? O9 C24 H24A 110.1 . . ? C23 C24 H24A 110.1 . . ? O9 C24 H24B 110.1 . . ? C23 C24 H24B 110.1 . . ? H24A C24 H24B 108.5 . . ? C24 O9 Fe6 118.69(18) . . ? C24 O9 Fe1 132.43(19) . . ? Fe6 O9 Fe1 96.66(9) . . ? C26 C25 C30 118.6(3) . . ? C26 C25 N3 120.1(3) . . ? C30 C25 N3 121.3(3) . . ? C25 C26 C27 121.5(3) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C28 C27 C26 119.9(4) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 119.4(4) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C28 C29 C30 120.8(4) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C29 C30 C25 119.7(4) . . ? C29 C30 H30 120.2 . . ? C25 C30 H30 120.2 . . ? C31 O10 Fe2 130.25(19) . . ? C31 O11 Fe3 128.78(19) . . ? O11 C31 O10 125.5(3) . . ? O11 C31 C32 117.9(3) . . ? O10 C31 C32 116.6(3) . . ? C33 C32 C34 110.7(3) . . ? C33 C32 C35 109.6(3) . . ? C34 C32 C35 109.4(3) . . ? C33 C32 C31 110.2(3) . . ? C34 C32 C31 110.3(3) . . ? C35 C32 C31 106.6(3) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C36 O12 Fe2 125.76(19) . . ? C36 O13 Fe3 134.9(2) . . ? O13 C36 O12 125.7(3) . . ? O13 C36 C37 116.9(3) . . ? O12 C36 C37 117.3(3) . . ? C39 C37 C40 111.4(3) . . ? C39 C37 C36 111.1(3) . . ? C40 C37 C36 110.2(3) . . ? C39 C37 C38 108.5(3) . . ? C40 C37 C38 110.1(3) . . ? C36 C37 C38 105.3(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C41 O14 Fe4 130.3(2) . . ? C41 O15 Fe5 129.4(2) . . ? O15 C41 O14 125.4(3) . . ? O15 C41 C42 118.7(3) . . ? O14 C41 C42 115.9(3) . . ? C45 C42 C43 111.8(3) . . ? C45 C42 C41 109.1(3) . . ? C43 C42 C41 110.3(3) . . ? C45 C42 C44 110.5(4) . . ? C43 C42 C44 109.5(4) . . ? C41 C42 C44 105.6(3) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C46 O16 Fe4 126.2(2) . . ? C46 O17 Fe5 136.1(2) . . ? O16 C46 O17 125.5(3) . . ? O16 C46 C47 116.8(3) . . ? O17 C46 C47 117.7(3) . . ? C48B C47 C46 112.2(8) . . ? C49A C47 C46 111.4(5) . . ? C49A C47 C50A 111.8(6) . . ? C46 C47 C50A 106.9(4) . . ? C49A C47 C48A 110.3(6) . . ? C46 C47 C48A 109.6(5) . . ? C50A C47 C48A 106.7(6) . . ? C48B C47 C50B 113.8(8) . . ? C46 C47 C50B 109.1(5) . . ? C48B C47 C49B 116.9(9) . . ? C46 C47 C49B 100.6(6) . . ? C50B C47 C49B 103.0(9) . . ? C47 C48A H48A 109.5 . . ? C47 C48A H48B 109.5 . . ? H48A C48A H48B 109.5 . . ? C47 C48A H48C 109.5 . . ? H48A C48A H48C 109.5 . . ? H48B C48A H48C 109.5 . . ? C47 C49A H49A 109.5 . . ? C47 C49A H49B 109.5 . . ? H49A C49A H49B 109.5 . . ? C47 C49A H49C 109.5 . . ? H49A C49A H49C 109.5 . . ? H49B C49A H49C 109.5 . . ? C47 C50A H50A 109.5 . . ? C47 C50A H50B 109.5 . . ? H50A C50A H50B 109.5 . . ? C47 C50A H50C 109.5 . . ? H50A C50A H50C 109.5 . . ? H50B C50A H50C 109.5 . . ? C47 C48B H48D 109.5 . . ? C47 C48B H48E 109.5 . . ? H48D C48B H48E 109.5 . . ? C47 C48B H48F 109.5 . . ? H48D C48B H48F 109.5 . . ? H48E C48B H48F 109.5 . . ? C47 C49B H49D 109.5 . . ? C47 C49B H49E 109.5 . . ? H49D C49B H49E 109.5 . . ? C47 C49B H49F 109.5 . . ? H49D C49B H49F 109.5 . . ? H49E C49B H49F 109.5 . . ? C47 C50B H50D 109.5 . . ? C47 C50B H50E 109.5 . . ? H50D C50B H50E 109.5 . . ? C47 C50B H50F 109.5 . . ? H50D C50B H50F 109.5 . . ? H50E C50B H50F 109.5 . . ? C51 O18 Fe6 130.4(2) . . ? C51 O19 Fe7 131.2(2) . . ? O18 C51 O19 125.1(3) . . ? O18 C51 C52 117.4(3) . . ? O19 C51 C52 117.4(3) . . ? C53A C52 C55A 111.7(5) . . ? C54B C52 C51 121.6(11) . . ? C53A C52 C51 112.1(4) . . ? C55A C52 C51 107.0(3) . . ? C54B C52 C53B 116.2(15) . . ? C51 C52 C53B 105.9(10) . . ? C53A C52 C54A 109.7(4) . . ? C55A C52 C54A 108.6(4) . . ? C51 C52 C54A 107.5(4) . . ? C54B C52 C55B 111.0(14) . . ? C51 C52 C55B 100.7(8) . . ? C53B C52 C55B 97.9(11) . . ? C52 C53A H53D 109.5 . . ? C52 C53A H53E 109.5 . . ? H53D C53A H53E 109.5 . . ? C52 C53A H53F 109.5 . . ? H53D C53A H53F 109.5 . . ? H53E C53A H53F 109.5 . . ? C52 C54A H54D 109.5 . . ? C52 C54A H54E 109.5 . . ? H54D C54A H54E 109.5 . . ? C52 C54A H54F 109.5 . . ? H54D C54A H54F 109.5 . . ? H54E C54A H54F 109.5 . . ? C52 C55A H55D 109.5 . . ? C52 C55A H55E 109.5 . . ? H55D C55A H55E 109.5 . . ? C52 C55A H55F 109.5 . . ? H55D C55A H55F 109.5 . . ? H55E C55A H55F 109.5 . . ? C52 C53B H53A 109.5 . . ? C52 C53B H53B 109.5 . . ? H53A C53B H53B 109.5 . . ? C52 C53B H53C 109.5 . . ? H53A C53B H53C 109.5 . . ? H53B C53B H53C 109.5 . . ? C52 C54B H54A 109.5 . . ? C52 C54B H54B 109.5 . . ? H54A C54B H54B 109.5 . . ? C52 C54B H54C 109.5 . . ? H54A C54B H54C 109.5 . . ? H54B C54B H54C 109.5 . . ? C52 C55B H55A 109.5 . . ? C52 C55B H55B 109.5 . . ? H55A C55B H55B 109.5 . . ? C52 C55B H55C 109.5 . . ? H55A C55B H55C 109.5 . . ? H55B C55B H55C 109.5 . . ? C56 O20 Fe6 127.9(2) . . ? C56 O21 Fe7 135.1(2) . . ? O21 C56 O20 125.1(3) . . ? O21 C56 C57 117.6(3) . . ? O20 C56 C57 117.3(3) . . ? C58 C57 C60 111.0(3) . . ? C58 C57 C56 110.9(3) . . ? C60 C57 C56 110.7(3) . . ? C58 C57 C59 108.4(3) . . ? C60 C57 C59 109.8(3) . . ? C56 C57 C59 105.9(3) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C61 O22 Fe3 134.6(2) . . ? O23 C61 O22 125.3(3) . . ? O23 C61 C62 120.1(3) . . ? O22 C61 C62 114.6(3) . . ? C63 C62 C65 110.6(4) . . ? C63 C62 C64 110.1(3) . . ? C65 C62 C64 110.6(4) . . ? C63 C62 C61 107.0(3) . . ? C65 C62 C61 110.4(3) . . ? C64 C62 C61 108.1(3) . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C62 C65 H65A 109.5 . . ? C62 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C62 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C66 O24 Fe5 135.4(2) . . ? O25 C66 O24 124.5(3) . . ? O25 C66 C67 120.2(3) . . ? O24 C66 C67 115.3(3) . . ? C68B C67 C66 116.5(7) . . ? C70A C67 C66 115.3(5) . . ? C70A C67 C69A 110.8(6) . . ? C66 C67 C69A 106.3(4) . . ? C68B C67 C69B 117.4(9) . . ? C66 C67 C69B 104.5(7) . . ? C70A C67 C68A 112.7(5) . . ? C66 C67 C68A 108.5(4) . . ? C69A C67 C68A 102.1(5) . . ? C68B C67 C70B 110.9(8) . . ? C66 C67 C70B 107.3(5) . . ? C69B C67 C70B 98.4(7) . . ? C67 C68A H68A 109.5 . . ? C67 C68A H68B 109.5 . . ? H68A C68A H68B 109.5 . . ? C67 C68A H68C 109.5 . . ? H68A C68A H68C 109.5 . . ? H68B C68A H68C 109.5 . . ? C67 C69A H69A 109.5 . . ? C67 C69A H69B 109.5 . . ? H69A C69A H69B 109.5 . . ? C67 C69A H69C 109.5 . . ? H69A C69A H69C 109.5 . . ? H69B C69A H69C 109.5 . . ? C67 C70A H70A 109.5 . . ? C67 C70A H70B 109.5 . . ? H70A C70A H70B 109.5 . . ? C67 C70A H70C 109.5 . . ? H70A C70A H70C 109.5 . . ? H70B C70A H70C 109.5 . . ? C67 C68B H68D 109.5 . . ? C67 C68B H68E 109.5 . . ? H68D C68B H68E 109.5 . . ? C67 C68B H68F 109.5 . . ? H68D C68B H68F 109.5 . . ? H68E C68B H68F 109.5 . . ? C67 C69B H69D 109.5 . . ? C67 C69B H69E 109.5 . . ? H69D C69B H69E 109.5 . . ? C67 C69B H69F 109.5 . . ? H69D C69B H69F 109.5 . . ? H69E C69B H69F 109.5 . . ? C67 C70B H70D 109.5 . . ? C67 C70B H70E 109.5 . . ? H70D C70B H70E 109.5 . . ? C67 C70B H70F 109.5 . . ? H70D C70B H70F 109.5 . . ? H70E C70B H70F 109.5 . . ? C71 O26 Fe7 135.7(2) . . ? O27 C71 O26 124.6(3) . . ? O27 C71 C72 120.4(3) . . ? O26 C71 C72 115.1(3) . . ? C75A C72 C74A 106.1(6) . . ? C75A C72 C71 108.5(5) . . ? C73B C72 C71 112.1(5) . . ? C74A C72 C71 111.1(4) . . ? C75A C72 C73A 113.2(6) . . ? C74A C72 C73A 107.3(5) . . ? C71 C72 C73A 110.6(4) . . ? C73B C72 C75B 106.6(8) . . ? C71 C72 C75B 105.7(7) . . ? C73B C72 C74B 114.2(6) . . ? C71 C72 C74B 106.7(4) . . ? C75B C72 C74B 111.3(8) . . ? C72 C73A H73A 109.5 . . ? C72 C73A H73B 109.5 . . ? H73A C73A H73B 109.5 . . ? C72 C73A H73C 109.5 . . ? H73A C73A H73C 109.5 . . ? H73B C73A H73C 109.5 . . ? C72 C74A H74A 109.5 . . ? C72 C74A H74B 109.5 . . ? H74A C74A H74B 109.5 . . ? C72 C74A H74C 109.5 . . ? H74A C74A H74C 109.5 . . ? H74B C74A H74C 109.5 . . ? C72 C75A H75A 109.5 . . ? C72 C75A H75B 109.5 . . ? H75A C75A H75B 109.5 . . ? C72 C75A H75C 109.5 . . ? H75A C75A H75C 109.5 . . ? H75B C75A H75C 109.5 . . ? C72 C73B H73D 109.5 . . ? C72 C73B H73E 109.5 . . ? H73D C73B H73E 109.5 . . ? C72 C73B H73F 109.5 . . ? H73D C73B H73F 109.5 . . ? H73E C73B H73F 109.5 . . ? C72 C74B H74D 109.5 . . ? C72 C74B H74E 109.5 . . ? H74D C74B H74E 109.5 . . ? C72 C74B H74F 109.5 . . ? H74D C74B H74F 109.5 . . ? H74E C74B H74F 109.5 . . ? C72 C75B H75D 109.5 . . ? C72 C75B H75E 109.5 . . ? H75D C75B H75E 109.5 . . ? C72 C75B H75F 109.5 . . ? H75D C75B H75F 109.5 . . ? H75E C75B H75F 109.5 . . ? Fe3 O28 H281 105(2) . . ? Fe3 O28 H282 96(2) . . ? H281 O28 H282 135(4) . . ? Fe5 O29 H291 107(2) . . ? Fe5 O29 H292 89(3) . . ? H291 O29 H292 145(4) . . ? Fe7 O30 H301 113(3) . . ? Fe7 O30 H302 104(3) . . ? H301 O30 H302 134(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O28 H281 O23 0.89(3) 1.70(3) 2.553(3) 161(4) . O28 H282 O30 0.72(2) 2.26(2) 2.975(3) 177(3) . O29 H291 O25 0.91(3) 1.69(3) 2.570(3) 160(4) . O29 H292 O28 0.79(3) 2.22(3) 2.991(3) 165(4) . O30 H301 O27 0.83(3) 1.81(3) 2.574(3) 152(4) . O30 H302 O29 0.70(2) 2.42(2) 3.103(3) 166(4) . _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.504 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.097 ########################################################################### data_274 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H107.5 Fe8 N13.5 O27.5' _chemical_formula_weight 1844.84 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 23.6121(8) _cell_length_b 15.0975(5) _cell_length_c 44.6731(14) _cell_angle_alpha 90.00 _cell_angle_beta 94.5230(10) _cell_angle_gamma 90.00 _cell_volume 15875.6(9) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20977 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.33 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7680 _exptl_absorpt_coefficient_mu 1.501 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.701 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 79377 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0830 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 57 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.01 _reflns_number_total 35692 _reflns_number_gt 20937 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_data_reduction 'SAINT+ 6.0 (Bruker AXS Inc., 2000)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _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. Block-matrix refinement, with one cluster in each block, together with all the solvent atoms and the Fe atoms of the other cluster. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type userblock _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0598P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 35692 _refine_ls_number_parameters 1851 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0956 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1276 _refine_ls_wR_factor_gt 0.1173 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.010 _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 Fe1 Fe 0.30440(2) 0.45683(4) 0.355665(12) 0.02372(13) Uani 1 1 d . . . Fe2 Fe 0.41563(2) 0.46664(4) 0.388624(12) 0.02311(13) Uani 1 1 d . . . Fe3 Fe 0.30123(3) 0.63844(4) 0.389719(13) 0.03420(16) Uani 1 1 d . . . Fe4 Fe 0.33878(3) 0.47902(4) 0.438758(12) 0.02295(13) Uani 1 1 d . . . Fe5 Fe 0.30887(2) 0.28465(3) 0.395340(12) 0.02141(13) Uani 1 1 d . . . Fe6 Fe 0.42664(3) 0.29089(4) 0.359582(13) 0.02550(13) Uani 1 1 d . . . Fe7 Fe 0.38770(3) 0.45786(4) 0.304867(12) 0.02415(13) Uani 1 1 d . . . Fe8 Fe 0.42483(3) 0.62657(4) 0.349081(13) 0.03015(15) Uani 1 1 d . . . O1 O 0.33686(12) 0.51886(16) 0.39732(5) 0.0240(6) Uani 1 1 d . . . O2 O 0.36600(11) 0.35834(16) 0.37559(5) 0.0215(6) Uani 1 1 d . . . O3 O 0.38917(11) 0.51059(16) 0.34544(5) 0.0234(6) Uani 1 1 d . . . N1 N 0.20545(15) 0.4450(2) 0.32638(8) 0.0356(9) Uani 1 1 d . . . C1 C 0.1831(2) 0.5351(3) 0.32812(10) 0.0422(12) Uani 1 1 d . . . H1A H 0.1633 0.5421 0.3467 0.051 Uiso 1 1 calc R . . H1B H 0.1555 0.5467 0.3107 0.051 Uiso 1 1 calc R . . C2 C 0.2321(2) 0.6001(3) 0.32816(10) 0.0425(12) Uani 1 1 d . . . H2A H 0.2497 0.5976 0.3088 0.051 Uiso 1 1 calc R . . H2B H 0.2184 0.6612 0.3311 0.051 Uiso 1 1 calc R . . O7 O 0.27258(13) 0.57550(18) 0.35228(6) 0.0328(7) Uani 1 1 d . . . C3 C 0.17511(19) 0.3785(3) 0.34297(10) 0.0391(11) Uani 1 1 d . . . H3A H 0.1818 0.3186 0.3350 0.047 Uiso 1 1 calc R . . H3B H 0.1338 0.3905 0.3409 0.047 Uiso 1 1 calc R . . C4 C 0.19740(17) 0.3841(3) 0.37550(9) 0.0341(10) Uani 1 1 d . . . H4A H 0.1867 0.4415 0.3842 0.041 Uiso 1 1 calc R . . H4B H 0.1811 0.3359 0.3871 0.041 Uiso 1 1 calc R . . O8 O 0.25743(11) 0.37590(17) 0.37676(6) 0.0259(6) Uani 1 1 d . . . C5 C 0.2178(2) 0.4171(3) 0.29608(9) 0.0395(11) Uani 1 1 d . . . H5A H 0.2234 0.4696 0.2834 0.047 Uiso 1 1 calc R . . H5B H 0.1858 0.3820 0.2867 0.047 Uiso 1 1 calc R . . C6 C 0.27135(18) 0.3616(3) 0.29902(9) 0.0321(10) Uani 1 1 d . . . H6A H 0.2643 0.3055 0.3096 0.039 Uiso 1 1 calc R . . H6B H 0.2835 0.3470 0.2789 0.039 Uiso 1 1 calc R . . O9 O 0.31412(11) 0.41169(17) 0.31556(6) 0.0262(6) Uani 1 1 d . . . N2 N 0.37083(14) 0.4205(2) 0.48404(7) 0.0262(8) Uani 1 1 d . . . C7 C 0.43287(18) 0.4384(3) 0.48552(9) 0.0332(10) Uani 1 1 d . . . H7A H 0.4525 0.4014 0.5014 0.040 Uiso 1 1 calc R . . H7B H 0.4400 0.5013 0.4907 0.040 Uiso 1 1 calc R . . C8 C 0.45639(18) 0.4178(3) 0.45545(9) 0.0335(10) Uani 1 1 d . . . H8A H 0.4954 0.4415 0.4551 0.040 Uiso 1 1 calc R . . H8B H 0.4577 0.3530 0.4523 0.040 Uiso 1 1 calc R . . O10 O 0.42009(11) 0.45798(17) 0.43237(6) 0.0267(6) Uani 1 1 d . . . C9 C 0.35811(18) 0.3248(3) 0.48221(9) 0.0290(9) Uani 1 1 d . . . H9A H 0.3517 0.3016 0.5024 0.035 Uiso 1 1 calc R . . H9B H 0.3906 0.2926 0.4747 0.035 Uiso 1 1 calc R . . C10 C 0.30569(18) 0.3110(3) 0.46127(8) 0.0273(9) Uani 1 1 d . . . H10A H 0.2990 0.2469 0.4579 0.033 Uiso 1 1 calc R . . H10B H 0.2721 0.3363 0.4701 0.033 Uiso 1 1 calc R . . O11 O 0.31407(11) 0.35387(16) 0.43347(5) 0.0244(6) Uani 1 1 d . . . C11 C 0.34140(19) 0.4623(3) 0.50893(9) 0.0339(10) Uani 1 1 d . B . H11A H 0.3017 0.4407 0.5076 0.041 Uiso 1 1 calc R . . H11B H 0.3401 0.5270 0.5055 0.041 Uiso 1 1 calc R . . C12 C 0.3673(2) 0.4460(3) 0.54078(9) 0.0401(12) Uani 1 1 d . . . H12C H 0.3370 0.4512 0.5548 0.048 Uiso 0.58 1 calc PR A 1 H12D H 0.3820 0.3846 0.5421 0.048 Uiso 0.58 1 calc PR A 1 H12E H 0.4076 0.4649 0.5417 0.048 Uiso 0.42 1 calc PR A 2 H12F H 0.3478 0.4854 0.5544 0.048 Uiso 0.42 1 calc PR A 2 O12A O 0.4093(2) 0.5013(3) 0.54964(11) 0.0412(13) Uiso 0.58 1 d P B 1 H12A H 0.3972 0.5536 0.5489 0.062 Uiso 0.58 1 calc PRD B 1 O12B O 0.3659(3) 0.3624(5) 0.55202(15) 0.0372(17) Uiso 0.42 1 d P B 2 H12B H 0.3319 0.3458 0.5522 0.056 Uiso 0.42 1 calc PRD B 2 N3 N 0.51446(16) 0.2516(2) 0.34671(8) 0.0360(9) Uani 1 1 d . . . C13 C 0.5536(2) 0.2922(3) 0.37026(11) 0.0426(12) Uani 1 1 d . . . H13A H 0.5924 0.2948 0.3633 0.051 Uiso 1 1 calc R . . H13B H 0.5549 0.2555 0.3887 0.051 Uiso 1 1 calc R . . C14 C 0.53382(19) 0.3850(3) 0.37727(11) 0.0419(12) Uani 1 1 d . . . H14A H 0.5551 0.4074 0.3957 0.050 Uiso 1 1 calc R . . H14B H 0.5407 0.4254 0.3605 0.050 Uiso 1 1 calc R . . O13 O 0.47491(11) 0.38146(18) 0.38145(6) 0.0286(6) Uani 1 1 d . . . C15 C 0.5206(2) 0.2925(3) 0.31663(10) 0.0413(12) Uani 1 1 d . . . H15A H 0.5451 0.2549 0.3049 0.050 Uiso 1 1 calc R . . H15B H 0.5384 0.3516 0.3192 0.050 Uiso 1 1 calc R . . C16 C 0.46299(19) 0.3011(3) 0.30026(9) 0.0353(11) Uani 1 1 d . . . H16A H 0.4657 0.3339 0.2812 0.042 Uiso 1 1 calc R . . H16B H 0.4469 0.2418 0.2955 0.042 Uiso 1 1 calc R . . O14 O 0.42734(12) 0.34835(17) 0.31937(6) 0.0288(7) Uani 1 1 d . . . C17 C 0.5195(2) 0.1537(3) 0.34510(11) 0.0462(13) Uani 1 1 d . . . H17A H 0.4926 0.1326 0.3285 0.055 Uiso 1 1 calc R . . H17B H 0.5068 0.1287 0.3639 0.055 Uiso 1 1 calc R . . C18 C 0.5776(3) 0.1148(3) 0.34047(13) 0.0641(18) Uani 1 1 d . . . H18A H 0.5918 0.1383 0.3218 0.077 Uiso 1 1 calc R . . H18B H 0.6050 0.1307 0.3575 0.077 Uiso 1 1 calc R . . O15 O 0.5713(2) 0.0198(3) 0.33849(8) 0.0789(14) Uani 1 1 d . . . H15 H 0.5793 0.0026 0.3215 0.118 Uiso 1 1 calc R . . N4 N 0.47996(19) 0.7411(2) 0.36968(9) 0.0460(11) Uani 1 1 d . . . C19 C 0.5234(2) 0.6958(3) 0.38942(12) 0.0553(15) Uani 1 1 d . . . H19A H 0.5422 0.7389 0.4036 0.066 Uiso 1 1 calc R . . H19B H 0.5526 0.6702 0.3773 0.066 Uiso 1 1 calc R . . C20 C 0.4962(2) 0.6221(3) 0.40689(11) 0.0479(13) Uani 1 1 d . . . H20A H 0.5258 0.5854 0.4178 0.057 Uiso 1 1 calc R . . H20B H 0.4716 0.6477 0.4217 0.057 Uiso 1 1 calc R . . O16 O 0.46353(12) 0.57042(18) 0.38551(6) 0.0309(7) Uani 1 1 d . . . C21 C 0.4403(3) 0.7949(3) 0.38646(11) 0.0526(15) Uani 1 1 d . . . H21A H 0.4436 0.7770 0.4078 0.063 Uiso 1 1 calc R . . H21B H 0.4509 0.8582 0.3854 0.063 Uiso 1 1 calc R . . C22 C 0.3809(2) 0.7832(3) 0.37391(11) 0.0479(14) Uani 1 1 d . . . H22A H 0.3547 0.8121 0.3871 0.057 Uiso 1 1 calc R . . H22B H 0.3757 0.8111 0.3538 0.057 Uiso 1 1 calc R . . O17 O 0.36849(14) 0.68940(18) 0.37158(7) 0.0398(8) Uani 1 1 d . . . C23 C 0.5130(3) 0.7963(3) 0.34924(13) 0.0669(18) Uani 1 1 d . . . H23A H 0.5380 0.8365 0.3618 0.080 Uiso 1 1 calc R . . H23B H 0.5379 0.7564 0.3385 0.080 Uiso 1 1 calc R . . C24 C 0.4804(3) 0.8486(4) 0.32733(14) 0.0727(18) Uani 1 1 d . . . H24A H 0.5038 0.8605 0.3103 0.087 Uiso 1 1 calc R . . H24B H 0.4469 0.8139 0.3195 0.087 Uiso 1 1 calc R . . O18 O 0.4612(2) 0.9313(3) 0.33849(10) 0.0889(15) Uani 1 1 d . . . H18 H 0.4849 0.9500 0.3520 0.133 Uiso 1 1 calc R . . O19 O 0.23106(15) 0.5980(2) 0.41222(7) 0.0509(9) Uani 1 1 d . . . O20 O 0.26142(13) 0.5108(2) 0.45025(6) 0.0376(7) Uani 1 1 d . . . C25 C 0.2245(2) 0.5586(3) 0.43635(9) 0.0332(10) Uani 1 1 d . C . C26 C 0.1680(2) 0.5693(3) 0.45066(10) 0.0386(11) Uani 1 1 d . . . C27A C 0.1431(3) 0.6642(4) 0.44362(16) 0.0392(17) Uiso 0.64 1 d P C 1 H27A H 0.1582 0.6870 0.4253 0.059 Uiso 0.64 1 calc PR C 1 H27B H 0.1540 0.7039 0.4604 0.059 Uiso 0.64 1 calc PR C 1 H27C H 0.1016 0.6608 0.4407 0.059 Uiso 0.64 1 calc PR C 1 C28A C 0.1244(4) 0.4985(6) 0.43534(19) 0.055(2) Uiso 0.64 1 d P C 1 H28A H 0.1129 0.5170 0.4147 0.082 Uiso 0.64 1 calc PR C 1 H28B H 0.0908 0.4949 0.4468 0.082 Uiso 0.64 1 calc PR C 1 H28C H 0.1428 0.4404 0.4351 0.082 Uiso 0.64 1 calc PR C 1 C29A C 0.1749(4) 0.5558(6) 0.48329(18) 0.057(2) Uiso 0.64 1 d P C 1 H29A H 0.1890 0.6104 0.4931 0.086 Uiso 0.64 1 calc PR C 1 H29B H 0.2021 0.5077 0.4880 0.086 Uiso 0.64 1 calc PR C 1 H29C H 0.1381 0.5402 0.4906 0.086 Uiso 0.64 1 calc PR C 1 C27B C 0.1722(8) 0.6560(11) 0.4681(4) 0.070(5) Uiso 0.36 1 d P C 2 H27D H 0.1762 0.7052 0.4541 0.106 Uiso 0.36 1 calc PR C 2 H27E H 0.2054 0.6542 0.4827 0.106 Uiso 0.36 1 calc PR C 2 H27F H 0.1378 0.6644 0.4786 0.106 Uiso 0.36 1 calc PR C 2 C28B C 0.1208(8) 0.5609(12) 0.4284(4) 0.073(5) Uiso 0.36 1 d P C 2 H28D H 0.1243 0.6053 0.4126 0.109 Uiso 0.36 1 calc PR C 2 H28E H 0.0852 0.5703 0.4378 0.109 Uiso 0.36 1 calc PR C 2 H28F H 0.1209 0.5015 0.4196 0.109 Uiso 0.36 1 calc PR C 2 C29B C 0.1615(6) 0.4940(9) 0.4755(3) 0.042(3) Uiso 0.36 1 d P C 2 H29D H 0.1848 0.5094 0.4939 0.063 Uiso 0.36 1 calc PR C 2 H29E H 0.1741 0.4370 0.4679 0.063 Uiso 0.36 1 calc PR C 2 H29F H 0.1216 0.4895 0.4799 0.063 Uiso 0.36 1 calc PR C 2 O21 O 0.33004(18) 0.6994(2) 0.42893(7) 0.0558(10) Uani 1 1 d . . . O22 O 0.36406(15) 0.59484(19) 0.45959(7) 0.0422(8) Uani 1 1 d . . . C30 C 0.3540(2) 0.6733(3) 0.45339(10) 0.0405(12) Uani 1 1 d . D . C31 C 0.3700(3) 0.7435(3) 0.47818(11) 0.0574(16) Uani 1 1 d . . . C32A C 0.4089(7) 0.7084(10) 0.5025(3) 0.073(4) Uiso 0.50 1 d P D 1 H32A H 0.3940 0.6523 0.5096 0.110 Uiso 0.50 1 calc PR D 1 H32B H 0.4124 0.7510 0.5191 0.110 Uiso 0.50 1 calc PR D 1 H32C H 0.4463 0.6983 0.4951 0.110 Uiso 0.50 1 calc PR D 1 C33A C 0.3065(5) 0.7504(8) 0.4929(3) 0.044(3) Uiso 0.50 1 d P D 1 H33A H 0.2780 0.7732 0.4776 0.066 Uiso 0.50 1 calc PR D 1 H33B H 0.3095 0.7905 0.5102 0.066 Uiso 0.50 1 calc PR D 1 H33C H 0.2950 0.6915 0.4993 0.066 Uiso 0.50 1 calc PR D 1 C34A C 0.3921(5) 0.8278(7) 0.4666(2) 0.043(3) Uiso 0.50 1 d P D 1 H34A H 0.3656 0.8503 0.4504 0.064 Uiso 0.50 1 calc PR D 1 H34B H 0.4292 0.8172 0.4589 0.064 Uiso 0.50 1 calc PR D 1 H34C H 0.3961 0.8714 0.4829 0.064 Uiso 0.50 1 calc PR D 1 C32B C 0.4274(7) 0.7158(10) 0.4944(3) 0.074(4) Uiso 0.50 1 d P D 2 H32D H 0.4569 0.7170 0.4802 0.112 Uiso 0.50 1 calc PR D 2 H32E H 0.4242 0.6558 0.5024 0.112 Uiso 0.50 1 calc PR D 2 H32F H 0.4375 0.7570 0.5109 0.112 Uiso 0.50 1 calc PR D 2 C33B C 0.3281(7) 0.7423(11) 0.4991(4) 0.083(5) Uiso 0.50 1 d P D 2 H33D H 0.3377 0.7860 0.5149 0.124 Uiso 0.50 1 calc PR D 2 H33E H 0.3265 0.6832 0.5080 0.124 Uiso 0.50 1 calc PR D 2 H33F H 0.2910 0.7568 0.4888 0.124 Uiso 0.50 1 calc PR D 2 C34B C 0.3665(6) 0.8376(9) 0.4630(3) 0.070(4) Uiso 0.50 1 d P D 2 H34D H 0.3962 0.8430 0.4490 0.105 Uiso 0.50 1 calc PR D 2 H34E H 0.3720 0.8834 0.4786 0.105 Uiso 0.50 1 calc PR D 2 H34F H 0.3292 0.8452 0.4521 0.105 Uiso 0.50 1 calc PR D 2 O23 O 0.30036(13) 0.20219(18) 0.35816(6) 0.0362(7) Uani 1 1 d . . . O24 O 0.38473(14) 0.18829(19) 0.33993(7) 0.0411(8) Uani 1 1 d . . . C35 C 0.3334(2) 0.1664(3) 0.34121(9) 0.0332(10) Uani 1 1 d . . . C36 C 0.3111(2) 0.0888(3) 0.32146(11) 0.0459(13) Uani 1 1 d . . . C37 C 0.2488(2) 0.1066(3) 0.30956(11) 0.0563(15) Uani 1 1 d . . . H37A H 0.2474 0.1583 0.2962 0.085 Uiso 1 1 calc R . . H37B H 0.2259 0.1181 0.3265 0.085 Uiso 1 1 calc R . . H37C H 0.2337 0.0547 0.2984 0.085 Uiso 1 1 calc R . . C38 C 0.3112(2) 0.0081(3) 0.34160(12) 0.0552(15) Uani 1 1 d . . . H38A H 0.3503 -0.0048 0.3495 0.083 Uiso 1 1 calc R . . H38B H 0.2958 -0.0428 0.3300 0.083 Uiso 1 1 calc R . . H38C H 0.2877 0.0197 0.3583 0.083 Uiso 1 1 calc R . . C39 C 0.3464(3) 0.0762(4) 0.29512(12) 0.074(2) Uani 1 1 d . . . H39A H 0.3440 0.1295 0.2826 0.112 Uiso 1 1 calc R . . H39B H 0.3320 0.0252 0.2832 0.112 Uiso 1 1 calc R . . H39C H 0.3860 0.0656 0.3024 0.112 Uiso 1 1 calc R . . O25 O 0.36370(13) 0.19650(19) 0.41620(6) 0.0367(7) Uani 1 1 d . . . O26 O 0.44558(13) 0.20731(19) 0.39503(7) 0.0387(8) Uani 1 1 d . . . C40 C 0.41446(18) 0.1756(3) 0.41413(9) 0.0271(9) Uani 1 1 d . . . C41 C 0.4405(2) 0.1032(3) 0.43499(9) 0.0340(10) Uani 1 1 d . . . C42 C 0.5024(3) 0.1246(4) 0.44393(17) 0.098(3) Uani 1 1 d . . . H42A H 0.5188 0.0782 0.4573 0.147 Uiso 1 1 calc R . . H42B H 0.5049 0.1817 0.4544 0.147 Uiso 1 1 calc R . . H42C H 0.5234 0.1277 0.4259 0.147 Uiso 1 1 calc R . . C43 C 0.4088(3) 0.0939(4) 0.46300(11) 0.072(2) Uani 1 1 d . . . H43A H 0.3690 0.0787 0.4573 0.108 Uiso 1 1 calc R . . H43B H 0.4105 0.1499 0.4741 0.108 Uiso 1 1 calc R . . H43C H 0.4262 0.0469 0.4757 0.108 Uiso 1 1 calc R . . C44 C 0.4357(3) 0.0182(3) 0.41781(12) 0.084(2) Uani 1 1 d . . . H44A H 0.3955 0.0046 0.4126 0.125 Uiso 1 1 calc R . . H44B H 0.4531 -0.0298 0.4302 0.125 Uiso 1 1 calc R . . H44C H 0.4553 0.0239 0.3994 0.125 Uiso 1 1 calc R . . O27 O 0.34944(13) 0.57155(18) 0.28534(6) 0.0336(7) Uani 1 1 d . . . O28 O 0.39073(14) 0.68404(18) 0.31134(6) 0.0395(8) Uani 1 1 d . . . C45 C 0.35913(18) 0.6526(3) 0.28950(9) 0.0303(10) Uani 1 1 d . E . C46 C 0.3336(2) 0.7190(3) 0.26601(10) 0.0352(11) Uani 1 1 d . . . C47A C 0.3128(4) 0.8005(5) 0.28398(17) 0.0422(19) Uiso 0.62 1 d P E 1 H47A H 0.3452 0.8269 0.2959 0.063 Uiso 0.62 1 calc PR E 1 H47B H 0.2844 0.7810 0.2974 0.063 Uiso 0.62 1 calc PR E 1 H47C H 0.2959 0.8447 0.2699 0.063 Uiso 0.62 1 calc PR E 1 C48A C 0.2851(4) 0.6803(5) 0.24759(18) 0.046(2) Uiso 0.62 1 d P E 1 H48A H 0.2699 0.7241 0.2329 0.069 Uiso 0.62 1 calc PR E 1 H48B H 0.2554 0.6633 0.2606 0.069 Uiso 0.62 1 calc PR E 1 H48C H 0.2978 0.6278 0.2371 0.069 Uiso 0.62 1 calc PR E 1 C49A C 0.3822(3) 0.7472(6) 0.24766(18) 0.041(2) Uiso 0.62 1 d P E 1 H49A H 0.4130 0.7722 0.2610 0.062 Uiso 0.62 1 calc PR E 1 H49B H 0.3685 0.7918 0.2329 0.062 Uiso 0.62 1 calc PR E 1 H49C H 0.3963 0.6955 0.2372 0.062 Uiso 0.62 1 calc PR E 1 C47B C 0.2820(7) 0.7691(10) 0.2753(3) 0.062(4) Uiso 0.38 1 d P E 2 H47D H 0.2682 0.8093 0.2591 0.092 Uiso 0.38 1 calc PR E 2 H47E H 0.2925 0.8035 0.2935 0.092 Uiso 0.38 1 calc PR E 2 H47F H 0.2519 0.7269 0.2793 0.092 Uiso 0.38 1 calc PR E 2 C48B C 0.3091(6) 0.6665(9) 0.2357(3) 0.047(3) Uiso 0.38 1 d P E 2 H48D H 0.3394 0.6301 0.2283 0.071 Uiso 0.38 1 calc PR E 2 H48E H 0.2958 0.7094 0.2203 0.071 Uiso 0.38 1 calc PR E 2 H48F H 0.2775 0.6283 0.2405 0.071 Uiso 0.38 1 calc PR E 2 C49B C 0.3789(6) 0.7827(9) 0.2560(3) 0.042(3) Uiso 0.38 1 d P E 2 H49D H 0.4095 0.7488 0.2479 0.063 Uiso 0.38 1 calc PR E 2 H49E H 0.3944 0.8175 0.2733 0.063 Uiso 0.38 1 calc PR E 2 H49F H 0.3618 0.8226 0.2406 0.063 Uiso 0.38 1 calc PR E 2 O29 O 0.46249(13) 0.50543(18) 0.29263(6) 0.0339(7) Uani 1 1 d . . . O30 O 0.49468(13) 0.60730(19) 0.32560(7) 0.0384(8) Uani 1 1 d . . . C50 C 0.49822(19) 0.5624(3) 0.30206(9) 0.0308(10) Uani 1 1 d . F . C51 C 0.5481(2) 0.5779(3) 0.28288(11) 0.0411(12) Uani 1 1 d . . . C52A C 0.5974(6) 0.6240(9) 0.3069(3) 0.072(4) Uiso 0.50 1 d P F 1 H52A H 0.5828 0.6796 0.3145 0.108 Uiso 0.50 1 calc PR F 1 H52B H 0.6317 0.6359 0.2965 0.108 Uiso 0.50 1 calc PR F 1 H52C H 0.6067 0.5834 0.3236 0.108 Uiso 0.50 1 calc PR F 1 C53A C 0.5705(6) 0.4949(9) 0.2723(3) 0.034(4) Uiso 0.50 1 d P F 1 H53A H 0.5824 0.4574 0.2896 0.050 Uiso 0.50 1 calc PR F 1 H53B H 0.6031 0.5069 0.2607 0.050 Uiso 0.50 1 calc PR F 1 H53C H 0.5409 0.4644 0.2596 0.050 Uiso 0.50 1 calc PR F 1 C54A C 0.5306(6) 0.6473(9) 0.2617(3) 0.085(4) Uiso 0.50 1 d P F 1 H54A H 0.5173 0.6987 0.2725 0.128 Uiso 0.50 1 calc PR F 1 H54B H 0.4998 0.6254 0.2476 0.128 Uiso 0.50 1 calc PR F 1 H54C H 0.5630 0.6648 0.2505 0.128 Uiso 0.50 1 calc PR F 1 C52B C 0.5888(4) 0.6420(6) 0.2934(2) 0.029(2) Uiso 0.50 1 d P F 2 H52D H 0.6184 0.6467 0.2793 0.043 Uiso 0.50 1 calc PR F 2 H52E H 0.6060 0.6242 0.3132 0.043 Uiso 0.50 1 calc PR F 2 H52F H 0.5701 0.6996 0.2951 0.043 Uiso 0.50 1 calc PR F 2 C53B C 0.5777(7) 0.4854(10) 0.2773(3) 0.042(4) Uiso 0.50 1 d P F 2 H53D H 0.5489 0.4423 0.2699 0.064 Uiso 0.50 1 calc PR F 2 H53E H 0.5968 0.4640 0.2962 0.064 Uiso 0.50 1 calc PR F 2 H53F H 0.6057 0.4928 0.2624 0.064 Uiso 0.50 1 calc PR F 2 C54B C 0.5187(4) 0.6113(6) 0.25056(18) 0.0270(19) Uiso 0.50 1 d P F 2 H54D H 0.4902 0.5679 0.2429 0.040 Uiso 0.50 1 calc PR F 2 H54E H 0.5479 0.6173 0.2363 0.040 Uiso 0.50 1 calc PR F 2 H54F H 0.5003 0.6687 0.2531 0.040 Uiso 0.50 1 calc PR F 2 N11 N 0.2549(2) 0.7472(3) 0.37775(9) 0.0494(11) Uani 1 1 d . G . N12 N 0.2062(2) 0.7525(3) 0.37825(13) 0.0700(16) Uani 1 1 d . . . N13A N 0.1570(4) 0.7551(5) 0.37296(18) 0.058(2) Uiso 0.62 1 d P G 1 N13B N 0.1642(8) 0.7769(11) 0.3908(4) 0.092(5) Uiso 0.38 1 d P G 2 N21 N 0.24155(15) 0.2152(2) 0.40961(7) 0.0305(8) Uani 1 1 d . . . N22 N 0.21955(17) 0.1515(3) 0.39766(8) 0.0405(10) Uani 1 1 d . . . N23 N 0.1966(2) 0.0904(3) 0.38661(10) 0.0616(14) Uani 1 1 d . . . N31 N 0.37439(17) 0.4065(2) 0.26163(8) 0.0361(9) Uani 1 1 d . H . N32 N 0.39679(17) 0.4346(3) 0.24127(8) 0.0469(11) Uani 1 1 d . . . N33A N 0.4161(4) 0.4853(6) 0.2209(2) 0.038(2) Uiso 0.45 1 d P H 1 N33B N 0.4196(3) 0.4424(6) 0.21993(17) 0.044(2) Uiso 0.55 1 d P H 2 Fe9 Fe 0.18697(2) 0.14648(4) 0.649301(12) 0.02492(13) Uani 1 1 d . I . Fe10 Fe 0.08273(2) 0.17074(3) 0.610358(11) 0.02044(12) Uani 1 1 d . . . Fe11 Fe 0.08801(2) 0.15409(4) 0.693272(12) 0.02186(13) Uani 1 1 d . . . Fe12 Fe 0.04809(3) 0.00755(4) 0.641029(12) 0.02357(13) Uani 1 1 d . . . Fe13 Fe 0.18088(3) -0.02435(4) 0.608725(13) 0.02958(14) Uani 1 1 d . I . Fe14 Fe 0.16294(3) 0.14656(4) 0.562833(12) 0.02643(14) Uani 1 1 d . . . Fe15 Fe 0.20906(3) 0.32084(4) 0.613498(14) 0.03345(16) Uani 1 1 d . . . Fe16 Fe 0.08564(3) 0.34194(4) 0.644316(13) 0.02582(13) Uani 1 1 d . . . O4 O 0.09300(11) 0.11263(15) 0.65172(5) 0.0200(6) Uani 1 1 d . . . O5 O 0.15592(11) 0.10202(16) 0.60307(6) 0.0250(6) Uani 1 1 d . . . O6 O 0.14152(11) 0.26195(16) 0.62922(5) 0.0235(6) Uani 1 1 d . I . N5 N 0.27364(16) 0.1254(3) 0.68312(8) 0.0397(9) Uani 1 1 d . . . C55A C 0.2583(3) 0.1479(5) 0.71413(14) 0.0388(16) Uiso 0.68 1 d P I 3 H55A H 0.2466 0.0938 0.7245 0.047 Uiso 0.68 1 calc PR I 3 H55B H 0.2915 0.1739 0.7259 0.047 Uiso 0.68 1 calc PR I 3 C55B C 0.2680(6) 0.2071(9) 0.7032(3) 0.035(3) Uiso 0.32 1 d P I 4 H55C H 0.2946 0.2022 0.7214 0.042 Uiso 0.32 1 calc PR I 4 H55D H 0.2776 0.2614 0.6922 0.042 Uiso 0.32 1 calc PR I 4 C56 C 0.21092(18) 0.2124(3) 0.71157(10) 0.0382(11) Uani 1 1 d . . . H56A H 0.1944 0.2187 0.7312 0.046 Uiso 0.68 1 calc PR I 3 H56B H 0.2250 0.2712 0.7057 0.046 Uiso 0.68 1 calc PR I 3 H56C H 0.2081 0.1777 0.7302 0.046 Uiso 0.32 1 calc PR I 4 H56D H 0.2025 0.2750 0.7162 0.046 Uiso 0.32 1 calc PR I 4 O31 O 0.16889(11) 0.18160(18) 0.68958(6) 0.0278(6) Uani 1 1 d . I . C57A C 0.2878(3) 0.0265(4) 0.68082(16) 0.0385(16) Uiso 0.68 1 d P I 3 H57A H 0.3145 0.0172 0.6651 0.046 Uiso 0.68 1 calc PR I 3 H57B H 0.3061 0.0053 0.7002 0.046 Uiso 0.68 1 calc PR I 3 C57B C 0.2683(7) 0.0443(10) 0.6927(3) 0.044(4) Uiso 0.32 1 d P I 4 H57C H 0.2496 0.0474 0.7117 0.053 Uiso 0.32 1 calc PR I 4 H57D H 0.3070 0.0208 0.6976 0.053 Uiso 0.32 1 calc PR I 4 C58 C 0.2373(2) -0.0214(3) 0.67354(12) 0.0566(15) Uani 1 1 d . . . H58A H 0.2152 -0.0252 0.6914 0.068 Uiso 0.68 1 calc PR I 3 H58B H 0.2468 -0.0825 0.6676 0.068 Uiso 0.68 1 calc PR I 3 H58C H 0.2647 -0.0624 0.6651 0.068 Uiso 0.32 1 calc PR I 4 H58D H 0.2124 -0.0567 0.6858 0.068 Uiso 0.32 1 calc PR I 4 O32 O 0.20349(12) 0.02042(18) 0.64946(6) 0.0317(7) Uani 1 1 d . I . C59A C 0.3171(3) 0.1816(5) 0.67285(15) 0.0394(17) Uiso 0.68 1 d P I 3 H59A H 0.3547 0.1528 0.6767 0.047 Uiso 0.68 1 calc PR I 3 H59B H 0.3179 0.2385 0.6839 0.047 Uiso 0.68 1 calc PR I 3 C59B C 0.3180(6) 0.1421(10) 0.6624(3) 0.037(3) Uiso 0.32 1 d P I 4 H59C H 0.3520 0.1648 0.6743 0.045 Uiso 0.32 1 calc PR I 4 H59D H 0.3285 0.0846 0.6537 0.045 Uiso 0.32 1 calc PR I 4 C60 C 0.3053(2) 0.1983(4) 0.63976(11) 0.0598(16) Uani 1 1 d . . . H60A H 0.3282 0.2493 0.6338 0.072 Uiso 0.68 1 calc PR I 3 H60B H 0.3166 0.1457 0.6284 0.072 Uiso 0.68 1 calc PR I 3 H60C H 0.3213 0.1744 0.6216 0.072 Uiso 0.32 1 calc PR I 4 H60D H 0.3247 0.2551 0.6447 0.072 Uiso 0.32 1 calc PR I 4 O33 O 0.24706(12) 0.21599(19) 0.63262(6) 0.0329(7) Uani 1 1 d . I . N6 N -0.00928(15) -0.0880(2) 0.61443(7) 0.0294(8) Uani 1 1 d . . . C61 C -0.04796(18) -0.0302(3) 0.59532(9) 0.0314(10) Uani 1 1 d . . . H61A H -0.0778 -0.0060 0.6074 0.038 Uiso 1 1 calc R . . H61B H -0.0667 -0.0654 0.5787 0.038 Uiso 1 1 calc R . . C62 C -0.01445(18) 0.0457(3) 0.58258(9) 0.0310(10) Uani 1 1 d . . . H62A H 0.0080 0.0237 0.5663 0.037 Uiso 1 1 calc R . . H62B H -0.0408 0.0921 0.5742 0.037 Uiso 1 1 calc R . . O34 O 0.02217(11) 0.08134(17) 0.60619(5) 0.0230(6) Uani 1 1 d . . . C63 C 0.02833(19) -0.1410(3) 0.59631(9) 0.0333(10) Uani 1 1 d . . . H63A H 0.0325 -0.1113 0.5769 0.040 Uiso 1 1 calc R . . H63B H 0.0115 -0.2003 0.5922 0.040 Uiso 1 1 calc R . . C64 C 0.0853(2) -0.1502(3) 0.61341(10) 0.0372(11) Uani 1 1 d . . . H64A H 0.0819 -0.1848 0.6320 0.045 Uiso 1 1 calc R . . H64B H 0.1122 -0.1811 0.6010 0.045 Uiso 1 1 calc R . . O35 O 0.10526(12) -0.06213(17) 0.62061(6) 0.0302(7) Uani 1 1 d . . . C65 C -0.0408(2) -0.1446(3) 0.63544(9) 0.0379(11) Uani 1 1 d . K . H65A H -0.0641 -0.1050 0.6472 0.045 Uiso 1 1 calc R . . H65B H -0.0124 -0.1732 0.6498 0.045 Uiso 1 1 calc R . . C66 C -0.0795(2) -0.2168(3) 0.62138(11) 0.0519(14) Uani 1 1 d . . . H66A H -0.1102 -0.2291 0.6347 0.062 Uiso 0.82 1 calc PR J 1 H66B H -0.0974 -0.1955 0.6019 0.062 Uiso 0.82 1 calc PR J 1 H66C H -0.0833 -0.2615 0.6373 0.062 Uiso 0.18 1 calc PR J 2 H66D H -0.1174 -0.1892 0.6175 0.062 Uiso 0.18 1 calc PR J 2 O36A O -0.0491(3) -0.2959(3) 0.61676(11) 0.0709(16) Uani 0.82 1 d PU K 1 H36A H -0.0309 -0.3109 0.6329 0.106 Uiso 0.82 1 calc PRD K 1 O36B O -0.0695(10) -0.2651(15) 0.5949(5) 0.067(6) Uiso 0.18 1 d PU K 2 N7 N 0.14425(18) 0.2214(2) 0.51915(8) 0.0402(10) Uani 1 1 d . . . C67 C 0.0818(2) 0.2261(3) 0.51542(9) 0.0445(13) Uani 1 1 d . . . H67A H 0.0662 0.1687 0.5079 0.053 Uiso 1 1 calc R . . H67B H 0.0700 0.2723 0.5005 0.053 Uiso 1 1 calc R . . C68 C 0.0583(2) 0.2481(3) 0.54561(9) 0.0383(11) Uani 1 1 d . . . H68A H 0.0668 0.3105 0.5511 0.046 Uiso 1 1 calc R . . H68B H 0.0166 0.2398 0.5443 0.046 Uiso 1 1 calc R . . O37 O 0.08468(12) 0.19031(17) 0.56742(5) 0.0259(6) Uani 1 1 d . . . C69 C 0.1706(2) 0.3104(3) 0.52404(10) 0.0444(13) Uani 1 1 d . S . H69A H 0.1420 0.3525 0.5307 0.053 Uiso 1 1 calc R . . H69B H 0.1840 0.3325 0.5050 0.053 Uiso 1 1 calc R . . C70 C 0.2194(2) 0.3045(3) 0.54730(10) 0.0420(12) Uani 1 1 d . . . H70A H 0.2507 0.2701 0.5394 0.050 Uiso 1 1 calc R S . H70B H 0.2337 0.3647 0.5525 0.050 Uiso 1 1 calc R . . O38 O 0.20070(12) 0.26197(17) 0.57359(6) 0.0314(7) Uani 1 1 d . S . C71 C 0.1689(3) 0.1725(4) 0.49385(10) 0.0591(17) Uani 1 1 d . M . H71A H 0.2104 0.1825 0.4957 0.071 Uiso 1 1 calc R . . H71B H 0.1627 0.1085 0.4970 0.071 Uiso 1 1 calc R . . C72 C 0.1481(3) 0.1932(5) 0.46247(12) 0.082(2) Uani 1 1 d . . . H72A H 0.1635 0.1484 0.4491 0.098 Uiso 0.82 1 calc PR L 1 H72B H 0.1062 0.1876 0.4606 0.098 Uiso 0.82 1 calc PR L 1 H72C H 0.1489 0.1366 0.4513 0.098 Uiso 0.18 1 calc PR L 2 H72D H 0.1775 0.2313 0.4545 0.098 Uiso 0.18 1 calc PR L 2 O39A O 0.16148(19) 0.2713(3) 0.45308(9) 0.0467(10) Uani 0.82 1 d P M 1 H39D H 0.1771 0.2665 0.4369 0.070 Uiso 0.82 1 calc PR M 1 O39B O 0.0862(6) 0.2401(8) 0.4518(3) 0.014(3) Uiso 0.18 1 d P M 2 N8 N -0.00179(16) 0.4037(2) 0.65379(8) 0.0355(9) Uani 1 1 d . S . C73 C -0.04069(19) 0.3664(3) 0.62903(10) 0.0376(11) Uani 1 1 d . . . H73A H -0.0377 0.4018 0.6106 0.045 Uiso 1 1 calc R S . H73B H -0.0804 0.3701 0.6346 0.045 Uiso 1 1 calc R . . C74 C -0.02613(18) 0.2708(3) 0.62293(10) 0.0332(10) Uani 1 1 d . S . H74A H -0.0332 0.2332 0.6404 0.040 Uiso 1 1 calc R . . H74B H -0.0494 0.2484 0.6051 0.040 Uiso 1 1 calc R . . O40 O 0.03280(11) 0.26970(16) 0.61765(6) 0.0252(6) Uani 1 1 d . S . C75 C -0.0159(2) 0.3668(3) 0.68322(10) 0.0381(11) Uani 1 1 d . . . H75A H -0.0433 0.3175 0.6799 0.046 Uiso 1 1 calc R S . H75B H -0.0338 0.4132 0.6949 0.046 Uiso 1 1 calc R . . C76 C 0.0380(2) 0.3333(3) 0.70080(9) 0.0360(11) Uani 1 1 d . S . H76A H 0.0622 0.3838 0.7079 0.043 Uiso 1 1 calc R . . H76B H 0.0281 0.2988 0.7185 0.043 Uiso 1 1 calc R . . O41 O 0.06767(12) 0.27867(17) 0.68122(6) 0.0290(7) Uani 1 1 d . S . C77 C -0.0110(2) 0.5016(3) 0.65282(12) 0.0487(13) Uani 1 1 d . . . H77A H -0.0078 0.5225 0.6320 0.058 Uiso 1 1 calc R S . H77B H -0.0502 0.5142 0.6580 0.058 Uiso 1 1 calc R . . C78 C 0.0292(2) 0.5528(3) 0.67333(13) 0.0533(14) Uani 1 1 d . S . H78A H 0.0299 0.5288 0.6940 0.064 Uiso 1 1 calc R . . H78B H 0.0681 0.5493 0.6666 0.064 Uiso 1 1 calc R . . O42 O 0.00936(19) 0.6445(2) 0.67265(9) 0.0698(12) Uani 1 1 d . . . H42 H -0.0148 0.6512 0.6853 0.105 Uiso 1 1 calc RD S . O43 O 0.10502(14) 0.02521(18) 0.70930(6) 0.0348(7) Uani 1 1 d . . . O44 O 0.06338(14) -0.06896(19) 0.67644(6) 0.0402(8) Uani 1 1 d . . . C79 C 0.08918(19) -0.0513(3) 0.70137(9) 0.0298(10) Uani 1 1 d . . . C80 C 0.0991(2) -0.1284(3) 0.72331(9) 0.0319(10) Uani 1 1 d . . . C81 C 0.0397(2) -0.1607(3) 0.73049(11) 0.0518(14) Uani 1 1 d . . . H81A H 0.0199 -0.1128 0.7402 0.078 Uiso 1 1 calc R . . H81B H 0.0437 -0.2117 0.7440 0.078 Uiso 1 1 calc R . . H81C H 0.0179 -0.1780 0.7118 0.078 Uiso 1 1 calc R . . C82 C 0.1291(2) -0.2033(3) 0.70793(10) 0.0444(12) Uani 1 1 d . . . H82A H 0.1668 -0.1833 0.7031 0.067 Uiso 1 1 calc R . . H82B H 0.1067 -0.2203 0.6894 0.067 Uiso 1 1 calc R . . H82C H 0.1332 -0.2545 0.7214 0.067 Uiso 1 1 calc R . . C83 C 0.1326(2) -0.0996(3) 0.75167(10) 0.0460(13) Uani 1 1 d . . . H83A H 0.1701 -0.0789 0.7469 0.069 Uiso 1 1 calc R . . H83B H 0.1369 -0.1498 0.7656 0.069 Uiso 1 1 calc R . . H83C H 0.1125 -0.0515 0.7610 0.069 Uiso 1 1 calc R . . O45 O 0.00431(12) 0.1298(2) 0.69766(6) 0.0364(7) Uani 1 1 d . . . O46 O -0.02532(13) 0.04113(19) 0.66004(6) 0.0352(7) Uani 1 1 d . . . C84 C -0.03332(18) 0.0842(3) 0.68328(9) 0.0276(9) Uani 1 1 d . . . C85 C -0.0918(2) 0.0782(3) 0.69551(10) 0.0387(11) Uani 1 1 d . . . C86 C -0.1377(2) 0.0612(4) 0.67025(12) 0.0679(18) Uani 1 1 d . . . H86A H -0.1401 0.1120 0.6566 0.102 Uiso 1 1 calc R . . H86B H -0.1743 0.0528 0.6787 0.102 Uiso 1 1 calc R . . H86C H -0.1281 0.0079 0.6592 0.102 Uiso 1 1 calc R . . C87 C -0.0893(3) -0.0028(4) 0.71655(14) 0.085(2) Uani 1 1 d . . . H87A H -0.0602 0.0069 0.7331 0.127 Uiso 1 1 calc R . . H87B H -0.0798 -0.0557 0.7053 0.127 Uiso 1 1 calc R . . H87C H -0.1263 -0.0109 0.7247 0.127 Uiso 1 1 calc R . . C88 C -0.1045(3) 0.1590(4) 0.71322(18) 0.117(3) Uani 1 1 d . . . H88A H -0.1060 0.2109 0.7000 0.175 Uiso 1 1 calc R . . H88B H -0.0747 0.1672 0.7295 0.175 Uiso 1 1 calc R . . H88C H -0.1412 0.1517 0.7217 0.175 Uiso 1 1 calc R . . O47 O 0.25940(13) 0.0113(2) 0.59361(7) 0.0383(8) Uani 1 1 d . . . O48 O 0.23721(13) 0.0962(2) 0.55358(7) 0.0370(7) Uani 1 1 d . . . C89 C 0.2722(2) 0.0507(3) 0.57056(11) 0.0407(12) Uani 1 1 d . N . C90 C 0.3337(2) 0.0438(4) 0.56132(12) 0.0545(15) Uani 1 1 d . . . C91A C 0.3446(6) 0.1359(8) 0.5404(3) 0.062(3) Uiso 0.50 1 d P N 1 H91A H 0.3160 0.1382 0.5233 0.093 Uiso 0.50 1 calc PR N 1 H91B H 0.3826 0.1334 0.5331 0.093 Uiso 0.50 1 calc PR N 1 H91C H 0.3414 0.1888 0.5528 0.093 Uiso 0.50 1 calc PR N 1 C92A C 0.3329(5) -0.0375(7) 0.5403(2) 0.041(3) Uiso 0.50 1 d P N 1 H92A H 0.3027 -0.0303 0.5241 0.061 Uiso 0.50 1 calc PR N 1 H92B H 0.3258 -0.0912 0.5517 0.061 Uiso 0.50 1 calc PR N 1 H92C H 0.3696 -0.0426 0.5316 0.061 Uiso 0.50 1 calc PR N 1 C93A C 0.3756(4) 0.0434(7) 0.5858(2) 0.038(2) Uiso 0.50 1 d P N 1 H93A H 0.4133 0.0389 0.5782 0.057 Uiso 0.50 1 calc PR N 1 H93B H 0.3694 -0.0074 0.5988 0.057 Uiso 0.50 1 calc PR N 1 H93C H 0.3731 0.0983 0.5972 0.057 Uiso 0.50 1 calc PR N 1 C91B C 0.3564(6) 0.1311(8) 0.5548(3) 0.066(4) Uiso 0.50 1 d P N 2 H91D H 0.3578 0.1677 0.5730 0.099 Uiso 0.50 1 calc PR N 2 H91E H 0.3319 0.1595 0.5389 0.099 Uiso 0.50 1 calc PR N 2 H91F H 0.3948 0.1246 0.5482 0.099 Uiso 0.50 1 calc PR N 2 C92B C 0.3326(5) -0.0083(8) 0.5332(3) 0.051(3) Uiso 0.50 1 d P N 2 H92D H 0.3182 -0.0679 0.5367 0.077 Uiso 0.50 1 calc PR N 2 H92E H 0.3712 -0.0124 0.5266 0.077 Uiso 0.50 1 calc PR N 2 H92F H 0.3078 0.0210 0.5176 0.077 Uiso 0.50 1 calc PR N 2 C93B C 0.3733(5) 0.0001(8) 0.5882(2) 0.054(3) Uiso 0.50 1 d P N 2 H93D H 0.3584 -0.0583 0.5929 0.082 Uiso 0.50 1 calc PR N 2 H93E H 0.3738 0.0381 0.6060 0.082 Uiso 0.50 1 calc PR N 2 H93F H 0.4121 -0.0062 0.5820 0.082 Uiso 0.50 1 calc PR N 2 O49 O 0.15904(13) -0.07065(19) 0.56652(7) 0.0369(7) Uani 1 1 d . . . O50 O 0.12556(13) 0.04281(19) 0.53820(6) 0.0341(7) Uani 1 1 d . . . C94 C 0.13565(18) -0.0390(3) 0.54290(10) 0.0301(10) Uani 1 1 d . O . C95 C 0.1201(2) -0.1037(3) 0.51681(10) 0.0422(12) Uani 1 1 d . . . C96A C 0.1151(5) -0.1954(7) 0.5270(2) 0.056(3) Uiso 0.58 1 d P O 3 H96A H 0.1049 -0.2337 0.5097 0.084 Uiso 0.58 1 calc PR O 3 H96B H 0.0856 -0.1991 0.5412 0.084 Uiso 0.58 1 calc PR O 3 H96C H 0.1515 -0.2148 0.5369 0.084 Uiso 0.58 1 calc PR O 3 C97A C 0.0589(4) -0.0706(6) 0.5009(2) 0.057(2) Uiso 0.58 1 d P O 3 H97A H 0.0615 -0.0079 0.4954 0.085 Uiso 0.58 1 calc PR O 3 H97B H 0.0295 -0.0780 0.5150 0.085 Uiso 0.58 1 calc PR O 3 H97C H 0.0491 -0.1059 0.4829 0.085 Uiso 0.58 1 calc PR O 3 C98A C 0.1588(5) -0.0913(7) 0.4929(2) 0.077(3) Uiso 0.58 1 d P O 3 H98A H 0.1553 -0.0305 0.4852 0.116 Uiso 0.58 1 calc PR O 3 H98B H 0.1488 -0.1330 0.4765 0.116 Uiso 0.58 1 calc PR O 3 H98C H 0.1980 -0.1020 0.5010 0.116 Uiso 0.58 1 calc PR O 3 C96B C 0.0892(5) -0.1870(8) 0.5274(2) 0.035(3) Uiso 0.42 1 d P O 4 H96D H 0.1098 -0.2104 0.5456 0.053 Uiso 0.42 1 calc PR O 4 H96E H 0.0880 -0.2322 0.5116 0.053 Uiso 0.42 1 calc PR O 4 H96F H 0.0504 -0.1714 0.5317 0.053 Uiso 0.42 1 calc PR O 4 C97B C 0.0959(6) -0.0672(8) 0.4906(3) 0.056(3) Uiso 0.42 1 d P O 4 H97D H 0.0877 -0.1141 0.4757 0.083 Uiso 0.42 1 calc PR O 4 H97E H 0.1223 -0.0244 0.4828 0.083 Uiso 0.42 1 calc PR O 4 H97F H 0.0605 -0.0370 0.4946 0.083 Uiso 0.42 1 calc PR O 4 C98B C 0.1831(6) -0.1427(9) 0.5105(3) 0.058(3) Uiso 0.42 1 d P O 4 H98D H 0.2002 -0.1711 0.5287 0.087 Uiso 0.42 1 calc PR O 4 H98E H 0.2074 -0.0940 0.5047 0.087 Uiso 0.42 1 calc PR O 4 H98F H 0.1791 -0.1863 0.4942 0.087 Uiso 0.42 1 calc PR O 4 O51 O 0.22182(15) 0.3956(2) 0.65307(8) 0.0568(10) Uani 1 1 d . S . O52 O 0.13720(13) 0.42251(19) 0.66926(7) 0.0386(8) Uani 1 1 d . S . C99 C 0.1895(2) 0.4343(3) 0.67004(10) 0.0352(11) Uani 1 1 d . . . C100 C 0.2156(2) 0.5018(3) 0.69269(12) 0.0497(14) Uani 1 1 d . P . C101 C 0.2770(7) 0.5128(11) 0.6930(4) 0.106(6) Uiso 0.50 1 d P P 1 H10C H 0.2896 0.5574 0.7080 0.159 Uiso 0.50 1 calc PR P 1 H10D H 0.2868 0.5322 0.6731 0.159 Uiso 0.50 1 calc PR P 1 H10E H 0.2957 0.4562 0.6980 0.159 Uiso 0.50 1 calc PR P 1 C102 C 0.1833(4) 0.4963(6) 0.7218(2) 0.039(2) Uiso 0.50 1 d P P 1 H10F H 0.1425 0.4908 0.7164 0.059 Uiso 0.50 1 calc PR P 1 H10G H 0.1906 0.5501 0.7338 0.059 Uiso 0.50 1 calc PR P 1 H10H H 0.1966 0.4446 0.7336 0.059 Uiso 0.50 1 calc PR P 1 C103 C 0.2083(8) 0.5886(12) 0.6798(4) 0.084(5) Uiso 0.50 1 d P P 1 H10I H 0.1677 0.6020 0.6766 0.126 Uiso 0.50 1 calc PR P 1 H10J H 0.2254 0.5904 0.6605 0.126 Uiso 0.50 1 calc PR P 1 H10K H 0.2268 0.6325 0.6934 0.126 Uiso 0.50 1 calc PR P 1 C111 C 0.2758(4) 0.4754(6) 0.7029(2) 0.032(2) Uiso 0.50 1 d P P 2 H11C H 0.2950 0.4535 0.6857 0.048 Uiso 0.50 1 calc PR P 2 H11D H 0.2752 0.4287 0.7181 0.048 Uiso 0.50 1 calc PR P 2 H11E H 0.2963 0.5270 0.7115 0.048 Uiso 0.50 1 calc PR P 2 C112 C 0.1765(5) 0.5396(8) 0.7121(3) 0.065(3) Uiso 0.50 1 d P P 2 H11F H 0.1965 0.5822 0.7257 0.097 Uiso 0.50 1 calc PR P 2 H11G H 0.1603 0.4924 0.7239 0.097 Uiso 0.50 1 calc PR P 2 H11H H 0.1459 0.5699 0.7000 0.097 Uiso 0.50 1 calc PR P 2 C113 C 0.2136(8) 0.5982(11) 0.6684(4) 0.088(5) Uiso 0.50 1 d P P 2 H11I H 0.2390 0.5889 0.6524 0.131 Uiso 0.50 1 calc PR P 2 H11J H 0.2261 0.6505 0.6802 0.131 Uiso 0.50 1 calc PR P 2 H11K H 0.1747 0.6075 0.6596 0.131 Uiso 0.50 1 calc PR P 2 O53 O 0.16746(18) 0.4265(2) 0.59487(8) 0.0639(12) Uani 1 1 d . Q . O54 O 0.08296(14) 0.43972(19) 0.61277(7) 0.0426(8) Uani 1 1 d . Q . C104 C 0.1208(3) 0.4642(3) 0.59677(10) 0.0470(14) Uani 1 1 d . . . C105 C 0.1191(5) 0.5519(7) 0.5811(2) 0.055(3) Uiso 0.58 1 d P Q 1 C106 C 0.1004(5) 0.6220(6) 0.5981(2) 0.057(3) Uiso 0.58 1 d P Q 1 H10L H 0.0686 0.6022 0.6093 0.086 Uiso 0.58 1 calc PR Q 1 H10M H 0.0879 0.6710 0.5848 0.086 Uiso 0.58 1 calc PR Q 1 H10N H 0.1316 0.6421 0.6123 0.086 Uiso 0.58 1 calc PR Q 1 C107 C 0.1678(5) 0.5732(7) 0.5631(2) 0.064(3) Uiso 0.58 1 d P Q 1 H10O H 0.1786 0.5203 0.5522 0.095 Uiso 0.58 1 calc PR Q 1 H10P H 0.2001 0.5931 0.5765 0.095 Uiso 0.58 1 calc PR Q 1 H10Q H 0.1568 0.6204 0.5487 0.095 Uiso 0.58 1 calc PR Q 1 C108 C 0.0682(6) 0.5249(8) 0.5501(3) 0.085(4) Uiso 0.58 1 d P Q 1 H10R H 0.0828 0.4760 0.5385 0.128 Uiso 0.58 1 calc PR Q 1 H10S H 0.0619 0.5769 0.5371 0.128 Uiso 0.58 1 calc PR Q 1 H10T H 0.0322 0.5072 0.5579 0.128 Uiso 0.58 1 calc PR Q 1 C115 C 0.0955(5) 0.5462(7) 0.5743(2) 0.024(2) Uiso 0.42 1 d P Q 2 C116 C 0.0687(7) 0.6114(10) 0.5891(3) 0.073(4) Uiso 0.42 1 d PD Q 2 H11L H 0.0971 0.6505 0.5994 0.109 Uiso 0.42 1 calc PR Q 2 H11M H 0.0454 0.5845 0.6039 0.109 Uiso 0.42 1 calc PR Q 2 H11N H 0.0443 0.6458 0.5746 0.109 Uiso 0.42 1 calc PR Q 2 C117 C 0.1375(7) 0.5561(9) 0.5519(3) 0.062(4) Uiso 0.42 1 d P Q 2 H11O H 0.1498 0.4975 0.5456 0.093 Uiso 0.42 1 calc PR Q 2 H11P H 0.1705 0.5891 0.5608 0.093 Uiso 0.42 1 calc PR Q 2 H11Q H 0.1204 0.5885 0.5345 0.093 Uiso 0.42 1 calc PR Q 2 C118 C 0.0309(12) 0.5276(17) 0.5633(6) 0.180(12) Uiso 0.42 1 d PD Q 2 H11R H 0.0287 0.4775 0.5494 0.270 Uiso 0.42 1 calc PR Q 2 H11S H 0.0145 0.5804 0.5532 0.270 Uiso 0.42 1 calc PR Q 2 H11T H 0.0096 0.5136 0.5807 0.270 Uiso 0.42 1 calc PR Q 2 N41 N 0.09622(15) 0.1866(2) 0.73825(7) 0.0294(8) Uani 1 1 d . . . N42 N 0.07530(15) 0.1488(2) 0.75806(8) 0.0319(8) Uani 1 1 d . . . N43 N 0.05592(19) 0.1128(3) 0.77768(9) 0.0513(11) Uani 1 1 d . . . N51 N 0.21562(18) -0.1452(3) 0.61792(10) 0.0490(11) Uani 1 1 d . . . N52A N 0.2572(6) -0.1723(8) 0.6283(3) 0.062(3) Uiso 0.42 1 d P R 1 N53A N 0.3039(8) -0.1976(10) 0.6372(4) 0.112(5) Uiso 0.42 1 d P R 1 N52B N 0.2568(4) -0.1709(5) 0.6039(2) 0.062(2) Uiso 0.58 1 d P R 2 N53B N 0.2922(6) -0.2011(9) 0.5905(3) 0.134(5) Uiso 0.58 1 d P R 2 N61A N 0.2903(3) 0.3661(4) 0.60685(15) 0.0297(17) Uiso 0.58 1 d P S 1 N61B N 0.2784(4) 0.3851(6) 0.59786(19) 0.022(2) Uiso 0.42 1 d PD S 2 N62 N 0.31057(18) 0.4314(3) 0.61467(9) 0.0485(11) Uani 1 1 d . . . N63A N 0.3273(4) 0.5046(5) 0.62138(17) 0.053(2) Uiso 0.58 1 d P S 1 N63B N 0.3484(5) 0.4646(7) 0.6305(2) 0.051(3) Uiso 0.42 1 d P S 2 O201 O 0.3371(3) 0.6399(5) 0.57305(13) 0.172(3) Uani 1 1 d D . . N201 N 0.2595(3) 0.0363(5) 0.46188(15) 0.117(3) Uani 1 1 d . . . C201 C 0.2488(4) -0.0167(6) 0.44410(17) 0.094(3) Uani 1 1 d . . . C202 C 0.2322(5) -0.0912(5) 0.42139(17) 0.146(4) Uani 1 1 d . . . H20C H 0.2617 -0.1370 0.4226 0.220 Uiso 1 1 calc R . . H20D H 0.2283 -0.0666 0.4010 0.220 Uiso 1 1 calc R . . H20E H 0.1959 -0.1173 0.4261 0.220 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 Fe1 0.0236(3) 0.0237(3) 0.0244(3) 0.0023(2) 0.0053(2) 0.0020(2) Fe2 0.0234(3) 0.0215(3) 0.0249(3) 0.0005(2) 0.0052(2) -0.0045(2) Fe3 0.0485(4) 0.0226(3) 0.0332(3) 0.0049(3) 0.0142(3) 0.0095(3) Fe4 0.0269(3) 0.0202(3) 0.0222(3) -0.0016(2) 0.0049(2) -0.0020(2) Fe5 0.0213(3) 0.0197(3) 0.0238(3) -0.0012(2) 0.0058(2) -0.0035(2) Fe6 0.0254(3) 0.0217(3) 0.0309(3) 0.0010(2) 0.0112(3) 0.0014(2) Fe7 0.0272(3) 0.0231(3) 0.0229(3) -0.0012(2) 0.0067(2) -0.0015(3) Fe8 0.0431(4) 0.0206(3) 0.0277(3) 0.0013(2) 0.0090(3) -0.0069(3) O1 0.0304(17) 0.0208(14) 0.0216(13) 0.0010(11) 0.0081(12) 0.0020(12) O2 0.0223(15) 0.0167(13) 0.0265(14) -0.0003(11) 0.0081(11) -0.0027(11) O3 0.0278(16) 0.0189(14) 0.0242(14) -0.0011(11) 0.0066(12) -0.0019(12) N1 0.027(2) 0.050(2) 0.0295(19) 0.0060(17) 0.0046(16) 0.0035(18) C1 0.036(3) 0.058(3) 0.033(2) 0.009(2) 0.004(2) 0.019(2) C2 0.041(3) 0.049(3) 0.038(3) 0.013(2) 0.006(2) 0.016(2) O7 0.0341(18) 0.0311(16) 0.0336(16) 0.0071(13) 0.0041(13) 0.0099(14) C3 0.024(3) 0.051(3) 0.042(3) 0.006(2) 0.000(2) -0.003(2) C4 0.020(2) 0.047(3) 0.036(2) 0.009(2) 0.0079(19) 0.002(2) O8 0.0177(15) 0.0309(16) 0.0295(15) 0.0053(12) 0.0040(12) -0.0021(12) C5 0.033(3) 0.059(3) 0.026(2) 0.005(2) -0.001(2) 0.000(2) C6 0.033(3) 0.037(2) 0.026(2) -0.0011(18) -0.0003(18) -0.008(2) O9 0.0234(16) 0.0300(15) 0.0253(14) -0.0037(12) 0.0021(12) -0.0033(12) N2 0.027(2) 0.0283(19) 0.0233(17) -0.0033(14) 0.0027(15) -0.0052(15) C7 0.029(3) 0.043(3) 0.026(2) -0.0002(19) -0.0019(19) -0.010(2) C8 0.026(3) 0.043(3) 0.031(2) 0.006(2) 0.0002(19) -0.004(2) O10 0.0241(16) 0.0325(16) 0.0237(14) 0.0030(12) 0.0031(12) -0.0031(12) C9 0.033(3) 0.025(2) 0.029(2) 0.0000(17) 0.0070(19) -0.0040(18) C10 0.031(2) 0.026(2) 0.026(2) 0.0011(17) 0.0059(18) -0.0075(18) O11 0.0278(16) 0.0233(14) 0.0229(14) -0.0009(11) 0.0068(12) -0.0084(12) C11 0.038(3) 0.038(3) 0.027(2) -0.0034(19) 0.0084(19) -0.006(2) C12 0.041(3) 0.054(3) 0.026(2) -0.004(2) 0.001(2) -0.009(2) N3 0.035(2) 0.037(2) 0.039(2) 0.0093(17) 0.0170(18) 0.0100(17) C13 0.027(3) 0.055(3) 0.048(3) 0.009(2) 0.016(2) 0.010(2) C14 0.021(2) 0.055(3) 0.051(3) 0.002(2) 0.009(2) -0.005(2) O13 0.0167(15) 0.0350(16) 0.0348(16) -0.0001(13) 0.0069(12) -0.0028(12) C15 0.048(3) 0.037(3) 0.042(3) 0.011(2) 0.026(2) 0.010(2) C16 0.041(3) 0.035(3) 0.032(2) 0.0023(19) 0.017(2) 0.012(2) O14 0.0350(18) 0.0268(15) 0.0258(14) -0.0017(12) 0.0095(13) 0.0052(13) C17 0.057(4) 0.038(3) 0.048(3) 0.012(2) 0.029(3) 0.021(2) C18 0.075(4) 0.052(3) 0.070(4) 0.020(3) 0.039(3) 0.033(3) O15 0.122(4) 0.068(3) 0.051(2) 0.016(2) 0.033(3) 0.057(3) N4 0.070(3) 0.025(2) 0.047(2) -0.0037(18) 0.025(2) -0.018(2) C19 0.050(4) 0.050(3) 0.064(4) -0.008(3) -0.001(3) -0.029(3) C20 0.052(3) 0.043(3) 0.046(3) -0.003(2) -0.008(2) -0.024(3) O16 0.0328(18) 0.0304(16) 0.0295(15) -0.0003(12) 0.0016(13) -0.0159(13) C21 0.082(5) 0.029(3) 0.050(3) -0.006(2) 0.028(3) -0.021(3) C22 0.074(4) 0.022(2) 0.051(3) 0.003(2) 0.030(3) 0.004(2) O17 0.058(2) 0.0178(15) 0.0458(18) 0.0022(13) 0.0206(16) -0.0019(14) C23 0.097(5) 0.043(3) 0.066(4) -0.003(3) 0.039(4) -0.007(3) C24 0.069(5) 0.071(4) 0.079(4) -0.012(4) 0.013(4) 0.006(4) O18 0.096(4) 0.061(3) 0.114(4) 0.015(3) 0.039(3) 0.009(3) O19 0.052(2) 0.052(2) 0.052(2) 0.0231(17) 0.0257(17) 0.0261(17) O20 0.0366(19) 0.0482(19) 0.0291(16) 0.0056(14) 0.0094(14) 0.0133(15) C25 0.039(3) 0.032(2) 0.030(2) -0.0021(19) 0.008(2) 0.007(2) C26 0.038(3) 0.045(3) 0.034(2) 0.003(2) 0.010(2) 0.015(2) O21 0.106(3) 0.0246(17) 0.0372(19) -0.0027(14) 0.010(2) 0.0099(18) O22 0.065(2) 0.0235(17) 0.0375(18) -0.0072(13) -0.0009(16) -0.0052(15) C30 0.056(3) 0.031(3) 0.037(3) -0.002(2) 0.017(2) -0.005(2) C31 0.102(5) 0.027(3) 0.047(3) -0.008(2) 0.027(3) -0.004(3) O23 0.041(2) 0.0349(17) 0.0342(16) -0.0150(13) 0.0136(14) -0.0123(14) O24 0.038(2) 0.0287(17) 0.059(2) -0.0150(15) 0.0180(16) -0.0044(14) C35 0.045(3) 0.024(2) 0.031(2) 0.0006(18) 0.008(2) -0.008(2) C36 0.057(4) 0.035(3) 0.048(3) -0.018(2) 0.020(3) -0.015(2) C37 0.064(4) 0.052(3) 0.052(3) -0.020(3) 0.003(3) -0.023(3) C38 0.070(4) 0.029(3) 0.066(4) -0.015(2) 0.002(3) -0.004(3) C39 0.075(5) 0.084(4) 0.069(4) -0.047(3) 0.034(3) -0.030(4) O25 0.0339(19) 0.0363(18) 0.0421(18) 0.0144(14) 0.0159(14) 0.0079(14) O26 0.0352(19) 0.0345(17) 0.0488(19) 0.0144(14) 0.0184(15) 0.0108(14) C40 0.032(3) 0.023(2) 0.027(2) -0.0003(17) 0.0096(18) 0.0000(18) C41 0.039(3) 0.029(2) 0.035(2) 0.0046(19) 0.008(2) 0.011(2) C42 0.069(5) 0.085(5) 0.134(6) 0.057(5) -0.030(5) 0.012(4) C43 0.102(5) 0.075(4) 0.043(3) 0.031(3) 0.030(3) 0.051(4) C44 0.180(8) 0.023(3) 0.048(3) 0.007(2) 0.011(4) 0.019(4) O27 0.040(2) 0.0285(16) 0.0316(16) 0.0014(13) 0.0009(14) 0.0021(14) O28 0.056(2) 0.0279(16) 0.0344(17) 0.0060(13) 0.0015(16) -0.0092(15) C45 0.029(3) 0.030(2) 0.033(2) 0.0032(19) 0.0139(19) 0.0024(19) C46 0.036(3) 0.030(2) 0.040(3) 0.008(2) 0.009(2) 0.005(2) O29 0.0355(19) 0.0344(17) 0.0338(16) -0.0051(13) 0.0148(14) -0.0091(14) O30 0.041(2) 0.0376(18) 0.0383(18) -0.0020(14) 0.0122(15) -0.0105(15) C50 0.031(3) 0.028(2) 0.034(2) 0.0084(19) 0.007(2) 0.0032(19) C51 0.029(3) 0.043(3) 0.054(3) 0.018(2) 0.017(2) -0.003(2) N11 0.061(3) 0.036(2) 0.052(3) 0.0114(19) 0.011(2) 0.015(2) N12 0.029(3) 0.060(3) 0.121(5) 0.048(3) 0.004(3) 0.003(2) N21 0.034(2) 0.030(2) 0.0287(19) -0.0060(15) 0.0080(16) -0.0119(16) N22 0.044(3) 0.039(2) 0.041(2) -0.0046(19) 0.0173(19) -0.011(2) N23 0.066(3) 0.061(3) 0.060(3) -0.024(2) 0.019(2) -0.034(3) N31 0.042(2) 0.036(2) 0.030(2) -0.0047(16) 0.0034(18) 0.0007(18) N32 0.028(2) 0.088(3) 0.026(2) -0.003(2) 0.0058(17) 0.006(2) Fe9 0.0227(3) 0.0290(3) 0.0234(3) -0.0060(2) 0.0041(2) -0.0002(3) Fe10 0.0209(3) 0.0208(3) 0.0202(3) -0.0006(2) 0.0056(2) -0.0012(2) Fe11 0.0225(3) 0.0245(3) 0.0190(3) -0.0032(2) 0.0039(2) -0.0043(2) Fe12 0.0293(3) 0.0223(3) 0.0192(3) -0.0012(2) 0.0020(2) -0.0071(2) Fe13 0.0269(4) 0.0266(3) 0.0350(3) -0.0098(3) 0.0008(3) 0.0039(3) Fe14 0.0294(3) 0.0248(3) 0.0266(3) -0.0067(2) 0.0123(3) -0.0062(3) Fe15 0.0349(4) 0.0278(3) 0.0407(4) -0.0151(3) 0.0219(3) -0.0129(3) Fe16 0.0284(3) 0.0208(3) 0.0295(3) -0.0030(2) 0.0097(3) -0.0003(2) O4 0.0245(16) 0.0173(13) 0.0187(13) -0.0021(10) 0.0051(11) -0.0033(11) O5 0.0262(16) 0.0242(14) 0.0251(14) -0.0068(11) 0.0052(12) -0.0011(12) O6 0.0255(16) 0.0199(14) 0.0262(14) -0.0053(11) 0.0093(12) -0.0037(11) N5 0.027(2) 0.057(3) 0.036(2) -0.0149(19) 0.0035(17) -0.0051(19) C56 0.026(3) 0.051(3) 0.038(3) -0.016(2) 0.002(2) -0.005(2) O31 0.0211(16) 0.0374(16) 0.0253(14) -0.0088(12) 0.0034(12) -0.0066(13) C58 0.062(4) 0.049(3) 0.054(3) -0.005(3) -0.032(3) 0.011(3) O32 0.0295(17) 0.0318(16) 0.0329(16) -0.0032(13) -0.0026(13) 0.0053(13) C60 0.019(3) 0.117(5) 0.044(3) -0.009(3) 0.009(2) -0.001(3) O33 0.0222(17) 0.0417(18) 0.0356(16) -0.0130(13) 0.0072(13) -0.0072(13) N6 0.035(2) 0.031(2) 0.0231(17) -0.0030(14) 0.0051(15) -0.0118(16) C61 0.030(3) 0.036(2) 0.027(2) -0.0064(18) -0.0012(18) -0.013(2) C62 0.031(3) 0.038(2) 0.023(2) -0.0016(18) -0.0007(18) -0.005(2) O34 0.0209(15) 0.0271(15) 0.0208(13) -0.0009(11) 0.0000(11) -0.0042(12) C63 0.040(3) 0.028(2) 0.032(2) -0.0074(18) 0.004(2) -0.009(2) C64 0.046(3) 0.020(2) 0.046(3) -0.0084(19) 0.004(2) -0.007(2) O35 0.0298(17) 0.0197(14) 0.0414(17) -0.0050(12) 0.0045(13) -0.0018(12) C65 0.040(3) 0.038(3) 0.036(2) -0.002(2) 0.005(2) -0.015(2) C66 0.059(4) 0.048(3) 0.049(3) -0.005(2) 0.009(3) -0.027(3) O36A 0.110(5) 0.033(3) 0.076(3) -0.018(2) 0.046(3) -0.027(3) N7 0.054(3) 0.042(2) 0.0264(19) -0.0031(17) 0.0158(18) -0.018(2) C67 0.056(4) 0.054(3) 0.024(2) 0.010(2) 0.004(2) -0.014(3) C68 0.043(3) 0.040(3) 0.032(2) 0.014(2) 0.005(2) 0.000(2) O37 0.0312(17) 0.0276(15) 0.0196(13) 0.0035(11) 0.0059(12) -0.0015(12) C69 0.062(4) 0.039(3) 0.034(3) 0.006(2) 0.016(2) -0.015(2) C70 0.051(3) 0.034(3) 0.044(3) -0.004(2) 0.028(2) -0.017(2) O38 0.0349(18) 0.0262(15) 0.0349(16) -0.0069(12) 0.0149(14) -0.0121(13) C71 0.083(4) 0.066(4) 0.034(3) -0.014(2) 0.034(3) -0.033(3) C72 0.058(4) 0.151(7) 0.040(3) -0.017(4) 0.024(3) -0.027(4) O39A 0.046(3) 0.053(3) 0.042(2) 0.001(2) 0.004(2) 0.004(2) N8 0.043(2) 0.0244(19) 0.041(2) -0.0014(16) 0.0123(18) 0.0053(17) C73 0.031(3) 0.038(3) 0.044(3) -0.001(2) 0.003(2) 0.011(2) C74 0.022(2) 0.038(3) 0.039(2) -0.006(2) 0.0020(19) 0.0041(19) O40 0.0216(16) 0.0237(14) 0.0307(15) -0.0008(12) 0.0038(12) 0.0022(12) C75 0.040(3) 0.034(3) 0.043(3) -0.004(2) 0.019(2) 0.005(2) C76 0.042(3) 0.035(3) 0.033(2) -0.0077(19) 0.017(2) 0.007(2) O41 0.0353(18) 0.0268(15) 0.0262(15) -0.0041(12) 0.0104(13) 0.0066(13) C77 0.054(4) 0.033(3) 0.062(3) -0.005(2) 0.023(3) -0.002(2) C78 0.043(3) 0.042(3) 0.077(4) -0.007(3) 0.022(3) -0.002(2) O42 0.091(3) 0.0319(19) 0.094(3) -0.0138(19) 0.056(3) -0.0016(19) O43 0.054(2) 0.0263(16) 0.0236(15) 0.0000(12) -0.0019(14) -0.0025(14) O44 0.060(2) 0.0325(17) 0.0268(16) 0.0068(13) -0.0069(15) -0.0151(16) C79 0.038(3) 0.028(2) 0.024(2) -0.0006(17) 0.0007(19) -0.0011(19) C80 0.046(3) 0.023(2) 0.027(2) 0.0046(17) 0.002(2) -0.001(2) C81 0.063(4) 0.049(3) 0.045(3) 0.021(2) 0.010(3) 0.001(3) C82 0.058(4) 0.035(3) 0.041(3) 0.003(2) 0.005(2) 0.000(2) C83 0.069(4) 0.035(3) 0.032(3) 0.007(2) -0.009(2) 0.002(2) O45 0.0272(17) 0.0505(19) 0.0325(16) -0.0157(14) 0.0097(13) -0.0108(15) O46 0.0350(19) 0.0427(18) 0.0295(16) -0.0128(13) 0.0124(13) -0.0155(14) C84 0.027(2) 0.030(2) 0.026(2) -0.0013(17) 0.0045(18) -0.0076(19) C85 0.029(3) 0.051(3) 0.037(3) -0.009(2) 0.010(2) -0.014(2) C86 0.033(3) 0.116(5) 0.056(3) 0.009(3) 0.004(3) -0.008(3) C87 0.055(4) 0.130(6) 0.073(4) 0.045(4) 0.027(3) -0.007(4) C88 0.061(5) 0.104(6) 0.196(8) -0.101(6) 0.081(5) -0.041(4) O47 0.0287(18) 0.0440(19) 0.0430(19) -0.0138(15) 0.0071(15) 0.0036(14) O48 0.0293(19) 0.0435(19) 0.0406(18) -0.0130(15) 0.0172(15) -0.0051(15) C89 0.029(3) 0.047(3) 0.048(3) -0.031(2) 0.014(2) -0.006(2) C90 0.026(3) 0.082(4) 0.058(3) -0.031(3) 0.018(2) 0.003(3) O49 0.040(2) 0.0319(17) 0.0381(18) -0.0155(14) -0.0020(15) 0.0025(14) O50 0.0386(19) 0.0325(17) 0.0318(16) -0.0095(13) 0.0070(14) -0.0053(14) C94 0.021(2) 0.032(2) 0.039(3) -0.011(2) 0.0094(19) -0.0042(19) C95 0.062(4) 0.036(3) 0.030(2) -0.012(2) 0.013(2) -0.010(2) O51 0.044(2) 0.061(2) 0.069(2) -0.0432(19) 0.0311(18) -0.0262(18) O52 0.0307(19) 0.0344(17) 0.052(2) -0.0218(15) 0.0114(15) -0.0044(14) C99 0.040(3) 0.030(2) 0.037(2) -0.0123(19) 0.009(2) -0.006(2) C100 0.034(3) 0.049(3) 0.069(3) -0.033(3) 0.020(3) -0.009(2) O53 0.089(3) 0.0299(19) 0.081(3) 0.0125(18) 0.060(2) 0.0057(19) O54 0.051(2) 0.0277(17) 0.051(2) 0.0087(14) 0.0145(17) -0.0003(15) C104 0.080(4) 0.024(2) 0.040(3) -0.001(2) 0.026(3) -0.002(3) N41 0.034(2) 0.034(2) 0.0209(17) -0.0055(15) 0.0053(15) -0.0071(16) N42 0.028(2) 0.038(2) 0.0292(19) -0.0037(17) 0.0006(16) -0.0004(17) N43 0.055(3) 0.065(3) 0.036(2) 0.012(2) 0.019(2) -0.001(2) N51 0.041(3) 0.034(2) 0.069(3) -0.012(2) -0.009(2) 0.016(2) N62 0.047(3) 0.062(3) 0.039(2) -0.018(2) 0.019(2) -0.030(2) O201 0.214(8) 0.182(7) 0.106(5) -0.036(4) -0.067(5) 0.053(6) N201 0.107(6) 0.170(8) 0.078(5) -0.015(5) 0.021(4) 0.036(5) C201 0.108(7) 0.108(7) 0.072(5) 0.010(4) 0.031(5) 0.051(5) C202 0.265(14) 0.085(6) 0.095(6) -0.006(5) 0.049(7) 0.045(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 Fe1 O8 1.943(3) . ? Fe1 O7 1.944(3) . ? Fe1 O9 1.947(3) . ? Fe1 O1 2.168(3) . ? Fe1 O2 2.217(3) . ? Fe1 O3 2.240(3) . ? Fe1 N1 2.592(4) . ? Fe1 Fe2 2.9116(8) . ? Fe2 O16 1.944(3) . ? Fe2 O13 1.946(3) . ? Fe2 O10 1.953(3) . ? Fe2 O2 2.068(3) . ? Fe2 O1 2.085(3) . ? Fe2 O3 2.088(3) . ? Fe2 Fe6 2.9741(8) . ? Fe3 O17 1.994(3) . ? Fe3 O7 1.995(3) . ? Fe3 O1 2.009(3) . ? Fe3 N11 2.022(4) . ? Fe3 O21 2.047(3) . ? Fe3 O19 2.096(3) . ? Fe4 O1 1.944(2) . ? Fe4 O11 1.986(3) . ? Fe4 O10 1.989(3) . ? Fe4 O20 1.994(3) . ? Fe4 O22 2.047(3) . ? Fe4 N2 2.281(3) . ? Fe5 O8 1.976(3) . ? Fe5 O11 1.994(2) . ? Fe5 O2 2.006(2) . ? Fe5 O25 2.031(3) . ? Fe5 N21 2.047(3) . ? Fe5 O23 2.073(3) . ? Fe6 O2 1.939(2) . ? Fe6 O13 1.987(3) . ? Fe6 O14 1.996(3) . ? Fe6 O24 2.003(3) . ? Fe6 O26 2.046(3) . ? Fe6 N3 2.274(4) . ? Fe7 O9 1.966(3) . ? Fe7 O3 1.978(2) . ? Fe7 O14 1.983(3) . ? Fe7 O29 2.021(3) . ? Fe7 N31 2.082(3) . ? Fe7 O27 2.097(3) . ? Fe8 O3 1.944(3) . ? Fe8 O17 1.972(3) . ? Fe8 O16 1.992(3) . ? Fe8 O28 2.008(3) . ? Fe8 O30 2.044(3) . ? Fe8 N4 2.311(4) . ? N1 C1 1.463(6) . ? N1 C3 1.467(5) . ? N1 C5 1.469(5) . ? C1 C2 1.518(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O7 1.432(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.509(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O8 1.419(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.514(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O9 1.421(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N2 C9 1.477(5) . ? N2 C7 1.486(5) . ? N2 C11 1.496(5) . ? C7 C8 1.526(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O10 1.423(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.506(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O11 1.428(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.524(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O12A 1.332(7) . ? C12 O12B 1.360(8) . ? C12 H12C 0.9900 . ? C12 H12D 0.9900 . ? C12 H12E 0.9900 . ? C12 H12F 0.9900 . ? O12A H12A 0.8400 . ? O12B H12B 0.8400 . ? N3 C13 1.478(6) . ? N3 C17 1.486(5) . ? N3 C15 1.496(5) . ? C13 C14 1.516(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O13 1.419(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.497(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O14 1.435(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.520(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O15 1.443(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? O15 H15 0.8400 . ? N4 C19 1.467(7) . ? N4 C21 1.486(6) . ? N4 C23 1.501(6) . ? C19 C20 1.529(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O16 1.414(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.480(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O17 1.449(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.435(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O18 1.431(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? O18 H18 0.8400 . ? O19 C25 1.251(5) . ? O20 C25 1.257(5) . ? C25 C26 1.534(6) . ? C26 C28B 1.438(17) . ? C26 C29A 1.468(9) . ? C26 C27B 1.521(16) . ? C26 C27A 1.571(8) . ? C26 C28A 1.599(9) . ? C26 C29B 1.604(13) . ? C27A H27A 0.9800 . ? C27A H27B 0.9800 . ? C27A H27C 0.9800 . ? C28A H28A 0.9800 . ? C28A H28B 0.9800 . ? C28A H28C 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C27B H27D 0.9800 . ? C27B H27E 0.9800 . ? C27B H27F 0.9800 . ? C28B H28D 0.9800 . ? C28B H28E 0.9800 . ? C28B H28F 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? O21 C30 1.253(6) . ? O22 C30 1.235(5) . ? C30 C31 1.559(6) . ? C31 C33B 1.413(17) . ? C31 C32A 1.466(16) . ? C31 C34A 1.483(11) . ? C31 C32B 1.544(16) . ? C31 C34B 1.573(14) . ? C31 C33A 1.687(13) . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C33A H33A 0.9800 . ? C33A H33B 0.9800 . ? C33A H33C 0.9800 . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C33B H33D 0.9800 . ? C33B H33E 0.9800 . ? C33B H33F 0.9800 . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? O23 C35 1.252(5) . ? O24 C35 1.262(5) . ? C35 C36 1.535(6) . ? C36 C39 1.507(6) . ? C36 C38 1.514(7) . ? C36 C37 1.546(7) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? O25 C40 1.250(5) . ? O26 C40 1.264(5) . ? C40 C41 1.533(6) . ? C41 C44 1.496(6) . ? C41 C43 1.515(6) . ? C41 C42 1.519(8) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? O27 C45 1.256(5) . ? O28 C45 1.273(5) . ? C45 C46 1.540(6) . ? C46 C48A 1.478(9) . ? C46 C47B 1.520(15) . ? C46 C49A 1.521(9) . ? C46 C49B 1.530(13) . ? C46 C47A 1.569(8) . ? C46 C48B 1.634(13) . ? C47A H47A 0.9800 . ? C47A H47B 0.9800 . ? C47A H47C 0.9800 . ? C48A H48A 0.9800 . ? C48A H48B 0.9800 . ? C48A H48C 0.9800 . ? C49A H49A 0.9800 . ? C49A H49B 0.9800 . ? C49A H49C 0.9800 . ? C47B H47D 0.9800 . ? C47B H47E 0.9800 . ? C47B H47F 0.9800 . ? C48B H48D 0.9800 . ? C48B H48E 0.9800 . ? C48B H48F 0.9800 . ? C49B H49D 0.9800 . ? C49B H49E 0.9800 . ? C49B H49F 0.9800 . ? O29 C50 1.254(5) . ? O30 C50 1.260(5) . ? C50 C51 1.529(6) . ? C51 C52B 1.417(10) . ? C51 C54A 1.451(14) . ? C51 C53A 1.453(14) . ? C51 C53B 1.591(16) . ? C51 C54B 1.632(9) . ? C51 C52A 1.670(14) . ? C52A H52A 0.9800 . ? C52A H52B 0.9800 . ? C52A H52C 0.9800 . ? C53A H53A 0.9800 . ? C53A H53B 0.9800 . ? C53A H53C 0.9800 . ? C54A H54A 0.9800 . ? C54A H54B 0.9800 . ? C54A H54C 0.9800 . ? C52B H52D 0.9800 . ? C52B H52E 0.9800 . ? C52B H52F 0.9800 . ? C53B H53D 0.9800 . ? C53B H53E 0.9800 . ? C53B H53F 0.9800 . ? C54B H54D 0.9800 . ? C54B H54E 0.9800 . ? C54B H54F 0.9800 . ? N11 N12 1.155(6) . ? N12 N13A 1.168(9) . ? N12 N13B 1.232(17) . ? N21 N22 1.198(5) . ? N22 N23 1.160(5) . ? N31 N32 1.168(5) . ? N32 N33B 1.138(8) . ? N32 N33A 1.299(9) . ? Fe9 O32 1.943(3) . ? Fe9 O31 1.955(3) . ? Fe9 O33 1.959(3) . ? Fe9 O6 2.201(3) . ? Fe9 O5 2.239(3) . ? Fe9 O4 2.288(3) . ? Fe9 N5 2.466(4) . ? Fe9 Fe10 2.9230(8) . ? Fe10 O37 1.945(2) . ? Fe10 O40 1.947(3) . ? Fe10 O34 1.964(3) . ? Fe10 O4 2.043(2) . ? Fe10 O5 2.063(3) . ? Fe10 O6 2.086(3) . ? Fe10 Fe12 2.9653(7) . ? Fe10 Fe14 2.9769(7) . ? Fe11 O4 1.971(2) . ? Fe11 O31 1.974(3) . ? Fe11 O41 2.004(3) . ? Fe11 O45 2.035(3) . ? Fe11 N41 2.063(3) . ? Fe11 O43 2.101(3) . ? Fe12 O4 1.947(2) . ? Fe12 O44 1.969(3) . ? Fe12 O34 1.972(3) . ? Fe12 O35 1.989(3) . ? Fe12 O46 2.053(3) . ? Fe12 N6 2.253(3) . ? Fe13 O32 1.975(3) . ? Fe13 O35 1.986(3) . ? Fe13 O5 2.007(3) . ? Fe13 N51 2.029(4) . ? Fe13 O49 2.039(3) . ? Fe13 O47 2.093(3) . ? Fe14 O5 1.938(3) . ? Fe14 O48 1.985(3) . ? Fe14 O37 1.988(3) . ? Fe14 O38 1.999(3) . ? Fe14 O50 2.071(3) . ? Fe14 N7 2.268(4) . ? Fe15 O33 1.980(3) . ? Fe15 O38 1.988(3) . ? Fe15 O6 2.001(3) . ? Fe15 O53 2.018(4) . ? Fe15 N61B 2.072(8) . ? Fe15 N61A 2.079(7) . ? Fe15 O51 2.099(3) . ? Fe16 O6 1.948(3) . ? Fe16 O41 1.980(3) . ? Fe16 O40 1.982(3) . ? Fe16 O52 1.997(3) . ? Fe16 O54 2.038(3) . ? Fe16 N8 2.334(4) . ? N5 C57B 1.307(15) . ? N5 C59A 1.434(8) . ? N5 C59B 1.473(14) . ? N5 C55A 1.498(7) . ? N5 C57A 1.536(8) . ? N5 C55B 1.537(13) . ? C55A C56 1.481(8) . ? C55A H55A 0.9900 . ? C55A H55B 0.9900 . ? C55B C56 1.428(14) . ? C55B H55C 0.9900 . ? C55B H55D 0.9900 . ? C56 O31 1.419(5) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C56 H56C 0.9900 . ? C56 H56D 0.9900 . ? C57A C58 1.410(8) . ? C57A H57A 0.9900 . ? C57A H57B 0.9900 . ? C57B C58 1.468(16) . ? C57B H57C 0.9900 . ? C57B H57D 0.9900 . ? C58 O32 1.435(5) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C58 H58C 0.9900 . ? C58 H58D 0.9900 . ? C59A C60 1.504(8) . ? C59A H59A 0.9900 . ? C59A H59B 0.9900 . ? C59B C60 1.335(14) . ? C59B H59C 0.9900 . ? C59B H59D 0.9900 . ? C60 O33 1.413(5) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C60 H60C 0.9900 . ? C60 H60D 0.9900 . ? N6 C63 1.483(5) . ? N6 C61 1.484(5) . ? N6 C65 1.508(5) . ? C61 C62 1.528(5) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 O34 1.416(5) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.500(6) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 O35 1.438(4) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.525(6) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 O36A 1.417(7) . ? C66 O36B 1.42(2) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C66 H66C 0.9900 . ? C66 H66D 0.9900 . ? O36A H36A 0.8400 . ? N7 C67 1.473(6) . ? N7 C69 1.489(5) . ? N7 C71 1.504(6) . ? C67 C68 1.534(6) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 O37 1.415(5) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.492(7) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 O38 1.438(5) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.482(7) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 O39A 1.299(7) . ? C72 O39B 1.659(14) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C72 H72C 0.9900 . ? C72 H72D 0.9900 . ? O39A H39D 0.8400 . ? N8 C75 1.489(5) . ? N8 C73 1.492(6) . ? N8 C77 1.494(5) . ? C73 C74 1.513(6) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 O40 1.430(5) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.528(6) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 O41 1.425(4) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C78 1.484(7) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 O42 1.461(6) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? O42 H42 0.8400 . ? O43 C79 1.256(5) . ? O44 C79 1.255(5) . ? C79 C80 1.527(5) . ? C80 C83 1.504(6) . ? C80 C82 1.528(6) . ? C80 C81 1.540(6) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? O45 C84 1.259(5) . ? O46 C84 1.252(4) . ? C84 C85 1.527(6) . ? C85 C88 1.497(7) . ? C85 C86 1.523(7) . ? C85 C87 1.540(7) . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? O47 C89 1.248(6) . ? O48 C89 1.278(6) . ? C89 C90 1.543(6) . ? C90 C93A 1.414(11) . ? C90 C91B 1.460(13) . ? C90 C92B 1.482(12) . ? C90 C92A 1.546(11) . ? C90 C93B 1.604(12) . ? C90 C91A 1.705(13) . ? C91A H91A 0.9800 . ? C91A H91B 0.9800 . ? C91A H91C 0.9800 . ? C92A H92A 0.9800 . ? C92A H92B 0.9800 . ? C92A H92C 0.9800 . ? C93A H93A 0.9800 . ? C93A H93B 0.9800 . ? C93A H93C 0.9800 . ? C91B H91D 0.9800 . ? C91B H91E 0.9800 . ? C91B H91F 0.9800 . ? C92B H92D 0.9800 . ? C92B H92E 0.9800 . ? C92B H92F 0.9800 . ? C93B H93D 0.9800 . ? C93B H93E 0.9800 . ? C93B H93F 0.9800 . ? O49 C94 1.247(5) . ? O50 C94 1.272(5) . ? C94 C95 1.542(6) . ? C95 C97B 1.377(13) . ? C95 C96A 1.466(10) . ? C95 C98A 1.472(11) . ? C95 C96B 1.547(12) . ? C95 C97A 1.637(11) . ? C95 C98B 1.644(14) . ? C96A H96A 0.9800 . ? C96A H96B 0.9800 . ? C96A H96C 0.9800 . ? C97A H97A 0.9800 . ? C97A H97B 0.9800 . ? C97A H97C 0.9800 . ? C98A H98A 0.9800 . ? C98A H98B 0.9800 . ? C98A H98C 0.9800 . ? C96B H96D 0.9800 . ? C96B H96E 0.9800 . ? C96B H96F 0.9800 . ? C97B H97D 0.9800 . ? C97B H97E 0.9800 . ? C97B H97F 0.9800 . ? C98B H98D 0.9800 . ? C98B H98E 0.9800 . ? C98B H98F 0.9800 . ? O51 C99 1.261(5) . ? O52 C99 1.246(5) . ? C99 C100 1.531(6) . ? C100 C112 1.435(12) . ? C100 C103 1.436(17) . ? C100 C101 1.457(17) . ? C100 C111 1.511(10) . ? C100 C102 1.562(10) . ? C100 C113 1.813(17) . ? C101 C103 2.03(2) . ? C101 H10C 0.9800 . ? C101 H10D 0.9800 . ? C101 H10E 0.9800 . ? C102 H10F 0.9800 . ? C102 H10G 0.9800 . ? C102 H10H 0.9800 . ? C103 H10I 0.9800 . ? C103 H10J 0.9800 . ? C103 H10K 0.9800 . ? C111 H11C 0.9800 . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C112 H11F 0.9800 . ? C112 H11G 0.9800 . ? C112 H11H 0.9800 . ? C113 H11I 0.9800 . ? C113 H11J 0.9800 . ? C113 H11K 0.9800 . ? O53 C104 1.249(6) . ? O54 C104 1.244(5) . ? C104 C105 1.498(11) . ? C104 C115 1.674(11) . ? C105 C106 1.397(13) . ? C105 C107 1.489(14) . ? C105 C108 1.805(16) . ? C106 H10L 0.9800 . ? C106 H10M 0.9800 . ? C106 H10N 0.9800 . ? C107 H10O 0.9800 . ? C107 H10P 0.9800 . ? C107 H10Q 0.9800 . ? C108 H10R 0.9800 . ? C108 H10S 0.9800 . ? C108 H10T 0.9800 . ? C115 C116 1.368(18) . ? C115 C117 1.471(17) . ? C115 C118 1.59(3) . ? C116 H11L 0.9800 . ? C116 H11M 0.9800 . ? C116 H11N 0.9800 . ? C117 H11O 0.9800 . ? C117 H11P 0.9800 . ? C117 H11Q 0.9800 . ? C118 H11R 0.9800 . ? C118 H11S 0.9800 . ? C118 H11T 0.9800 . ? N41 N42 1.193(4) . ? N42 N43 1.156(5) . ? N51 N52A 1.129(13) . ? N51 N52B 1.259(10) . ? N52A N53A 1.204(18) . ? N52B N53B 1.159(14) . ? N61A N62 1.138(7) . ? N61B N62 1.240(9) . ? N62 N63B 1.203(11) . ? N62 N63A 1.205(8) . ? N201 C201 1.142(9) . ? C201 C202 1.544(11) . ? C202 H20C 0.9800 . ? C202 H20D 0.9800 . ? C202 H20E 0.9800 . ? 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 O8 Fe1 O7 112.65(12) . . ? O8 Fe1 O9 109.84(11) . . ? O7 Fe1 O9 108.90(11) . . ? O8 Fe1 O1 91.83(10) . . ? O7 Fe1 O1 77.11(11) . . ? O9 Fe1 O1 151.81(11) . . ? O8 Fe1 O2 76.42(10) . . ? O7 Fe1 O2 152.46(11) . . ? O9 Fe1 O2 90.78(10) . . ? O1 Fe1 O2 76.64(9) . . ? O8 Fe1 O3 151.65(11) . . ? O7 Fe1 O3 89.79(11) . . ? O9 Fe1 O3 76.54(10) . . ? O1 Fe1 O3 75.96(9) . . ? O2 Fe1 O3 75.90(9) . . ? O8 Fe1 N1 71.05(11) . . ? O7 Fe1 N1 72.35(12) . . ? O9 Fe1 N1 71.24(11) . . ? O1 Fe1 N1 134.94(11) . . ? O2 Fe1 N1 133.88(11) . . ? O3 Fe1 N1 134.94(10) . . ? O8 Fe1 Fe2 108.26(8) . . ? O7 Fe1 Fe2 108.67(9) . . ? O9 Fe1 Fe2 108.42(8) . . ? O1 Fe1 Fe2 45.61(7) . . ? O2 Fe1 Fe2 45.09(7) . . ? O3 Fe1 Fe2 45.56(7) . . ? N1 Fe1 Fe2 178.97(9) . . ? O16 Fe2 O13 95.21(12) . . ? O16 Fe2 O10 98.04(11) . . ? O13 Fe2 O10 97.92(11) . . ? O16 Fe2 O2 159.55(10) . . ? O13 Fe2 O2 80.22(11) . . ? O10 Fe2 O2 102.32(10) . . ? O16 Fe2 O1 103.96(11) . . ? O13 Fe2 O1 160.83(11) . . ? O10 Fe2 O1 79.47(10) . . ? O2 Fe2 O1 81.80(10) . . ? O16 Fe2 O3 79.12(11) . . ? O13 Fe2 O3 102.98(11) . . ? O10 Fe2 O3 159.07(11) . . ? O2 Fe2 O3 82.50(10) . . ? O1 Fe2 O3 81.12(10) . . ? O16 Fe2 Fe1 120.77(9) . . ? O13 Fe2 Fe1 121.00(8) . . ? O10 Fe2 Fe1 118.54(8) . . ? O2 Fe2 Fe1 49.38(7) . . ? O1 Fe2 Fe1 48.01(7) . . ? O3 Fe2 Fe1 49.97(7) . . ? O16 Fe2 Fe6 128.07(9) . . ? O13 Fe2 Fe6 41.39(8) . . ? O10 Fe2 Fe6 112.15(8) . . ? O2 Fe2 Fe6 40.45(7) . . ? O1 Fe2 Fe6 121.92(7) . . ? O3 Fe2 Fe6 84.87(7) . . ? Fe1 Fe2 Fe6 80.82(2) . . ? O17 Fe3 O7 94.10(12) . . ? O17 Fe3 O1 94.53(11) . . ? O7 Fe3 O1 79.83(11) . . ? O17 Fe3 N11 90.62(16) . . ? O7 Fe3 N11 91.42(15) . . ? O1 Fe3 N11 170.13(16) . . ? O17 Fe3 O21 87.29(14) . . ? O7 Fe3 O21 178.10(12) . . ? O1 Fe3 O21 98.78(12) . . ? N11 Fe3 O21 89.86(16) . . ? O17 Fe3 O19 173.16(13) . . ? O7 Fe3 O19 91.98(13) . . ? O1 Fe3 O19 89.61(11) . . ? N11 Fe3 O19 86.10(15) . . ? O21 Fe3 O19 86.70(15) . . ? O1 Fe4 O11 101.34(10) . . ? O1 Fe4 O10 82.12(11) . . ? O11 Fe4 O10 96.24(11) . . ? O1 Fe4 O20 102.58(12) . . ? O11 Fe4 O20 89.59(12) . . ? O10 Fe4 O20 171.69(12) . . ? O1 Fe4 O22 98.78(11) . . ? O11 Fe4 O22 159.86(11) . . ? O10 Fe4 O22 87.23(12) . . ? O20 Fe4 O22 85.29(13) . . ? O1 Fe4 N2 161.03(12) . . ? O11 Fe4 N2 79.10(11) . . ? O10 Fe4 N2 78.99(11) . . ? O20 Fe4 N2 96.39(12) . . ? O22 Fe4 N2 82.13(12) . . ? O8 Fe5 O11 89.30(11) . . ? O8 Fe5 O2 80.85(10) . . ? O11 Fe5 O2 94.99(10) . . ? O8 Fe5 O25 176.54(12) . . ? O11 Fe5 O25 87.56(12) . . ? O2 Fe5 O25 97.99(11) . . ? O8 Fe5 N21 91.20(13) . . ? O11 Fe5 N21 89.96(12) . . ? O2 Fe5 N21 170.56(13) . . ? O25 Fe5 N21 90.23(13) . . ? O8 Fe5 O23 93.71(12) . . ? O11 Fe5 O23 174.21(11) . . ? O2 Fe5 O23 90.39(10) . . ? O25 Fe5 O23 89.55(12) . . ? N21 Fe5 O23 85.03(12) . . ? O2 Fe6 O13 82.47(11) . . ? O2 Fe6 O14 99.34(11) . . ? O13 Fe6 O14 95.65(11) . . ? O2 Fe6 O24 102.36(12) . . ? O13 Fe6 O24 172.80(13) . . ? O14 Fe6 O24 88.88(12) . . ? O2 Fe6 O26 99.27(11) . . ? O13 Fe6 O26 87.82(12) . . ? O14 Fe6 O26 161.35(11) . . ? O24 Fe6 O26 86.13(13) . . ? O2 Fe6 N3 160.89(13) . . ? O13 Fe6 N3 78.73(13) . . ? O14 Fe6 N3 79.24(12) . . ? O24 Fe6 N3 96.69(13) . . ? O26 Fe6 N3 83.51(12) . . ? O2 Fe6 Fe2 43.79(7) . . ? O13 Fe6 Fe2 40.36(8) . . ? O14 Fe6 Fe2 90.69(8) . . ? O24 Fe6 Fe2 145.48(9) . . ? O26 Fe6 Fe2 103.52(9) . . ? N3 Fe6 Fe2 117.12(10) . . ? O9 Fe7 O3 82.64(11) . . ? O9 Fe7 O14 91.63(11) . . ? O3 Fe7 O14 93.59(11) . . ? O9 Fe7 O29 178.36(11) . . ? O3 Fe7 O29 98.76(11) . . ? O14 Fe7 O29 89.13(12) . . ? O9 Fe7 N31 91.23(13) . . ? O3 Fe7 N31 172.18(14) . . ? O14 Fe7 N31 91.44(13) . . ? O29 Fe7 N31 87.29(13) . . ? O9 Fe7 O27 91.79(12) . . ? O3 Fe7 O27 91.59(11) . . ? O14 Fe7 O27 174.13(11) . . ? O29 Fe7 O27 87.34(12) . . ? N31 Fe7 O27 83.72(13) . . ? O3 Fe8 O17 99.83(12) . . ? O3 Fe8 O16 81.53(11) . . ? O17 Fe8 O16 94.17(12) . . ? O3 Fe8 O28 100.18(12) . . ? O17 Fe8 O28 88.75(13) . . ? O16 Fe8 O28 176.33(13) . . ? O3 Fe8 O30 100.99(11) . . ? O17 Fe8 O30 159.04(12) . . ? O16 Fe8 O30 91.25(12) . . ? O28 Fe8 O30 85.24(13) . . ? O3 Fe8 N4 159.00(13) . . ? O17 Fe8 N4 79.56(14) . . ? O16 Fe8 N4 77.59(13) . . ? O28 Fe8 N4 100.79(14) . . ? O30 Fe8 N4 81.88(13) . . ? Fe4 O1 Fe3 114.64(12) . . ? Fe4 O1 Fe2 96.11(11) . . ? Fe3 O1 Fe2 132.54(13) . . ? Fe4 O1 Fe1 131.59(13) . . ? Fe3 O1 Fe1 97.36(11) . . ? Fe2 O1 Fe1 86.38(9) . . ? Fe6 O2 Fe5 114.37(12) . . ? Fe6 O2 Fe2 95.77(11) . . ? Fe5 O2 Fe2 134.45(12) . . ? Fe6 O2 Fe1 133.19(12) . . ? Fe5 O2 Fe1 96.09(10) . . ? Fe2 O2 Fe1 85.53(9) . . ? Fe8 O3 Fe7 114.54(12) . . ? Fe8 O3 Fe2 96.48(11) . . ? Fe7 O3 Fe2 134.51(13) . . ? Fe8 O3 Fe1 134.21(13) . . ? Fe7 O3 Fe1 95.15(11) . . ? Fe2 O3 Fe1 84.47(9) . . ? C1 N1 C3 114.6(4) . . ? C1 N1 C5 114.5(3) . . ? C3 N1 C5 114.2(4) . . ? C1 N1 Fe1 102.9(3) . . ? C3 N1 Fe1 104.4(2) . . ? C5 N1 Fe1 104.4(3) . . ? N1 C1 C2 108.9(4) . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? O7 C2 C1 107.2(3) . . ? O7 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? O7 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? C2 O7 Fe1 121.9(3) . . ? C2 O7 Fe3 132.0(3) . . ? Fe1 O7 Fe3 105.69(13) . . ? N1 C3 C4 107.5(4) . . ? N1 C3 H3A 110.2 . . ? C4 C3 H3A 110.2 . . ? N1 C3 H3B 110.2 . . ? C4 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? O8 C4 C3 107.7(3) . . ? O8 C4 H4A 110.2 . . ? C3 C4 H4A 110.2 . . ? O8 C4 H4B 110.2 . . ? C3 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? C4 O8 Fe1 122.2(2) . . ? C4 O8 Fe5 131.0(2) . . ? Fe1 O8 Fe5 106.65(13) . . ? N1 C5 C6 107.7(3) . . ? N1 C5 H5A 110.2 . . ? C6 C5 H5A 110.2 . . ? N1 C5 H5B 110.2 . . ? C6 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? O9 C6 C5 107.7(3) . . ? O9 C6 H6A 110.2 . . ? C5 C6 H6A 110.2 . . ? O9 C6 H6B 110.2 . . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? C6 O9 Fe1 122.3(2) . . ? C6 O9 Fe7 131.9(2) . . ? Fe1 O9 Fe7 105.66(12) . . ? C9 N2 C7 112.0(3) . . ? C9 N2 C11 110.4(3) . . ? C7 N2 C11 113.9(3) . . ? C9 N2 Fe4 106.1(2) . . ? C7 N2 Fe4 103.1(2) . . ? C11 N2 Fe4 110.8(2) . . ? N2 C7 C8 110.5(3) . . ? N2 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? N2 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? O10 C8 C7 108.1(3) . . ? O10 C8 H8A 110.1 . . ? C7 C8 H8A 110.1 . . ? O10 C8 H8B 110.1 . . ? C7 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? C8 O10 Fe2 137.3(2) . . ? C8 O10 Fe4 119.8(2) . . ? Fe2 O10 Fe4 99.01(12) . . ? N2 C9 C10 108.9(3) . . ? N2 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? N2 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? O11 C10 C9 108.3(3) . . ? O11 C10 H10A 110.0 . . ? C9 C10 H10A 110.0 . . ? O11 C10 H10B 110.0 . . ? C9 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? C10 O11 Fe4 112.8(2) . . ? C10 O11 Fe5 120.1(2) . . ? Fe4 O11 Fe5 126.72(12) . . ? N2 C11 C12 116.8(4) . . ? N2 C11 H11A 108.1 . . ? C12 C11 H11A 108.1 . . ? N2 C11 H11B 108.1 . . ? C12 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? O12A C12 O12B 120.8(5) . . ? O12A C12 C11 114.3(4) . . ? O12B C12 C11 118.3(5) . . ? O12A C12 H12C 108.7 . . ? O12B C12 H12C 78.4 . . ? C11 C12 H12C 108.7 . . ? O12A C12 H12D 108.7 . . ? O12B C12 H12D 29.2 . . ? C11 C12 H12D 108.7 . . ? H12C C12 H12D 107.6 . . ? O12A C12 H12E 28.1 . . ? O12B C12 H12E 107.7 . . ? C11 C12 H12E 107.7 . . ? H12C C12 H12E 133.7 . . ? H12D C12 H12E 86.4 . . ? O12A C12 H12F 79.2 . . ? O12B C12 H12F 107.7 . . ? C11 C12 H12F 107.7 . . ? H12C C12 H12F 33.9 . . ? H12D C12 H12F 134.7 . . ? H12E C12 H12F 107.1 . . ? C12 O12A H12A 109.5 . . ? C12 O12B H12B 109.5 . . ? C13 N3 C17 113.5(4) . . ? C13 N3 C15 111.7(4) . . ? C17 N3 C15 110.7(3) . . ? C13 N3 Fe6 104.1(2) . . ? C17 N3 Fe6 110.5(3) . . ? C15 N3 Fe6 105.9(3) . . ? N3 C13 C14 110.2(4) . . ? N3 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? N3 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? O13 C14 C13 108.3(4) . . ? O13 C14 H14A 110.0 . . ? C13 C14 H14A 110.0 . . ? O13 C14 H14B 110.0 . . ? C13 C14 H14B 110.0 . . ? H14A C14 H14B 108.4 . . ? C14 O13 Fe2 136.3(3) . . ? C14 O13 Fe6 119.4(3) . . ? Fe2 O13 Fe6 98.26(12) . . ? N3 C15 C16 109.1(4) . . ? N3 C15 H15A 109.9 . . ? C16 C15 H15A 109.9 . . ? N3 C15 H15B 109.9 . . ? C16 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? O14 C16 C15 107.8(3) . . ? O14 C16 H16A 110.1 . . ? C15 C16 H16A 110.1 . . ? O14 C16 H16B 110.1 . . ? C15 C16 H16B 110.1 . . ? H16A C16 H16B 108.5 . . ? C16 O14 Fe7 120.2(2) . . ? C16 O14 Fe6 111.5(2) . . ? Fe7 O14 Fe6 128.25(13) . . ? N3 C17 C18 117.9(4) . . ? N3 C17 H17A 107.8 . . ? C18 C17 H17A 107.8 . . ? N3 C17 H17B 107.8 . . ? C18 C17 H17B 107.8 . . ? H17A C17 H17B 107.2 . . ? O15 C18 C17 107.6(5) . . ? O15 C18 H18A 110.2 . . ? C17 C18 H18A 110.2 . . ? O15 C18 H18B 110.2 . . ? C17 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? C18 O15 H15 109.5 . . ? C19 N4 C21 112.9(4) . . ? C19 N4 C23 104.6(4) . . ? C21 N4 C23 112.4(4) . . ? C19 N4 Fe8 103.7(3) . . ? C21 N4 Fe8 104.7(3) . . ? C23 N4 Fe8 118.5(3) . . ? N4 C19 C20 110.1(4) . . ? N4 C19 H19A 109.6 . . ? C20 C19 H19A 109.6 . . ? N4 C19 H19B 109.6 . . ? C20 C19 H19B 109.6 . . ? H19A C19 H19B 108.2 . . ? O16 C20 C19 106.6(4) . . ? O16 C20 H20A 110.4 . . ? C19 C20 H20A 110.4 . . ? O16 C20 H20B 110.4 . . ? C19 C20 H20B 110.4 . . ? H20A C20 H20B 108.6 . . ? C20 O16 Fe2 133.3(3) . . ? C20 O16 Fe8 120.5(3) . . ? Fe2 O16 Fe8 99.75(12) . . ? C22 C21 N4 111.0(4) . . ? C22 C21 H21A 109.4 . . ? N4 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? N4 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? O17 C22 C21 109.0(4) . . ? O17 C22 H22A 109.9 . . ? C21 C22 H22A 109.9 . . ? O17 C22 H22B 109.9 . . ? C21 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C22 O17 Fe8 111.5(3) . . ? C22 O17 Fe3 120.8(3) . . ? Fe8 O17 Fe3 127.76(14) . . ? C24 C23 N4 116.4(6) . . ? C24 C23 H23A 108.2 . . ? N4 C23 H23A 108.2 . . ? C24 C23 H23B 108.2 . . ? N4 C23 H23B 108.2 . . ? H23A C23 H23B 107.4 . . ? O18 C24 C23 114.3(5) . . ? O18 C24 H24A 108.7 . . ? C23 C24 H24A 108.7 . . ? O18 C24 H24B 108.7 . . ? C23 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? C24 O18 H18 109.5 . . ? C25 O19 Fe3 135.1(3) . . ? C25 O20 Fe4 128.6(3) . . ? O19 C25 O20 124.8(4) . . ? O19 C25 C26 118.7(4) . . ? O20 C25 C26 116.5(4) . . ? C28B C26 C29A 133.9(9) . . ? C28B C26 C27B 116.4(10) . . ? C29A C26 C27B 67.3(7) . . ? C28B C26 C25 110.7(8) . . ? C29A C26 C25 111.5(5) . . ? C27B C26 C25 106.2(7) . . ? C28B C26 C27A 71.6(8) . . ? C29A C26 C27A 109.6(5) . . ? C27B C26 C27A 47.6(7) . . ? C25 C26 C27A 109.7(4) . . ? C28B C26 C28A 37.7(7) . . ? C29A C26 C28A 110.5(6) . . ? C27B C26 C28A 143.9(8) . . ? C25 C26 C28A 107.6(4) . . ? C27A C26 C28A 107.8(5) . . ? C28B C26 C29B 107.7(9) . . ? C29A C26 C29B 39.1(5) . . ? C27B C26 C29B 105.2(8) . . ? C25 C26 C29B 110.3(6) . . ? C27A C26 C29B 136.9(6) . . ? C28A C26 C29B 74.3(6) . . ? C26 C27A H27A 109.5 . . ? C26 C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C26 C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C26 C28A H28A 109.5 . . ? C26 C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C26 C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C26 C29A H29A 109.5 . . ? C26 C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C26 C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C26 C27B H27D 109.5 . . ? C26 C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C26 C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C26 C28B H28D 109.5 . . ? C26 C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C26 C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C26 C29B H29D 109.5 . . ? C26 C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C26 C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C30 O21 Fe3 134.5(3) . . ? C30 O22 Fe4 132.3(3) . . ? O22 C30 O21 124.2(4) . . ? O22 C30 C31 117.5(4) . . ? O21 C30 C31 118.2(4) . . ? C33B C31 C32A 86.3(9) . . ? C33B C31 C34A 121.8(9) . . ? C32A C31 C34A 110.6(9) . . ? C33B C31 C32B 108.7(9) . . ? C32A C31 C32B 22.8(8) . . ? C34A C31 C32B 94.4(8) . . ? C33B C31 C30 108.5(8) . . ? C32A C31 C30 112.5(7) . . ? C34A C31 C30 114.1(6) . . ? C32B C31 C30 107.7(7) . . ? C33B C31 C34B 106.3(9) . . ? C32A C31 C34B 130.9(9) . . ? C34A C31 C34B 23.6(7) . . ? C32B C31 C34B 117.5(9) . . ? C30 C31 C34B 107.9(6) . . ? C33B C31 C33A 18.8(8) . . ? C32A C31 C33A 105.0(8) . . ? C34A C31 C33A 115.6(7) . . ? C32B C31 C33A 127.5(8) . . ? C30 C31 C33A 98.4(6) . . ? C34B C31 C33A 95.4(7) . . ? C31 C32A H32A 109.5 . . ? C31 C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C31 C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C31 C33A H33A 109.5 . . ? C31 C33A H33B 109.5 . . ? H33A C33A H33B 109.5 . . ? C31 C33A H33C 109.5 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? C31 C34A H34A 109.5 . . ? C31 C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? C31 C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? C31 C32B H32D 109.5 . . ? C31 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C31 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C31 C33B H33D 109.5 . . ? C31 C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? C31 C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? C31 C34B H34D 109.5 . . ? C31 C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C31 C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C35 O23 Fe5 135.9(3) . . ? C35 O24 Fe6 128.8(3) . . ? O23 C35 O24 124.1(4) . . ? O23 C35 C36 118.4(4) . . ? O24 C35 C36 117.5(4) . . ? C39 C36 C38 112.8(5) . . ? C39 C36 C35 111.0(4) . . ? C38 C36 C35 106.7(4) . . ? C39 C36 C37 108.8(5) . . ? C38 C36 C37 107.6(4) . . ? C35 C36 C37 109.8(4) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C40 O25 Fe5 135.4(3) . . ? C40 O26 Fe6 130.8(3) . . ? O25 C40 O26 124.5(4) . . ? O25 C40 C41 118.4(3) . . ? O26 C40 C41 117.0(4) . . ? C44 C41 C43 108.7(4) . . ? C44 C41 C42 110.5(5) . . ? C43 C41 C42 109.4(5) . . ? C44 C41 C40 106.8(4) . . ? C43 C41 C40 111.5(4) . . ? C42 C41 C40 109.9(4) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C45 O27 Fe7 131.9(3) . . ? C45 O28 Fe8 130.9(3) . . ? O27 C45 O28 124.5(4) . . ? O27 C45 C46 118.5(4) . . ? O28 C45 C46 117.0(4) . . ? C48A C46 C47B 75.2(7) . . ? C48A C46 C49A 113.2(5) . . ? C47B C46 C49A 131.5(7) . . ? C48A C46 C49B 128.0(7) . . ? C47B C46 C49B 111.2(8) . . ? C49A C46 C49B 25.1(5) . . ? C48A C46 C45 111.5(4) . . ? C47B C46 C45 114.7(6) . . ? C49A C46 C45 106.1(4) . . ? C49B C46 C45 111.3(6) . . ? C48A C46 C47A 109.6(5) . . ? C47B C46 C47A 34.9(6) . . ? C49A C46 C47A 109.7(5) . . ? C49B C46 C47A 84.9(6) . . ? C45 C46 C47A 106.5(4) . . ? C48A C46 C48B 30.5(5) . . ? C47B C46 C48B 103.2(8) . . ? C49A C46 C48B 85.5(6) . . ? C49B C46 C48B 105.9(7) . . ? C45 C46 C48B 109.9(6) . . ? C47A C46 C48B 134.4(7) . . ? C46 C47A H47A 109.5 . . ? C46 C47A H47B 109.5 . . ? H47A C47A H47B 109.5 . . ? C46 C47A H47C 109.5 . . ? H47A C47A H47C 109.5 . . ? H47B C47A H47C 109.5 . . ? C46 C48A H48A 109.5 . . ? C46 C48A H48B 109.5 . . ? H48A C48A H48B 109.5 . . ? C46 C48A H48C 109.5 . . ? H48A C48A H48C 109.5 . . ? H48B C48A H48C 109.5 . . ? C46 C49A H49A 109.5 . . ? C46 C49A H49B 109.5 . . ? H49A C49A H49B 109.5 . . ? C46 C49A H49C 109.5 . . ? H49A C49A H49C 109.5 . . ? H49B C49A H49C 109.5 . . ? C46 C47B H47D 109.5 . . ? C46 C47B H47E 109.5 . . ? H47D C47B H47E 109.5 . . ? C46 C47B H47F 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? C46 C48B H48D 109.5 . . ? C46 C48B H48E 109.5 . . ? H48D C48B H48E 109.5 . . ? C46 C48B H48F 109.5 . . ? H48D C48B H48F 109.5 . . ? H48E C48B H48F 109.5 . . ? C46 C49B H49D 109.5 . . ? C46 C49B H49E 109.5 . . ? H49D C49B H49E 109.5 . . ? C46 C49B H49F 109.5 . . ? H49D C49B H49F 109.5 . . ? H49E C49B H49F 109.5 . . ? C50 O29 Fe7 137.1(3) . . ? C50 O30 Fe8 127.9(3) . . ? O29 C50 O30 124.2(4) . . ? O29 C50 C51 116.4(4) . . ? O30 C50 C51 119.3(4) . . ? C52B C51 C54A 82.8(7) . . ? C52B C51 C53A 116.3(8) . . ? C54A C51 C53A 120.2(8) . . ? C52B C51 C50 116.7(5) . . ? C54A C51 C50 106.6(7) . . ? C53A C51 C50 111.4(7) . . ? C52B C51 C53B 111.0(8) . . ? C54A C51 C53B 129.7(9) . . ? C53A C51 C53B 10.3(10) . . ? C50 C51 C53B 108.7(6) . . ? C52B C51 C54B 108.3(5) . . ? C54A C51 C54B 28.3(6) . . ? C53A C51 C54B 96.8(7) . . ? C50 C51 C54B 104.5(4) . . ? C53B C51 C54B 107.1(7) . . ? C52B C51 C52A 23.5(5) . . ? C54A C51 C52A 105.4(8) . . ? C53A C51 C52A 108.4(8) . . ? C50 C51 C52A 103.5(6) . . ? C53B C51 C52A 100.0(8) . . ? C54B C51 C52A 131.7(6) . . ? C51 C52A H52A 109.5 . . ? C51 C52A H52B 109.5 . . ? H52A C52A H52B 109.5 . . ? C51 C52A H52C 109.5 . . ? H52A C52A H52C 109.5 . . ? H52B C52A H52C 109.5 . . ? C51 C53A H53A 109.5 . . ? C51 C53A H53B 109.5 . . ? H53A C53A H53B 109.5 . . ? C51 C53A H53C 109.5 . . ? H53A C53A H53C 109.5 . . ? H53B C53A H53C 109.5 . . ? C51 C54A H54A 109.5 . . ? C51 C54A H54B 109.5 . . ? H54A C54A H54B 109.5 . . ? C51 C54A H54C 109.5 . . ? H54A C54A H54C 109.5 . . ? H54B C54A H54C 109.5 . . ? C51 C52B H52D 109.5 . . ? C51 C52B H52E 109.5 . . ? H52D C52B H52E 109.5 . . ? C51 C52B H52F 109.5 . . ? H52D C52B H52F 109.5 . . ? H52E C52B H52F 109.5 . . ? C51 C53B H53D 109.5 . . ? C51 C53B H53E 109.5 . . ? H53D C53B H53E 109.5 . . ? C51 C53B H53F 109.5 . . ? H53D C53B H53F 109.5 . . ? H53E C53B H53F 109.5 . . ? C51 C54B H54D 109.5 . . ? C51 C54B H54E 109.5 . . ? H54D C54B H54E 109.5 . . ? C51 C54B H54F 109.5 . . ? H54D C54B H54F 109.5 . . ? H54E C54B H54F 109.5 . . ? N12 N11 Fe3 124.7(4) . . ? N11 N12 N13A 167.1(8) . . ? N11 N12 N13B 150.2(11) . . ? N13A N12 N13B 42.1(8) . . ? N22 N21 Fe5 126.3(3) . . ? N23 N22 N21 177.7(5) . . ? N32 N31 Fe7 122.9(3) . . ? N33B N32 N31 164.6(7) . . ? N33B N32 N33A 30.3(5) . . ? N31 N32 N33A 164.9(6) . . ? O32 Fe9 O31 108.71(12) . . ? O32 Fe9 O33 112.02(12) . . ? O31 Fe9 O33 114.97(11) . . ? O32 Fe9 O6 150.32(11) . . ? O31 Fe9 O6 91.45(10) . . ? O33 Fe9 O6 76.41(11) . . ? O32 Fe9 O5 76.16(10) . . ? O31 Fe9 O5 148.29(11) . . ? O33 Fe9 O5 90.23(11) . . ? O6 Fe9 O5 75.40(9) . . ? O32 Fe9 O4 88.64(11) . . ? O31 Fe9 O4 74.58(10) . . ? O33 Fe9 O4 150.70(11) . . ? O6 Fe9 O4 75.68(9) . . ? O5 Fe9 O4 74.24(9) . . ? O32 Fe9 N5 73.44(12) . . ? O31 Fe9 N5 72.67(12) . . ? O33 Fe9 N5 73.20(13) . . ? O6 Fe9 N5 134.91(12) . . ? O5 Fe9 N5 136.20(11) . . ? O4 Fe9 N5 134.69(11) . . ? O32 Fe9 Fe10 106.52(9) . . ? O31 Fe9 Fe10 106.20(9) . . ? O33 Fe9 Fe10 107.92(9) . . ? O6 Fe9 Fe10 45.37(7) . . ? O5 Fe9 Fe10 44.73(7) . . ? O4 Fe9 Fe10 44.10(6) . . ? N5 Fe9 Fe10 178.72(9) . . ? O37 Fe10 O40 96.33(11) . . ? O37 Fe10 O34 94.85(11) . . ? O40 Fe10 O34 95.58(11) . . ? O37 Fe10 O4 161.28(11) . . ? O40 Fe10 O4 102.03(10) . . ? O34 Fe10 O4 79.88(10) . . ? O37 Fe10 O5 80.53(11) . . ? O40 Fe10 O5 159.75(11) . . ? O34 Fe10 O5 104.60(11) . . ? O4 Fe10 O5 83.43(10) . . ? O37 Fe10 O6 103.38(11) . . ? O40 Fe10 O6 79.52(11) . . ? O34 Fe10 O6 161.51(10) . . ? O4 Fe10 O6 83.70(10) . . ? O5 Fe10 O6 81.76(10) . . ? O37 Fe10 Fe9 121.44(9) . . ? O40 Fe10 Fe9 119.29(8) . . ? O34 Fe10 Fe9 122.88(8) . . ? O4 Fe10 Fe9 51.20(7) . . ? O5 Fe10 Fe9 49.79(7) . . ? O6 Fe10 Fe9 48.68(7) . . ? O37 Fe10 Fe12 127.65(8) . . ? O40 Fe10 Fe12 111.57(8) . . ? O34 Fe10 Fe12 41.22(7) . . ? O4 Fe10 Fe12 40.76(7) . . ? O5 Fe10 Fe12 85.42(7) . . ? O6 Fe10 Fe12 124.12(7) . . ? Fe9 Fe10 Fe12 82.58(2) . . ? O37 Fe10 Fe14 41.35(8) . . ? O40 Fe10 Fe14 129.89(8) . . ? O34 Fe10 Fe14 110.33(8) . . ? O4 Fe10 Fe14 123.76(7) . . ? O5 Fe10 Fe14 40.36(7) . . ? O6 Fe10 Fe14 85.90(7) . . ? Fe9 Fe10 Fe14 81.71(2) . . ? Fe12 Fe10 Fe14 116.22(2) . . ? O4 Fe11 O31 81.84(10) . . ? O4 Fe11 O41 94.36(10) . . ? O31 Fe11 O41 89.60(12) . . ? O4 Fe11 O45 99.44(11) . . ? O31 Fe11 O45 178.10(12) . . ? O41 Fe11 O45 88.91(12) . . ? O4 Fe11 N41 170.03(13) . . ? O31 Fe11 N41 90.81(12) . . ? O41 Fe11 N41 92.31(12) . . ? O45 Fe11 N41 88.07(12) . . ? O4 Fe11 O43 90.15(10) . . ? O31 Fe11 O43 93.62(12) . . ? O41 Fe11 O43 174.79(11) . . ? O45 Fe11 O43 87.78(13) . . ? N41 Fe11 O43 83.56(12) . . ? O4 Fe12 O44 102.66(11) . . ? O4 Fe12 O34 82.09(10) . . ? O44 Fe12 O34 172.50(13) . . ? O4 Fe12 O35 99.64(11) . . ? O44 Fe12 O35 88.29(13) . . ? O34 Fe12 O35 96.68(11) . . ? O4 Fe12 O46 99.12(11) . . ? O44 Fe12 O46 85.40(13) . . ? O34 Fe12 O46 88.13(11) . . ? O35 Fe12 O46 161.10(11) . . ? O4 Fe12 N6 160.84(11) . . ? O44 Fe12 N6 96.47(12) . . ? O34 Fe12 N6 79.00(11) . . ? O35 Fe12 N6 79.68(12) . . ? O46 Fe12 N6 83.35(12) . . ? O4 Fe12 Fe10 43.24(7) . . ? O44 Fe12 Fe10 144.97(9) . . ? O34 Fe12 Fe10 41.02(7) . . ? O35 Fe12 Fe10 90.32(8) . . ? O46 Fe12 Fe10 104.99(8) . . ? N6 Fe12 Fe10 117.69(9) . . ? O32 Fe13 O35 92.04(12) . . ? O32 Fe13 O5 81.14(11) . . ? O35 Fe13 O5 92.60(11) . . ? O32 Fe13 N51 92.61(14) . . ? O35 Fe13 N51 92.59(15) . . ? O5 Fe13 N51 172.01(15) . . ? O32 Fe13 O49 178.97(13) . . ? O35 Fe13 O49 88.94(12) . . ? O5 Fe13 O49 99.16(11) . . ? N51 Fe13 O49 87.00(15) . . ? O32 Fe13 O47 91.57(12) . . ? O35 Fe13 O47 176.35(11) . . ? O5 Fe13 O47 88.52(12) . . ? N51 Fe13 O47 86.68(16) . . ? O49 Fe13 O47 87.46(12) . . ? O5 Fe14 O48 101.64(12) . . ? O5 Fe14 O37 82.62(11) . . ? O48 Fe14 O37 172.98(12) . . ? O5 Fe14 O38 98.54(11) . . ? O48 Fe14 O38 89.96(12) . . ? O37 Fe14 O38 94.95(11) . . ? O5 Fe14 O50 99.57(11) . . ? O48 Fe14 O50 86.91(12) . . ? O37 Fe14 O50 86.88(11) . . ? O38 Fe14 O50 161.88(11) . . ? O5 Fe14 N7 161.02(13) . . ? O48 Fe14 N7 97.29(14) . . ? O37 Fe14 N7 78.68(12) . . ? O38 Fe14 N7 79.95(12) . . ? O50 Fe14 N7 82.75(12) . . ? O5 Fe14 Fe10 43.57(8) . . ? O48 Fe14 Fe10 144.87(10) . . ? O37 Fe14 Fe10 40.27(7) . . ? O38 Fe14 Fe10 91.06(8) . . ? O50 Fe14 Fe10 101.73(8) . . ? N7 Fe14 Fe10 117.45(10) . . ? O33 Fe15 O38 92.24(11) . . ? O33 Fe15 O6 80.78(11) . . ? O38 Fe15 O6 95.20(11) . . ? O33 Fe15 O53 177.65(13) . . ? O38 Fe15 O53 88.44(14) . . ? O6 Fe15 O53 96.92(13) . . ? O33 Fe15 N61B 100.2(3) . . ? O38 Fe15 N61B 86.1(2) . . ? O6 Fe15 N61B 178.4(2) . . ? O53 Fe15 N61B 82.1(3) . . ? O33 Fe15 N61A 86.1(2) . . ? O38 Fe15 N61A 92.7(2) . . ? O6 Fe15 N61A 165.0(2) . . ? O53 Fe15 N61A 96.1(2) . . ? N61B Fe15 N61A 15.3(3) . . ? O33 Fe15 O51 92.08(14) . . ? O38 Fe15 O51 173.34(13) . . ? O6 Fe15 O51 90.49(11) . . ? O53 Fe15 O51 87.44(16) . . ? N61B Fe15 O51 88.1(2) . . ? N61A Fe15 O51 82.6(2) . . ? O6 Fe16 O41 100.64(11) . . ? O6 Fe16 O40 82.09(11) . . ? O41 Fe16 O40 93.95(11) . . ? O6 Fe16 O52 99.84(12) . . ? O41 Fe16 O52 89.46(12) . . ? O40 Fe16 O52 175.72(12) . . ? O6 Fe16 O54 101.22(12) . . ? O41 Fe16 O54 158.12(12) . . ? O40 Fe16 O54 89.96(12) . . ? O52 Fe16 O54 85.93(13) . . ? O6 Fe16 N8 160.64(12) . . ? O41 Fe16 N8 77.94(12) . . ? O40 Fe16 N8 78.76(12) . . ? O52 Fe16 N8 99.46(12) . . ? O54 Fe16 N8 81.74(13) . . ? Fe12 O4 Fe11 114.72(12) . . ? Fe12 O4 Fe10 96.00(10) . . ? Fe11 O4 Fe10 134.73(13) . . ? Fe12 O4 Fe9 133.00(12) . . ? Fe11 O4 Fe9 95.96(10) . . ? Fe10 O4 Fe9 84.70(9) . . ? Fe14 O5 Fe13 113.62(12) . . ? Fe14 O5 Fe10 96.07(12) . . ? Fe13 O5 Fe10 134.38(14) . . ? Fe14 O5 Fe9 134.87(13) . . ? Fe13 O5 Fe9 95.59(11) . . ? Fe10 O5 Fe9 85.48(9) . . ? Fe16 O6 Fe15 115.24(12) . . ? Fe16 O6 Fe10 95.84(11) . . ? Fe15 O6 Fe10 132.46(12) . . ? Fe16 O6 Fe9 132.21(12) . . ? Fe15 O6 Fe9 96.81(11) . . ? Fe10 O6 Fe9 85.95(9) . . ? C57B N5 C59A 138.5(9) . . ? C57B N5 C59B 117.2(10) . . ? C59A N5 C59B 30.3(6) . . ? C57B N5 C55A 82.7(8) . . ? C59A N5 C55A 113.1(5) . . ? C59B N5 C55A 141.1(7) . . ? C57B N5 C57A 30.4(7) . . ? C59A N5 C57A 112.9(5) . . ? C59B N5 C57A 87.4(7) . . ? C55A N5 C57A 110.6(5) . . ? C57B N5 C55B 123.1(9) . . ? C59A N5 C55B 79.1(6) . . ? C59B N5 C55B 109.3(8) . . ? C55A N5 C55B 40.5(5) . . ? C57A N5 C55B 148.0(7) . . ? C57B N5 Fe9 103.0(8) . . ? C59A N5 Fe9 108.0(4) . . ? C59B N5 Fe9 100.9(6) . . ? C55A N5 Fe9 106.7(3) . . ? C57A N5 Fe9 105.0(3) . . ? C55B N5 Fe9 98.5(6) . . ? C56 C55A N5 108.3(5) . . ? C56 C55A H55A 110.0 . . ? N5 C55A H55A 110.0 . . ? C56 C55A H55B 110.0 . . ? N5 C55A H55B 110.0 . . ? H55A C55A H55B 108.4 . . ? C56 C55B N5 109.0(9) . . ? C56 C55B H55C 109.9 . . ? N5 C55B H55C 109.9 . . ? C56 C55B H55D 109.9 . . ? N5 C55B H55D 109.9 . . ? H55C C55B H55D 108.3 . . ? O31 C56 C55B 115.0(6) . . ? O31 C56 C55A 108.7(4) . . ? C55B C56 C55A 42.3(6) . . ? O31 C56 H56A 109.9 . . ? C55B C56 H56A 132.9 . . ? C55A C56 H56A 109.9 . . ? O31 C56 H56B 109.9 . . ? C55B C56 H56B 68.7 . . ? C55A C56 H56B 109.9 . . ? H56A C56 H56B 108.3 . . ? O31 C56 H56C 108.5 . . ? C55B C56 H56C 108.5 . . ? C55A C56 H56C 71.8 . . ? H56A C56 H56C 41.4 . . ? H56B C56 H56C 138.1 . . ? O31 C56 H56D 108.5 . . ? C55B C56 H56D 108.5 . . ? C55A C56 H56D 140.7 . . ? H56A C56 H56D 68.0 . . ? H56B C56 H56D 43.9 . . ? H56C C56 H56D 107.5 . . ? C56 O31 Fe9 122.3(2) . . ? C56 O31 Fe11 129.8(2) . . ? Fe9 O31 Fe11 107.63(12) . . ? C58 C57A N5 109.3(5) . . ? C58 C57A H57A 109.8 . . ? N5 C57A H57A 109.8 . . ? C58 C57A H57B 109.8 . . ? N5 C57A H57B 109.8 . . ? H57A C57A H57B 108.3 . . ? N5 C57B C58 120.0(11) . . ? N5 C57B H57C 107.3 . . ? C58 C57B H57C 107.3 . . ? N5 C57B H57D 107.3 . . ? C58 C57B H57D 107.3 . . ? H57C C57B H57D 106.9 . . ? C57A C58 O32 110.9(5) . . ? C57A C58 C57B 31.2(6) . . ? O32 C58 C57B 111.2(7) . . ? C57A C58 H58A 109.5 . . ? O32 C58 H58A 109.5 . . ? C57B C58 H58A 80.7 . . ? C57A C58 H58B 109.5 . . ? O32 C58 H58B 109.5 . . ? C57B C58 H58B 132.2 . . ? H58A C58 H58B 108.0 . . ? C57A C58 H58C 80.9 . . ? O32 C58 H58C 109.4 . . ? C57B C58 H58C 109.4 . . ? H58A C58 H58C 132.3 . . ? H58B C58 H58C 31.5 . . ? C57A C58 H58D 132.6 . . ? O32 C58 H58D 109.4 . . ? C57B C58 H58D 109.4 . . ? H58A C58 H58D 31.6 . . ? H58B C58 H58D 78.9 . . ? H58C C58 H58D 108.0 . . ? C58 O32 Fe9 122.3(3) . . ? C58 O32 Fe13 129.4(3) . . ? Fe9 O32 Fe13 107.00(13) . . ? N5 C59A C60 109.3(5) . . ? N5 C59A H59A 109.8 . . ? C60 C59A H59A 109.8 . . ? N5 C59A H59B 109.8 . . ? C60 C59A H59B 109.8 . . ? H59A C59A H59B 108.3 . . ? C60 C59B N5 117.1(11) . . ? C60 C59B H59C 108.0 . . ? N5 C59B H59C 108.0 . . ? C60 C59B H59D 108.0 . . ? N5 C59B H59D 108.0 . . ? H59C C59B H59D 107.3 . . ? C59B C60 O33 116.6(7) . . ? C59B C60 C59A 30.3(6) . . ? O33 C60 C59A 110.8(4) . . ? C59B C60 H60A 127.2 . . ? O33 C60 H60A 109.5 . . ? C59A C60 H60A 109.5 . . ? C59B C60 H60B 79.9 . . ? O33 C60 H60B 109.5 . . ? C59A C60 H60B 109.5 . . ? H60A C60 H60B 108.1 . . ? C59B C60 H60C 108.1 . . ? O33 C60 H60C 108.1 . . ? C59A C60 H60C 133.8 . . ? H60A C60 H60C 79.1 . . ? H60B C60 H60C 32.0 . . ? C59B C60 H60D 108.1 . . ? O33 C60 H60D 108.1 . . ? C59A C60 H60D 83.1 . . ? H60A C60 H60D 29.7 . . ? H60B C60 H60D 132.0 . . ? H60C C60 H60D 107.3 . . ? C60 O33 Fe9 122.3(3) . . ? C60 O33 Fe15 130.5(3) . . ? Fe9 O33 Fe15 105.99(13) . . ? C63 N6 C61 111.8(3) . . ? C63 N6 C65 112.3(3) . . ? C61 N6 C65 112.3(3) . . ? C63 N6 Fe12 105.8(2) . . ? C61 N6 Fe12 104.1(2) . . ? C65 N6 Fe12 109.9(2) . . ? N6 C61 C62 110.0(3) . . ? N6 C61 H61A 109.7 . . ? C62 C61 H61A 109.7 . . ? N6 C61 H61B 109.7 . . ? C62 C61 H61B 109.7 . . ? H61A C61 H61B 108.2 . . ? O34 C62 C61 108.1(3) . . ? O34 C62 H62A 110.1 . . ? C61 C62 H62A 110.1 . . ? O34 C62 H62B 110.1 . . ? C61 C62 H62B 110.1 . . ? H62A C62 H62B 108.4 . . ? C62 O34 Fe10 136.8(2) . . ? C62 O34 Fe12 120.4(2) . . ? Fe10 O34 Fe12 97.76(11) . . ? N6 C63 C64 108.9(3) . . ? N6 C63 H63A 109.9 . . ? C64 C63 H63A 109.9 . . ? N6 C63 H63B 109.9 . . ? C64 C63 H63B 109.9 . . ? H63A C63 H63B 108.3 . . ? O35 C64 C63 107.1(3) . . ? O35 C64 H64A 110.3 . . ? C63 C64 H64A 110.3 . . ? O35 C64 H64B 110.3 . . ? C63 C64 H64B 110.3 . . ? H64A C64 H64B 108.6 . . ? C64 O35 Fe13 119.4(2) . . ? C64 O35 Fe12 111.7(2) . . ? Fe13 O35 Fe12 128.88(13) . . ? N6 C65 C66 117.2(4) . . ? N6 C65 H65A 108.0 . . ? C66 C65 H65A 108.0 . . ? N6 C65 H65B 108.0 . . ? C66 C65 H65B 108.0 . . ? H65A C65 H65B 107.2 . . ? O36A C66 O36B 47.8(9) . . ? O36A C66 C65 111.6(5) . . ? O36B C66 C65 125.0(10) . . ? O36A C66 H66A 109.3 . . ? O36B C66 H66A 125.4 . . ? C65 C66 H66A 109.3 . . ? O36A C66 H66B 109.3 . . ? O36B C66 H66B 61.6 . . ? C65 C66 H66B 109.3 . . ? H66A C66 H66B 108.0 . . ? O36A C66 H66C 66.7 . . ? O36B C66 H66C 106.1 . . ? C65 C66 H66C 106.1 . . ? H66A C66 H66C 47.8 . . ? H66B C66 H66C 142.8 . . ? O36A C66 H66D 142.2 . . ? O36B C66 H66D 106.1 . . ? C65 C66 H66D 106.1 . . ? H66A C66 H66D 59.4 . . ? H66B C66 H66D 52.6 . . ? H66C C66 H66D 106.3 . . ? C66 O36A H36A 109.5 . . ? C67 N7 C69 112.1(4) . . ? C67 N7 C71 112.4(4) . . ? C69 N7 C71 111.8(4) . . ? C67 N7 Fe14 104.3(2) . . ? C69 N7 Fe14 105.8(3) . . ? C71 N7 Fe14 110.0(3) . . ? N7 C67 C68 109.8(4) . . ? N7 C67 H67A 109.7 . . ? C68 C67 H67A 109.7 . . ? N7 C67 H67B 109.7 . . ? C68 C67 H67B 109.7 . . ? H67A C67 H67B 108.2 . . ? O37 C68 C67 107.6(4) . . ? O37 C68 H68A 110.2 . . ? C67 C68 H68A 110.2 . . ? O37 C68 H68B 110.2 . . ? C67 C68 H68B 110.2 . . ? H68A C68 H68B 108.5 . . ? C68 O37 Fe10 136.8(2) . . ? C68 O37 Fe14 119.7(2) . . ? Fe10 O37 Fe14 98.37(12) . . ? N7 C69 C70 109.9(4) . . ? N7 C69 H69A 109.7 . . ? C70 C69 H69A 109.7 . . ? N7 C69 H69B 109.7 . . ? C70 C69 H69B 109.7 . . ? H69A C69 H69B 108.2 . . ? O38 C70 C69 109.0(4) . . ? O38 C70 H70A 109.9 . . ? C69 C70 H70A 109.9 . . ? O38 C70 H70B 109.9 . . ? C69 C70 H70B 109.9 . . ? H70A C70 H70B 108.3 . . ? C70 O38 Fe15 121.1(2) . . ? C70 O38 Fe14 110.7(2) . . ? Fe15 O38 Fe14 128.05(13) . . ? C72 C71 N7 119.3(5) . . ? C72 C71 H71A 107.5 . . ? N7 C71 H71A 107.5 . . ? C72 C71 H71B 107.5 . . ? N7 C71 H71B 107.5 . . ? H71A C71 H71B 107.0 . . ? O39A C72 C71 115.2(5) . . ? O39A C72 O39B 75.6(6) . . ? C71 C72 O39B 125.4(6) . . ? O39A C72 H72A 108.5 . . ? C71 C72 H72A 108.5 . . ? O39B C72 H72A 118.3 . . ? O39A C72 H72B 108.5 . . ? C71 C72 H72B 108.5 . . ? O39B C72 H72B 32.9 . . ? H72A C72 H72B 107.5 . . ? O39A C72 H72C 127.4 . . ? C71 C72 H72C 106.0 . . ? O39B C72 H72C 106.0 . . ? H72A C72 H72C 23.7 . . ? H72B C72 H72C 86.6 . . ? O39A C72 H72D 32.9 . . ? C71 C72 H72D 106.0 . . ? O39B C72 H72D 106.0 . . ? H72A C72 H72D 83.1 . . ? H72B C72 H72D 138.0 . . ? H72C C72 H72D 106.3 . . ? C72 O39A H39D 109.5 . . ? C75 N8 C73 110.2(4) . . ? C75 N8 C77 110.7(3) . . ? C73 N8 C77 105.8(4) . . ? C75 N8 Fe16 105.8(3) . . ? C73 N8 Fe16 102.5(2) . . ? C77 N8 Fe16 121.3(3) . . ? N8 C73 C74 111.0(4) . . ? N8 C73 H73A 109.4 . . ? C74 C73 H73A 109.4 . . ? N8 C73 H73B 109.4 . . ? C74 C73 H73B 109.4 . . ? H73A C73 H73B 108.0 . . ? O40 C74 C73 106.2(3) . . ? O40 C74 H74A 110.5 . . ? C73 C74 H74A 110.5 . . ? O40 C74 H74B 110.5 . . ? C73 C74 H74B 110.5 . . ? H74A C74 H74B 108.7 . . ? C74 O40 Fe10 130.3(2) . . ? C74 O40 Fe16 118.0(2) . . ? Fe10 O40 Fe16 99.33(12) . . ? N8 C75 C76 110.1(4) . . ? N8 C75 H75A 109.6 . . ? C76 C75 H75A 109.6 . . ? N8 C75 H75B 109.6 . . ? C76 C75 H75B 109.6 . . ? H75A C75 H75B 108.2 . . ? O41 C76 C75 107.8(3) . . ? O41 C76 H76A 110.1 . . ? C75 C76 H76A 110.1 . . ? O41 C76 H76B 110.1 . . ? C75 C76 H76B 110.1 . . ? H76A C76 H76B 108.5 . . ? C76 O41 Fe16 112.3(2) . . ? C76 O41 Fe11 119.8(2) . . ? Fe16 O41 Fe11 127.86(13) . . ? C78 C77 N8 114.3(4) . . ? C78 C77 H77A 108.7 . . ? N8 C77 H77A 108.7 . . ? C78 C77 H77B 108.7 . . ? N8 C77 H77B 108.7 . . ? H77A C77 H77B 107.6 . . ? O42 C78 C77 107.0(5) . . ? O42 C78 H78A 110.3 . . ? C77 C78 H78A 110.3 . . ? O42 C78 H78B 110.3 . . ? C77 C78 H78B 110.3 . . ? H78A C78 H78B 108.6 . . ? C78 O42 H42 109.5 . . ? C79 O43 Fe11 135.3(3) . . ? C79 O44 Fe12 129.3(3) . . ? O44 C79 O43 123.9(4) . . ? O44 C79 C80 116.5(4) . . ? O43 C79 C80 119.5(4) . . ? C83 C80 C79 111.4(3) . . ? C83 C80 C82 111.1(4) . . ? C79 C80 C82 109.2(3) . . ? C83 C80 C81 110.0(4) . . ? C79 C80 C81 106.2(4) . . ? C82 C80 C81 108.7(4) . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C80 C82 H82A 109.5 . . ? C80 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C80 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C80 C83 H83A 109.5 . . ? C80 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C80 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C84 O45 Fe11 134.5(3) . . ? C84 O46 Fe12 131.2(3) . . ? O46 C84 O45 124.1(4) . . ? O46 C84 C85 117.7(4) . . ? O45 C84 C85 118.2(4) . . ? C88 C85 C86 111.6(5) . . ? C88 C85 C84 111.4(4) . . ? C86 C85 C84 110.8(4) . . ? C88 C85 C87 108.9(5) . . ? C86 C85 C87 108.1(4) . . ? C84 C85 C87 105.9(4) . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C85 C87 H87A 109.5 . . ? C85 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C85 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C85 C88 H88A 109.5 . . ? C85 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C85 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C89 O47 Fe13 131.9(3) . . ? C89 O48 Fe14 128.6(3) . . ? O47 C89 O48 124.0(4) . . ? O47 C89 C90 118.9(5) . . ? O48 C89 C90 117.1(5) . . ? C93A C90 C91B 85.0(7) . . ? C93A C90 C92B 128.1(7) . . ? C91B C90 C92B 107.0(8) . . ? C93A C90 C89 114.2(6) . . ? C91B C90 C89 111.2(7) . . ? C92B C90 C89 108.0(6) . . ? C93A C90 C92A 116.1(7) . . ? C91B C90 C92A 125.7(8) . . ? C92B C90 C92A 20.5(6) . . ? C89 C90 C92A 104.4(5) . . ? C93A C90 C93B 24.4(5) . . ? C91B C90 C93B 108.5(8) . . ? C92B C90 C93B 112.7(7) . . ? C89 C90 C93B 109.5(6) . . ? C92A C90 C93B 96.1(7) . . ? C93A C90 C91A 107.5(7) . . ? C91B C90 C91A 23.4(6) . . ? C92B C90 C91A 87.8(7) . . ? C89 C90 C91A 106.1(6) . . ? C92A C90 C91A 108.0(7) . . ? C93B C90 C91A 129.9(7) . . ? C90 C91A H91A 109.5 . . ? C90 C91A H91B 109.5 . . ? H91A C91A H91B 109.5 . . ? C90 C91A H91C 109.5 . . ? H91A C91A H91C 109.5 . . ? H91B C91A H91C 109.5 . . ? C90 C92A H92A 109.5 . . ? C90 C92A H92B 109.5 . . ? H92A C92A H92B 109.5 . . ? C90 C92A H92C 109.5 . . ? H92A C92A H92C 109.5 . . ? H92B C92A H92C 109.5 . . ? C90 C93A H93A 109.5 . . ? C90 C93A H93B 109.5 . . ? H93A C93A H93B 109.5 . . ? C90 C93A H93C 109.5 . . ? H93A C93A H93C 109.5 . . ? H93B C93A H93C 109.5 . . ? C90 C91B H91D 109.5 . . ? C90 C91B H91E 109.5 . . ? H91D C91B H91E 109.5 . . ? C90 C91B H91F 109.5 . . ? H91D C91B H91F 109.5 . . ? H91E C91B H91F 109.5 . . ? C90 C92B H92D 109.5 . . ? C90 C92B H92E 109.5 . . ? H92D C92B H92E 109.5 . . ? C90 C92B H92F 109.5 . . ? H92D C92B H92F 109.5 . . ? H92E C92B H92F 109.5 . . ? C90 C93B H93D 109.5 . . ? C90 C93B H93E 109.5 . . ? H93D C93B H93E 109.5 . . ? C90 C93B H93F 109.5 . . ? H93D C93B H93F 109.5 . . ? H93E C93B H93F 109.5 . . ? C94 O49 Fe13 135.6(3) . . ? C94 O50 Fe14 125.5(3) . . ? O49 C94 O50 125.2(4) . . ? O49 C94 C95 117.4(4) . . ? O50 C94 C95 117.3(4) . . ? C97B C95 C96A 127.2(8) . . ? C97B C95 C98A 64.6(7) . . ? C96A C95 C98A 114.6(7) . . ? C97B C95 C94 116.6(6) . . ? C96A C95 C94 112.5(5) . . ? C98A C95 C94 110.1(6) . . ? C97B C95 C96B 114.3(8) . . ? C96A C95 C96B 23.8(6) . . ? C98A C95 C96B 131.3(7) . . ? C94 C95 C96B 111.9(5) . . ? C97B C95 C97A 38.4(6) . . ? C96A C95 C97A 109.5(6) . . ? C98A C95 C97A 102.9(6) . . ? C94 C95 C97A 106.5(5) . . ? C96B C95 C97A 87.7(6) . . ? C97B C95 C98B 108.4(8) . . ? C96A C95 C98B 79.1(7) . . ? C98A C95 C98B 45.5(6) . . ? C94 C95 C98B 101.1(6) . . ? C96B C95 C98B 102.4(7) . . ? C97A C95 C98B 144.5(6) . . ? C95 C96A H96A 109.5 . . ? C95 C96A H96B 109.5 . . ? H96A C96A H96B 109.5 . . ? C95 C96A H96C 109.5 . . ? H96A C96A H96C 109.5 . . ? H96B C96A H96C 109.5 . . ? C95 C97A H97A 109.5 . . ? C95 C97A H97B 109.5 . . ? H97A C97A H97B 109.5 . . ? C95 C97A H97C 109.5 . . ? H97A C97A H97C 109.5 . . ? H97B C97A H97C 109.5 . . ? C95 C98A H98A 109.5 . . ? C95 C98A H98B 109.5 . . ? H98A C98A H98B 109.5 . . ? C95 C98A H98C 109.5 . . ? H98A C98A H98C 109.5 . . ? H98B C98A H98C 109.5 . . ? C95 C96B H96D 109.5 . . ? C95 C96B H96E 109.5 . . ? H96D C96B H96E 109.5 . . ? C95 C96B H96F 109.5 . . ? H96D C96B H96F 109.5 . . ? H96E C96B H96F 109.5 . . ? C95 C97B H97D 109.5 . . ? C95 C97B H97E 109.5 . . ? H97D C97B H97E 109.5 . . ? C95 C97B H97F 109.5 . . ? H97D C97B H97F 109.5 . . ? H97E C97B H97F 109.5 . . ? C95 C98B H98D 109.5 . . ? C95 C98B H98E 109.5 . . ? H98D C98B H98E 109.5 . . ? C95 C98B H98F 109.5 . . ? H98D C98B H98F 109.5 . . ? H98E C98B H98F 109.5 . . ? C99 O51 Fe15 134.6(3) . . ? C99 O52 Fe16 131.5(3) . . ? O52 C99 O51 124.2(4) . . ? O52 C99 C100 117.4(4) . . ? O51 C99 C100 118.3(4) . . ? C112 C100 C103 79.5(8) . . ? C112 C100 C101 129.6(9) . . ? C103 C100 C101 89.3(10) . . ? C112 C100 C111 123.9(7) . . ? C103 C100 C111 116.3(9) . . ? C101 C100 C111 28.0(7) . . ? C112 C100 C99 114.8(6) . . ? C103 C100 C99 108.2(8) . . ? C101 C100 C99 115.4(7) . . ? C111 C100 C99 110.1(5) . . ? C112 C100 C102 30.3(5) . . ? C103 C100 C102 109.4(8) . . ? C101 C100 C102 123.3(9) . . ? C111 C100 C102 104.1(6) . . ? C99 C100 C102 108.5(5) . . ? C112 C100 C113 93.2(8) . . ? C103 C100 C113 14.3(10) . . ? C101 C100 C113 83.8(9) . . ? C111 C100 C113 111.8(8) . . ? C99 C100 C113 98.6(7) . . ? C102 C100 C113 123.3(8) . . ? C100 C101 C103 44.9(7) . . ? C100 C101 H10C 109.5 . . ? C103 C101 H10C 90.3 . . ? C100 C101 H10D 109.5 . . ? C103 C101 H10D 79.1 . . ? H10C C101 H10D 109.5 . . ? C100 C101 H10E 109.5 . . ? C103 C101 H10E 153.2 . . ? H10C C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? C100 C102 H10F 109.5 . . ? C100 C102 H10G 109.5 . . ? H10F C102 H10G 109.5 . . ? C100 C102 H10H 109.5 . . ? H10F C102 H10H 109.5 . . ? H10G C102 H10H 109.5 . . ? C100 C103 C101 45.8(7) . . ? C100 C103 H10I 109.5 . . ? C101 C103 H10I 155.2 . . ? C100 C103 H10J 109.5 . . ? C101 C103 H10J 84.0 . . ? H10I C103 H10J 109.5 . . ? C100 C103 H10K 109.5 . . ? C101 C103 H10K 83.9 . . ? H10I C103 H10K 109.5 . . ? H10J C103 H10K 109.5 . . ? C100 C111 H11C 109.5 . . ? C100 C111 H11D 109.5 . . ? H11C C111 H11D 109.5 . . ? C100 C111 H11E 109.5 . . ? H11C C111 H11E 109.5 . . ? H11D C111 H11E 109.5 . . ? C100 C112 H11F 109.5 . . ? C100 C112 H11G 109.5 . . ? H11F C112 H11G 109.5 . . ? C100 C112 H11H 109.5 . . ? H11F C112 H11H 109.5 . . ? H11G C112 H11H 109.5 . . ? C100 C113 H11I 109.5 . . ? C100 C113 H11J 109.5 . . ? H11I C113 H11J 109.5 . . ? C100 C113 H11K 109.5 . . ? H11I C113 H11K 109.5 . . ? H11J C113 H11K 109.5 . . ? C104 O53 Fe15 137.4(3) . . ? C104 O54 Fe16 128.9(3) . . ? O54 C104 O53 125.5(4) . . ? O54 C104 C105 122.6(6) . . ? O53 C104 C105 111.3(6) . . ? O54 C104 C115 109.0(6) . . ? O53 C104 C115 124.8(5) . . ? C105 C104 C115 21.6(5) . . ? C106 C105 C107 114.9(10) . . ? C106 C105 C104 114.3(8) . . ? C107 C105 C104 116.8(9) . . ? C106 C105 C108 111.7(10) . . ? C107 C105 C108 97.6(8) . . ? C104 C105 C108 98.7(7) . . ? C105 C106 H10L 109.5 . . ? C105 C106 H10M 109.5 . . ? H10L C106 H10M 109.5 . . ? C105 C106 H10N 109.5 . . ? H10L C106 H10N 109.5 . . ? H10M C106 H10N 109.5 . . ? C105 C107 H10O 109.5 . . ? C105 C107 H10P 109.5 . . ? H10O C107 H10P 109.5 . . ? C105 C107 H10Q 109.5 . . ? H10O C107 H10Q 109.5 . . ? H10P C107 H10Q 109.5 . . ? C105 C108 H10R 109.5 . . ? C105 C108 H10S 109.5 . . ? H10R C108 H10S 109.5 . . ? C105 C108 H10T 109.5 . . ? H10R C108 H10T 109.5 . . ? H10S C108 H10T 109.5 . . ? C116 C115 C117 128.2(11) . . ? C116 C115 C118 78.8(12) . . ? C117 C115 C118 119.5(14) . . ? C116 C115 C104 113.5(9) . . ? C117 C115 C104 104.8(9) . . ? C118 C115 C104 110.0(12) . . ? C115 C116 H11L 109.5 . . ? C115 C116 H11M 109.5 . . ? H11L C116 H11M 109.5 . . ? C115 C116 H11N 109.5 . . ? H11L C116 H11N 109.5 . . ? H11M C116 H11N 109.5 . . ? C115 C117 H11O 109.5 . . ? C115 C117 H11P 109.5 . . ? H11O C117 H11P 109.5 . . ? C115 C117 H11Q 109.5 . . ? H11O C117 H11Q 109.5 . . ? H11P C117 H11Q 109.5 . . ? C115 C118 H11R 109.5 . . ? C115 C118 H11S 109.5 . . ? H11R C118 H11S 109.5 . . ? C115 C118 H11T 109.5 . . ? H11R C118 H11T 109.5 . . ? H11S C118 H11T 109.5 . . ? N42 N41 Fe11 126.6(3) . . ? N43 N42 N41 178.5(5) . . ? N52A N51 N52B 54.0(6) . . ? N52A N51 Fe13 137.2(7) . . ? N52B N51 Fe13 119.5(5) . . ? N51 N52A N53A 173.8(16) . . ? N53B N52B N51 174.1(12) . . ? N62 N61A Fe15 127.7(5) . . ? N62 N61B Fe15 121.5(6) . . ? N61A N62 N63B 144.6(8) . . ? N61A N62 N63A 173.3(8) . . ? N63B N62 N63A 42.0(5) . . ? N61A N62 N61B 26.3(5) . . ? N63B N62 N61B 168.6(8) . . ? N63A N62 N61B 147.3(8) . . ? N201 C201 C202 176.5(9) . . ? C201 C202 H20C 109.5 . . ? C201 C202 H20D 109.5 . . ? H20C C202 H20D 109.5 . . ? C201 C202 H20E 109.5 . . ? H20C C202 H20E 109.5 . . ? H20D C202 H20E 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O12A H12A O201 0.84 2.26 2.943(7) 138.4 . O12B H12B N61B 0.84 2.55 3.040(8) 118.2 . O15 H15 N33A 0.84 1.92 2.743(9) 165.6 2_645 O15 H15 N33B 0.84 2.06 2.883(9) 165.5 2_645 O18 H18 O15 0.84 2.42 2.923(7) 119.6 1_565 O36A H36A O42 0.84 2.06 2.900(7) 175.6 1_545 O39A H39D N21 0.84 2.17 2.940(4) 153.0 . O42 H42 N43 0.84 2.07 2.840(5) 153.1 2_556 _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.917 _refine_diff_density_min -1.176 _refine_diff_density_rms 0.100 ########################################################################### data_189 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H111 Fe8 N9 O27 S3' _chemical_formula_weight 1945.57 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' 'S' 'S' 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 55.495(2) _cell_length_b 15.4971(9) _cell_length_c 21.1361(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.000(3) _cell_angle_gamma 90.00 _cell_volume 16969.9(14) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30393 _cell_measurement_theta_min 1.57 _cell_measurement_theta_max 27.24 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8096 _exptl_absorpt_coefficient_mu 1.477 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.621 _exptl_absorpt_correction_T_max 0.809 _exptl_absorpt_process_details ; XPREP in SHELXTL 5.1 (Bruker AXS Inc., 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56154 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -65 _diffrn_reflns_limit_h_max 70 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 26.89 _reflns_number_total 17443 _reflns_number_gt 11437 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.05 (Stoe & Cie GmbH, 2000)' _computing_cell_refinement 'X-Area 1.09 (Stoe & Cie GmbH, 2000)' _computing_data_reduction 'X-Area 1.09 (Stoe & Cie GmbH, 2000)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _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^)+(0.0667P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17443 _refine_ls_number_parameters 972 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1254 _refine_ls_wR_factor_gt 0.1171 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _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 Fe1 Fe 0.120758(10) 0.25343(3) 0.59279(3) 0.02000(11) Uani 1 1 d . . . Fe2 Fe 0.143780(10) 0.25673(3) 0.48755(3) 0.01905(11) Uani 1 1 d . . . Fe3 Fe 0.192500(10) 0.24363(3) 0.60820(3) 0.02165(12) Uani 1 1 d . . . Fe4 Fe 0.154856(11) 0.08494(3) 0.61761(3) 0.01995(12) Uani 1 1 d . . . Fe5 Fe 0.113310(11) 0.09329(3) 0.44510(3) 0.02029(12) Uani 1 1 d . . . Fe6 Fe 0.073552(10) 0.24448(3) 0.45537(3) 0.01967(11) Uani 1 1 d . . . Fe7 Fe 0.113852(11) 0.42186(3) 0.45379(3) 0.02155(12) Uani 1 1 d . . . Fe8 Fe 0.153441(12) 0.42503(3) 0.61515(3) 0.02374(13) Uani 1 1 d . . . O1 O 0.15708(5) 0.20138(15) 0.58253(13) 0.0208(5) Uani 1 1 d . . . O2 O 0.10918(5) 0.20393(15) 0.48464(13) 0.0198(5) Uani 1 1 d . . . O3 O 0.13314(5) 0.35534(15) 0.53603(13) 0.0208(5) Uani 1 1 d . . . N1 N 0.10299(6) 0.2517(2) 0.67518(16) 0.0243(7) Uani 1 1 d . . . C1 C 0.09088(8) 0.1663(2) 0.6701(2) 0.0268(9) Uani 1 1 d . . . H1A H 0.0748 0.1641 0.6298 0.032 Uiso 1 1 calc R . . H1B H 0.0865 0.1552 0.7108 0.032 Uiso 1 1 calc R . . C2 C 0.10968(8) 0.0983(2) 0.6642(2) 0.0255(8) Uani 1 1 d . . . H2A H 0.1227 0.0854 0.7095 0.031 Uiso 1 1 calc R . . H2B H 0.1004 0.0444 0.6451 0.031 Uiso 1 1 calc R . . O4 O 0.12201(5) 0.13173(15) 0.62092(14) 0.0217(6) Uani 1 1 d . . . C3 C 0.08416(8) 0.3232(3) 0.6576(2) 0.0280(9) Uani 1 1 d . . . H3A H 0.0933 0.3793 0.6677 0.034 Uiso 1 1 calc R . . H3B H 0.0729 0.3190 0.6846 0.034 Uiso 1 1 calc R . . C4 C 0.06821(8) 0.3170(3) 0.5830(2) 0.0264(9) Uani 1 1 d . . . H4A H 0.0546 0.2726 0.5753 0.032 Uiso 1 1 calc R . . H4B H 0.0598 0.3731 0.5663 0.032 Uiso 1 1 calc R . . O5 O 0.08501(5) 0.29452(16) 0.54794(14) 0.0224(6) Uani 1 1 d . . . C5 C 0.12482(8) 0.2653(3) 0.7390(2) 0.0280(8) Uani 1 1 d . . . H5A H 0.1354 0.2123 0.7515 0.034 Uiso 1 1 calc R . . H5B H 0.1184 0.2788 0.7759 0.034 Uiso 1 1 calc R . . C6 C 0.14093(9) 0.3394(3) 0.7294(2) 0.0281(9) Uani 1 1 d . . . H6A H 0.1331 0.3952 0.7347 0.034 Uiso 1 1 calc R . . H6B H 0.1586 0.3365 0.7637 0.034 Uiso 1 1 calc R . . O6 O 0.14178(5) 0.33288(16) 0.66323(14) 0.0241(6) Uani 1 1 d . . . N2 N 0.22831(7) 0.3096(2) 0.60269(19) 0.0286(8) Uani 1 1 d . B . C7 C 0.22465(8) 0.3034(3) 0.5295(2) 0.0321(9) Uani 1 1 d . . . H7A H 0.2294 0.2449 0.5194 0.039 Uiso 1 1 calc R . . H7B H 0.2361 0.3455 0.5188 0.039 Uiso 1 1 calc R . . C8 C 0.19674(8) 0.3217(3) 0.4859(2) 0.0318(10) Uani 1 1 d . . . H8A H 0.1928 0.3836 0.4887 0.038 Uiso 1 1 calc R . . H8B H 0.1937 0.3074 0.4380 0.038 Uiso 1 1 calc R . . O7 O 0.18083(5) 0.27030(16) 0.51027(14) 0.0235(6) Uani 1 1 d . . . C9 C 0.22676(9) 0.4017(3) 0.6224(3) 0.0338(10) Uani 1 1 d . . . H9C H 0.2186 0.4372 0.5813 0.041 Uiso 1 1 calc R . . H9D H 0.2443 0.4245 0.6466 0.041 Uiso 1 1 calc R . . C10 C 0.21103(8) 0.4064(3) 0.6677(2) 0.0318(9) Uani 1 1 d . . . H10A H 0.2205 0.3783 0.7117 0.038 Uiso 1 1 calc R . . H10B H 0.2079 0.4674 0.6763 0.038 Uiso 1 1 calc R . . O8 O 0.18692(5) 0.36310(17) 0.63416(15) 0.0275(6) Uani 1 1 d . . . C11 C 0.25262(9) 0.2687(3) 0.6466(3) 0.0478(13) Uani 1 1 d . . . H11A H 0.2532 0.2734 0.6939 0.057 Uiso 0.78 1 calc PR A 1 H11B H 0.2514 0.2065 0.6353 0.057 Uiso 0.78 1 calc PR A 1 H11C H 0.2508 0.2104 0.6289 0.057 Uiso 0.22 1 d PR A 2 H11D H 0.2653 0.2956 0.6310 0.057 Uiso 0.22 1 d PR A 2 C12A C 0.27752(12) 0.2992(5) 0.6458(4) 0.0486(16) Uani 0.78 1 d P B 1 H12A H 0.2909 0.2556 0.6681 0.058 Uiso 0.78 1 calc PR B 1 H12B H 0.2764 0.3044 0.5981 0.058 Uiso 0.78 1 calc PR B 1 O9A O 0.28523(10) 0.3796(4) 0.6786(4) 0.093(2) Uani 0.78 1 d PDU B 1 H9A H 0.3026(7) 0.378(7) 0.693(5) 0.139 Uiso 0.78 1 d PD C 1 C12B C 0.2655(5) 0.2569(15) 0.7102(12) 0.045(5) Uiso 0.22 1 d P B 2 H12C H 0.2801 0.2176 0.7155 0.054 Uiso 0.22 1 calc PR B 2 H12D H 0.2542 0.2291 0.7314 0.054 Uiso 0.22 1 calc PR B 2 O9B O 0.2751(4) 0.3365(12) 0.7441(10) 0.062(5) Uiso 0.22 1 d P B 2 N3 N 0.13034(7) -0.0106(2) 0.39527(17) 0.0258(7) Uani 1 1 d . . . C13 C 0.14493(9) 0.0425(3) 0.3611(2) 0.0312(10) Uani 1 1 d . . . H13A H 0.1327 0.0658 0.3179 0.037 Uiso 1 1 calc R . . H13B H 0.1575 0.0054 0.3506 0.037 Uiso 1 1 calc R . . C14 C 0.15901(8) 0.1163(3) 0.4061(2) 0.0304(9) Uani 1 1 d . . . H14A H 0.1734 0.0940 0.4457 0.036 Uiso 1 1 calc R . . H14B H 0.1661 0.1561 0.3806 0.036 Uiso 1 1 calc R . . O10 O 0.14081(5) 0.15972(16) 0.42763(14) 0.0236(6) Uani 1 1 d . . . C15 C 0.14867(9) -0.0610(3) 0.4528(2) 0.0297(9) Uani 1 1 d . . . H15A H 0.1663 -0.0372 0.4648 0.036 Uiso 1 1 calc R . . H15B H 0.1489 -0.1219 0.4390 0.036 Uiso 1 1 calc R . . C16 C 0.14040(8) -0.0562(2) 0.5133(2) 0.0265(9) Uani 1 1 d . . . H16A H 0.1239 -0.0872 0.5038 0.032 Uiso 1 1 calc R . . H16B H 0.1536 -0.0830 0.5533 0.032 Uiso 1 1 calc R . . O11 O 0.13739(5) 0.03382(15) 0.52618(14) 0.0244(6) Uani 1 1 d . . . C17 C 0.11225(9) -0.0671(3) 0.3429(2) 0.0305(9) Uani 1 1 d . . . H17A H 0.1226 -0.1058 0.3251 0.037 Uiso 1 1 calc R . . H17B H 0.1017 -0.0303 0.3048 0.037 Uiso 1 1 calc R . . C18 C 0.09428(10) -0.1221(3) 0.3651(2) 0.0354(10) Uani 1 1 d . . . H18A H 0.0868 -0.0866 0.3924 0.042 Uiso 1 1 calc R . . H18B H 0.0799 -0.1429 0.3247 0.042 Uiso 1 1 calc R . . O12 O 0.10739(9) -0.1943(2) 0.4042(2) 0.0638(11) Uani 1 1 d D . . H12 H 0.0980(13) -0.245(3) 0.390(4) 0.096 Uiso 1 1 d D . . N4 N 0.09814(7) 0.45944(19) 0.33950(17) 0.0244(7) Uani 1 1 d . . . C19 C 0.11875(9) 0.4259(3) 0.3158(2) 0.0312(9) Uani 1 1 d . . . H19A H 0.1336 0.4662 0.3297 0.037 Uiso 1 1 calc R . . H19B H 0.1120 0.4222 0.2657 0.037 Uiso 1 1 calc R . . C20 C 0.12765(9) 0.3376(3) 0.3456(2) 0.0309(9) Uani 1 1 d . . . H20A H 0.1138 0.2945 0.3258 0.037 Uiso 1 1 calc R . . H20B H 0.1431 0.3196 0.3359 0.037 Uiso 1 1 calc R . . O13 O 0.13362(5) 0.34378(16) 0.41634(14) 0.0233(6) Uani 1 1 d . . . C21 C 0.07366(8) 0.4100(3) 0.3081(2) 0.0283(9) Uani 1 1 d . . . H21A H 0.0773 0.3545 0.2901 0.034 Uiso 1 1 calc R . . H21B H 0.0615 0.4433 0.2700 0.034 Uiso 1 1 calc R . . C22 C 0.06179(8) 0.3935(3) 0.3613(2) 0.0268(9) Uani 1 1 d . . . H22A H 0.0560 0.4484 0.3751 0.032 Uiso 1 1 calc R . . H22B H 0.0467 0.3546 0.3431 0.032 Uiso 1 1 calc R . . O14 O 0.08133(5) 0.35417(17) 0.41799(14) 0.0254(6) Uani 1 1 d . . . C23 C 0.09426(9) 0.5521(2) 0.3204(2) 0.0322(10) Uani 1 1 d . . . H23A H 0.0895 0.5572 0.2707 0.039 Uiso 1 1 calc R . . H23B H 0.1108 0.5831 0.3421 0.039 Uiso 1 1 calc R . . C24 C 0.07351(10) 0.5956(3) 0.3407(3) 0.0375(11) Uani 1 1 d . . . H24A H 0.0564 0.5698 0.3157 0.045 Uiso 1 1 calc R . . H24B H 0.0773 0.5885 0.3899 0.045 Uiso 1 1 calc R . . O15 O 0.07359(7) 0.6849(2) 0.3240(2) 0.0502(9) Uani 1 1 d D . . H15 H 0.0586(10) 0.724(4) 0.322(3) 0.075 Uiso 1 1 d D . . O16 O 0.20658(6) 0.20879(18) 0.70504(15) 0.0296(6) Uani 1 1 d . . . O17 O 0.17459(5) 0.12999(17) 0.71638(15) 0.0270(6) Uani 1 1 d . . . C25 C 0.19570(8) 0.1690(2) 0.7406(2) 0.0239(8) Uani 1 1 d . . . C26 C 0.21044(8) 0.1690(3) 0.8167(2) 0.0302(9) Uani 1 1 d . . . C27 C 0.21981(14) 0.2591(4) 0.8412(3) 0.0626(17) Uani 1 1 d . . . H27A H 0.2309 0.2801 0.8174 0.094 Uiso 1 1 calc R . . H27B H 0.2296 0.2578 0.8901 0.094 Uiso 1 1 calc R . . H27C H 0.2050 0.2977 0.8319 0.094 Uiso 1 1 calc R . . C28 C 0.19337(12) 0.1362(4) 0.8542(3) 0.0589(16) Uani 1 1 d . . . H28A H 0.1874 0.0778 0.8387 0.088 Uiso 1 1 calc R . . H28B H 0.1785 0.1746 0.8451 0.088 Uiso 1 1 calc R . . H28C H 0.2033 0.1353 0.9031 0.088 Uiso 1 1 calc R . . C29 C 0.23333(13) 0.1095(5) 0.8292(3) 0.074(2) Uani 1 1 d . . . H29A H 0.2442 0.1313 0.8049 0.112 Uiso 1 1 calc R . . H29B H 0.2272 0.0514 0.8129 0.112 Uiso 1 1 calc R . . H29C H 0.2435 0.1073 0.8779 0.112 Uiso 1 1 calc R . . O18 O 0.20995(6) 0.13555(17) 0.58795(16) 0.0290(6) Uani 1 1 d . . . O19 O 0.18834(5) 0.03290(17) 0.61924(16) 0.0298(7) Uani 1 1 d . . . C30 C 0.20689(8) 0.0583(2) 0.6019(2) 0.0247(8) Uani 1 1 d . . . C31 C 0.22710(8) -0.0082(3) 0.6017(2) 0.0301(9) Uani 1 1 d . . . C32 C 0.23922(11) 0.0166(3) 0.5495(3) 0.0477(13) Uani 1 1 d . . . H32A H 0.2469 0.0743 0.5599 0.071 Uiso 1 1 calc R . . H32B H 0.2259 0.0167 0.5041 0.071 Uiso 1 1 calc R . . H32C H 0.2527 -0.0253 0.5512 0.071 Uiso 1 1 calc R . . C33 C 0.24741(9) -0.0067(3) 0.6729(3) 0.0400(11) Uani 1 1 d . . . H33A H 0.2394 -0.0228 0.7057 0.060 Uiso 1 1 calc R . . H33B H 0.2547 0.0514 0.6831 0.060 Uiso 1 1 calc R . . H33C H 0.2612 -0.0479 0.6756 0.060 Uiso 1 1 calc R . . C34 C 0.21522(10) -0.0987(3) 0.5864(3) 0.0464(13) Uani 1 1 d . . . H34A H 0.2076 -0.1140 0.6201 0.070 Uiso 1 1 calc R . . H34B H 0.2287 -0.1406 0.5881 0.070 Uiso 1 1 calc R . . H34C H 0.2018 -0.0993 0.5411 0.070 Uiso 1 1 calc R . . O20 O 0.08392(6) 0.03140(17) 0.45844(16) 0.0287(6) Uani 1 1 d . . . O21 O 0.06267(6) 0.13335(16) 0.49223(15) 0.0267(6) Uani 1 1 d . . . C35 C 0.06691(8) 0.0560(2) 0.4820(2) 0.0220(8) Uani 1 1 d . . . C36 C 0.04971(8) -0.0134(2) 0.4943(2) 0.0285(9) Uani 1 1 d . . . C37 C 0.03792(9) 0.0165(3) 0.5462(2) 0.0352(10) Uani 1 1 d . . . H37A H 0.0517 0.0261 0.5901 0.053 Uiso 1 1 calc R . . H37B H 0.0261 -0.0279 0.5509 0.053 Uiso 1 1 calc R . . H37C H 0.0284 0.0704 0.5306 0.053 Uiso 1 1 calc R . . C38 C 0.06490(11) -0.0973(3) 0.5183(3) 0.0492(14) Uani 1 1 d . . . H38A H 0.0724 -0.1157 0.4850 0.074 Uiso 1 1 calc R . . H38B H 0.0533 -0.1422 0.5232 0.074 Uiso 1 1 calc R . . H38C H 0.0788 -0.0875 0.5621 0.074 Uiso 1 1 calc R . . C39 C 0.02809(11) -0.0280(4) 0.4260(3) 0.0520(14) Uani 1 1 d . . . H39A H 0.0355 -0.0470 0.3927 0.078 Uiso 1 1 calc R . . H39B H 0.0186 0.0260 0.4106 0.078 Uiso 1 1 calc R . . H39C H 0.0163 -0.0723 0.4308 0.078 Uiso 1 1 calc R . . O22 O 0.08980(6) 0.10907(18) 0.34685(15) 0.0299(6) Uani 1 1 d . . . O23 O 0.05991(5) 0.19457(18) 0.36038(14) 0.0279(6) Uani 1 1 d . . . C40 C 0.06843(8) 0.1486(2) 0.3243(2) 0.0243(8) Uani 1 1 d . . . C41 C 0.05238(9) 0.1385(3) 0.2495(2) 0.0333(10) Uani 1 1 d . . . C42 C 0.06975(12) 0.1442(4) 0.2074(3) 0.0570(15) Uani 1 1 d . . . H42A H 0.0830 0.0992 0.2220 0.086 Uiso 1 1 calc R . . H42B H 0.0781 0.2010 0.2140 0.086 Uiso 1 1 calc R . . H42C H 0.0593 0.1362 0.1594 0.086 Uiso 1 1 calc R . . C43 C 0.03994(13) 0.0485(4) 0.2414(3) 0.0633(17) Uani 1 1 d . . . H43A H 0.0290 0.0450 0.2687 0.095 Uiso 1 1 calc R . . H43B H 0.0535 0.0045 0.2567 0.095 Uiso 1 1 calc R . . H43C H 0.0295 0.0386 0.1936 0.095 Uiso 1 1 calc R . . C44 C 0.03173(12) 0.2088(4) 0.2263(3) 0.0654(18) Uani 1 1 d . . . H44A H 0.0206 0.2056 0.2533 0.098 Uiso 1 1 calc R . . H44B H 0.0213 0.2003 0.1783 0.098 Uiso 1 1 calc R . . H44C H 0.0401 0.2655 0.2324 0.098 Uiso 1 1 calc R . . O24 O 0.09584(6) 0.50497(18) 0.49386(16) 0.0337(7) Uani 1 1 d . . . O25 O 0.12078(7) 0.4992(2) 0.60304(17) 0.0430(8) Uani 1 1 d . . . C45 C 0.10241(9) 0.5301(3) 0.5547(2) 0.0328(10) Uani 1 1 d . D . C46 C 0.08707(11) 0.6037(3) 0.5707(3) 0.0463(13) Uani 1 1 d . . . C47A C 0.07133(13) 0.5672(4) 0.6102(3) 0.0373(13) Uiso 0.78 1 d P D 1 H47D H 0.0821 0.5647 0.6585 0.056 Uiso 0.78 1 calc PR D 1 H47E H 0.0654 0.5090 0.5938 0.056 Uiso 0.78 1 calc PR D 1 H47F H 0.0564 0.6044 0.6040 0.056 Uiso 0.78 1 calc PR D 1 C48A C 0.07158(14) 0.6537(4) 0.5103(4) 0.0504(16) Uiso 0.78 1 d P D 1 H48A H 0.0812 0.7053 0.5065 0.076 Uiso 0.78 1 calc PR D 1 H48B H 0.0553 0.6709 0.5147 0.076 Uiso 0.78 1 calc PR D 1 H48C H 0.0680 0.6180 0.4697 0.076 Uiso 0.78 1 calc PR D 1 C49A C 0.10795(14) 0.6674(4) 0.6226(4) 0.0501(16) Uiso 0.78 1 d P D 1 H49A H 0.1241 0.6360 0.6449 0.075 Uiso 0.78 1 calc PR D 1 H49B H 0.1013 0.6882 0.6569 0.075 Uiso 0.78 1 calc PR D 1 H49C H 0.1111 0.7166 0.5976 0.075 Uiso 0.78 1 calc PR D 1 C47B C 0.0538(4) 0.5756(14) 0.5092(12) 0.043(5) Uiso 0.22 1 d P D 2 H47A H 0.0535 0.5152 0.4952 0.065 Uiso 0.22 1 calc PR D 2 H47B H 0.0495 0.6130 0.4693 0.065 Uiso 0.22 1 calc PR D 2 H47C H 0.0411 0.5840 0.5311 0.065 Uiso 0.22 1 calc PR D 2 C48B C 0.0912(6) 0.6778(18) 0.5426(16) 0.064(7) Uiso 0.22 1 d P D 2 H48D H 0.1081 0.7012 0.5700 0.096 Uiso 0.22 1 calc PR D 2 H48E H 0.0778 0.7198 0.5410 0.096 Uiso 0.22 1 calc PR D 2 H48F H 0.0907 0.6664 0.4966 0.096 Uiso 0.22 1 calc PR D 2 C49B C 0.0841(7) 0.593(2) 0.6335(18) 0.077(9) Uiso 0.22 1 d P D 2 H49D H 0.1008 0.6015 0.6701 0.116 Uiso 0.22 1 calc PR D 2 H49E H 0.0779 0.5342 0.6364 0.116 Uiso 0.22 1 calc PR D 2 H49F H 0.0716 0.6349 0.6378 0.116 Uiso 0.22 1 calc PR D 2 O26 O 0.13837(6) 0.52190(17) 0.45845(16) 0.0330(7) Uani 1 1 d . . . O27 O 0.16585(7) 0.5142(2) 0.56466(17) 0.0426(8) Uani 1 1 d . . . C50 C 0.15746(8) 0.5484(2) 0.5071(2) 0.0270(9) Uani 1 1 d . . . C51 C 0.17155(9) 0.6294(3) 0.4977(3) 0.0368(11) Uani 1 1 d . . . C52 C 0.16534(16) 0.7012(3) 0.5395(4) 0.075(2) Uani 1 1 d . . . H52A H 0.1714 0.6842 0.5873 0.112 Uiso 1 1 calc R . . H52B H 0.1466 0.7108 0.5231 0.112 Uiso 1 1 calc R . . H52C H 0.1740 0.7546 0.5348 0.112 Uiso 1 1 calc R . . C53 C 0.16200(13) 0.6582(4) 0.4236(3) 0.0607(16) Uani 1 1 d . . . H53A H 0.1660 0.6135 0.3960 0.091 Uiso 1 1 calc R . . H53B H 0.1706 0.7121 0.4198 0.091 Uiso 1 1 calc R . . H53C H 0.1433 0.6675 0.4075 0.091 Uiso 1 1 calc R . . C54 C 0.20027(12) 0.6124(4) 0.5234(5) 0.092(3) Uani 1 1 d . . . H54A H 0.2040 0.5669 0.4961 0.137 Uiso 1 1 calc R . . H54B H 0.2060 0.5940 0.5708 0.137 Uiso 1 1 calc R . . H54C H 0.2094 0.6653 0.5198 0.137 Uiso 1 1 calc R . . N5 N 0.14974(7) -0.0268(2) 0.66464(18) 0.0294(8) Uani 1 1 d . . . C61 C 0.15313(9) -0.0929(3) 0.6912(2) 0.0322(10) Uani 1 1 d . . . S1 S 0.15765(4) -0.18679(8) 0.72780(9) 0.0640(4) Uani 1 1 d . . . N6 N 0.03555(7) 0.2822(2) 0.43802(18) 0.0272(7) Uani 1 1 d . . . C62 C 0.01697(9) 0.2750(3) 0.4509(2) 0.0363(10) Uani 1 1 d . . . S2 S -0.00861(3) 0.26472(17) 0.47008(10) 0.0882(7) Uani 1 1 d . . . N7 N 0.16899(8) 0.4939(2) 0.7036(2) 0.0349(9) Uani 1 1 d . . . C63 C 0.17678(9) 0.5236(3) 0.7571(2) 0.0327(10) Uani 1 1 d . . . S3 S 0.18765(3) 0.56427(13) 0.83260(8) 0.0671(5) Uani 1 1 d . . . N71 N 0.02742(12) 0.7518(4) 0.3343(4) 0.0867(19) Uani 1 1 d . . . C71 C 0.00728(14) 0.7638(4) 0.3365(4) 0.0669(17) Uani 1 1 d . . . C72 C -0.01865(15) 0.7817(6) 0.3375(5) 0.089(2) Uani 1 1 d . . . N73 N 0.0302(3) 0.4354(9) 0.6667(7) 0.189(5) Uiso 1 1 d . . . C73 C 0.0122(4) 0.4811(11) 0.6474(10) 0.186(6) Uiso 1 1 d . . . C74 C -0.0062(4) 0.5044(12) 0.5721(11) 0.214(7) Uiso 1 1 d . . . 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 Fe1 0.0234(3) 0.0196(2) 0.0185(3) 0.0000(2) 0.0093(2) -0.0001(2) Fe2 0.0208(3) 0.0186(2) 0.0188(3) 0.0001(2) 0.0083(2) 0.0002(2) Fe3 0.0218(3) 0.0208(2) 0.0216(3) 0.0018(2) 0.0068(2) -0.0019(2) Fe4 0.0213(3) 0.0180(2) 0.0204(3) 0.0011(2) 0.0072(3) 0.0000(2) Fe5 0.0220(3) 0.0190(2) 0.0203(3) -0.0020(2) 0.0082(3) -0.0001(2) Fe6 0.0201(3) 0.0202(2) 0.0197(3) -0.0001(2) 0.0084(2) 0.0002(2) Fe7 0.0247(3) 0.0189(2) 0.0209(3) 0.0019(2) 0.0080(3) 0.0009(2) Fe8 0.0300(3) 0.0188(2) 0.0212(3) -0.0017(2) 0.0078(3) -0.0024(2) O1 0.0210(14) 0.0221(12) 0.0186(14) 0.0021(10) 0.0063(12) 0.0010(10) O2 0.0215(14) 0.0203(12) 0.0174(14) -0.0020(10) 0.0068(12) -0.0013(10) O3 0.0240(13) 0.0194(11) 0.0208(14) 0.0007(10) 0.0101(12) -0.0015(10) N1 0.0293(17) 0.0239(15) 0.0224(17) -0.0009(13) 0.0125(15) -0.0010(14) C1 0.031(2) 0.0273(19) 0.028(2) -0.0002(16) 0.018(2) -0.0047(16) C2 0.032(2) 0.0234(18) 0.028(2) 0.0038(15) 0.018(2) -0.0017(15) O4 0.0259(14) 0.0222(12) 0.0207(15) 0.0012(10) 0.0128(13) -0.0013(10) C3 0.033(2) 0.0294(19) 0.025(2) -0.0030(16) 0.014(2) 0.0065(16) C4 0.028(2) 0.033(2) 0.024(2) -0.0016(16) 0.016(2) 0.0064(16) O5 0.0236(14) 0.0239(12) 0.0221(15) -0.0007(10) 0.0112(13) 0.0010(10) C5 0.032(2) 0.035(2) 0.015(2) 0.0018(15) 0.0071(19) 0.0010(17) C6 0.037(2) 0.034(2) 0.015(2) -0.0028(15) 0.011(2) -0.0030(17) O6 0.0288(15) 0.0268(13) 0.0192(15) -0.0030(10) 0.0116(13) -0.0034(11) N2 0.0234(18) 0.0280(17) 0.032(2) 0.0027(14) 0.0069(17) -0.0039(13) C7 0.026(2) 0.039(2) 0.036(3) 0.0048(18) 0.018(2) -0.0020(17) C8 0.029(2) 0.037(2) 0.036(3) 0.0117(18) 0.019(2) -0.0033(17) O7 0.0234(14) 0.0245(13) 0.0251(15) 0.0032(10) 0.0116(13) -0.0011(10) C9 0.033(2) 0.0254(19) 0.047(3) -0.0003(18) 0.019(2) -0.0084(17) C10 0.024(2) 0.031(2) 0.034(3) -0.0051(17) 0.003(2) -0.0084(16) O8 0.0265(15) 0.0259(13) 0.0284(17) -0.0029(11) 0.0078(14) -0.0084(11) C11 0.032(2) 0.033(2) 0.062(4) 0.001(2) -0.003(3) -0.0033(19) C12A 0.025(3) 0.059(4) 0.058(5) -0.005(3) 0.010(3) -0.002(3) O9A 0.035(3) 0.048(3) 0.173(8) -0.016(4) 0.010(4) -0.008(2) N3 0.0314(19) 0.0231(15) 0.0234(19) -0.0037(13) 0.0106(17) 0.0026(13) C13 0.037(2) 0.031(2) 0.035(3) -0.0043(17) 0.023(2) 0.0036(17) C14 0.028(2) 0.031(2) 0.040(3) -0.0095(17) 0.021(2) 0.0026(16) O10 0.0236(14) 0.0252(13) 0.0247(16) -0.0031(11) 0.0120(13) 0.0018(10) C15 0.033(2) 0.0273(19) 0.029(2) -0.0027(16) 0.010(2) 0.0097(16) C16 0.034(2) 0.0182(17) 0.026(2) -0.0043(15) 0.008(2) 0.0029(15) O11 0.0300(15) 0.0177(12) 0.0252(16) -0.0020(10) 0.0097(14) 0.0042(10) C17 0.037(2) 0.0282(19) 0.024(2) -0.0089(16) 0.008(2) 0.0008(17) C18 0.044(3) 0.027(2) 0.031(3) -0.0054(17) 0.009(2) -0.0029(18) O12 0.077(3) 0.0363(19) 0.060(3) 0.0050(18) 0.002(2) -0.0071(19) N4 0.0256(18) 0.0231(15) 0.0241(19) 0.0052(13) 0.0086(16) 0.0007(13) C19 0.035(2) 0.040(2) 0.022(2) 0.0107(17) 0.014(2) 0.0070(18) C20 0.038(3) 0.040(2) 0.016(2) 0.0052(16) 0.013(2) 0.0108(18) O13 0.0267(15) 0.0246(13) 0.0189(15) 0.0032(10) 0.0087(13) 0.0033(11) C21 0.032(2) 0.029(2) 0.021(2) 0.0037(15) 0.006(2) -0.0022(16) C22 0.021(2) 0.0285(19) 0.025(2) 0.0110(16) 0.0022(19) 0.0031(15) O14 0.0237(14) 0.0275(13) 0.0217(16) 0.0081(11) 0.0043(13) 0.0025(11) C23 0.039(3) 0.0224(18) 0.037(3) 0.0105(17) 0.015(2) 0.0016(17) C24 0.052(3) 0.024(2) 0.039(3) 0.0027(17) 0.018(3) 0.0061(19) O15 0.056(2) 0.0274(16) 0.063(3) 0.0091(15) 0.015(2) 0.0040(15) O16 0.0273(16) 0.0347(15) 0.0247(17) 0.0056(12) 0.0070(14) -0.0055(12) O17 0.0258(15) 0.0299(14) 0.0233(16) 0.0007(11) 0.0062(14) -0.0061(11) C25 0.023(2) 0.0225(17) 0.023(2) 0.0027(15) 0.0041(18) 0.0016(15) C26 0.030(2) 0.036(2) 0.022(2) 0.0031(16) 0.007(2) -0.0059(17) C27 0.085(5) 0.056(3) 0.035(3) -0.009(2) 0.009(3) -0.031(3) C28 0.054(4) 0.092(4) 0.031(3) 0.002(3) 0.016(3) -0.030(3) C29 0.057(4) 0.108(5) 0.042(4) 0.009(3) -0.003(3) 0.042(4) O18 0.0273(15) 0.0242(13) 0.0364(18) 0.0035(12) 0.0124(15) 0.0014(11) O19 0.0248(15) 0.0246(13) 0.0426(19) 0.0059(12) 0.0152(15) 0.0017(11) C30 0.024(2) 0.0231(18) 0.024(2) 0.0008(15) 0.0049(19) 0.0030(15) C31 0.025(2) 0.029(2) 0.035(3) 0.0031(17) 0.009(2) 0.0063(16) C32 0.046(3) 0.054(3) 0.051(3) 0.006(2) 0.027(3) 0.019(2) C33 0.031(2) 0.037(2) 0.048(3) 0.005(2) 0.009(2) 0.0115(19) C34 0.035(3) 0.026(2) 0.073(4) -0.005(2) 0.015(3) 0.0067(19) O20 0.0292(15) 0.0242(13) 0.0369(18) -0.0056(12) 0.0170(15) -0.0016(11) O21 0.0316(16) 0.0211(12) 0.0316(17) 0.0002(11) 0.0164(14) -0.0011(11) C35 0.023(2) 0.0194(17) 0.022(2) -0.0003(14) 0.0072(18) -0.0027(14) C36 0.030(2) 0.0258(19) 0.034(3) -0.0041(16) 0.017(2) -0.0082(16) C37 0.036(3) 0.036(2) 0.040(3) 0.0011(19) 0.023(2) -0.0070(18) C38 0.065(4) 0.024(2) 0.074(4) 0.010(2) 0.044(3) 0.003(2) C39 0.046(3) 0.065(3) 0.045(3) -0.017(3) 0.017(3) -0.029(3) O22 0.0259(15) 0.0375(15) 0.0233(16) -0.0049(12) 0.0053(14) 0.0037(12) O23 0.0240(15) 0.0342(15) 0.0232(16) -0.0061(12) 0.0057(13) 0.0055(11) C40 0.023(2) 0.0282(19) 0.020(2) -0.0003(15) 0.0053(19) -0.0020(15) C41 0.031(2) 0.044(2) 0.019(2) -0.0054(17) 0.002(2) 0.0002(19) C42 0.055(4) 0.093(4) 0.024(3) -0.001(3) 0.016(3) 0.004(3) C43 0.065(4) 0.067(4) 0.041(4) -0.007(3) -0.003(3) -0.028(3) C44 0.058(4) 0.089(4) 0.029(3) -0.009(3) -0.009(3) 0.030(3) O24 0.0404(18) 0.0337(15) 0.0259(17) 0.0015(12) 0.0105(16) 0.0117(13) O25 0.050(2) 0.0370(17) 0.035(2) -0.0108(14) 0.0074(18) 0.0157(15) C45 0.037(3) 0.028(2) 0.036(3) 0.0032(18) 0.016(2) 0.0061(18) C46 0.064(4) 0.039(2) 0.046(3) 0.012(2) 0.033(3) 0.023(2) O26 0.0348(17) 0.0272(14) 0.0326(18) 0.0036(12) 0.0066(16) -0.0081(12) O27 0.049(2) 0.0376(17) 0.0315(19) 0.0087(14) 0.0022(17) -0.0192(15) C50 0.029(2) 0.0206(17) 0.032(3) 0.0037(16) 0.011(2) -0.0025(15) C51 0.039(3) 0.028(2) 0.041(3) 0.0096(18) 0.012(2) -0.0071(18) C52 0.118(6) 0.034(3) 0.079(5) -0.014(3) 0.042(5) -0.027(3) C53 0.077(4) 0.050(3) 0.053(4) 0.020(3) 0.020(3) -0.020(3) C54 0.037(3) 0.070(4) 0.151(8) 0.059(5) 0.015(4) -0.009(3) N5 0.032(2) 0.0282(17) 0.028(2) 0.0033(14) 0.0104(18) -0.0012(14) C61 0.041(3) 0.027(2) 0.030(2) 0.0039(17) 0.015(2) -0.0012(17) S1 0.0964(13) 0.0316(6) 0.0599(10) 0.0186(6) 0.0229(10) 0.0038(7) N6 0.0231(18) 0.0310(17) 0.028(2) -0.0003(13) 0.0093(17) 0.0015(13) C62 0.027(2) 0.052(3) 0.028(3) -0.0024(19) 0.007(2) 0.0038(19) S2 0.0335(8) 0.177(2) 0.0635(11) -0.0110(12) 0.0285(8) -0.0113(10) N7 0.045(2) 0.0266(17) 0.029(2) -0.0069(15) 0.008(2) -0.0041(15) C63 0.028(2) 0.035(2) 0.037(3) -0.0092(19) 0.015(2) 0.0004(17) S3 0.0424(8) 0.1123(13) 0.0455(9) -0.0453(9) 0.0143(8) -0.0089(8) N71 0.064(4) 0.103(5) 0.090(5) -0.012(4) 0.023(4) 0.015(4) C71 0.070(4) 0.062(4) 0.072(5) -0.006(3) 0.030(4) -0.002(3) C72 0.061(4) 0.123(6) 0.097(6) -0.018(5) 0.045(5) -0.003(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 Fe1 O6 1.962(3) . ? Fe1 O4 1.971(2) . ? Fe1 O5 1.973(3) . ? Fe1 O3 2.235(2) . ? Fe1 O1 2.253(2) . ? Fe1 O2 2.275(3) . ? Fe1 N1 2.288(3) . ? Fe1 Fe2 2.9359(7) . ? Fe2 O10 1.934(3) . ? Fe2 O13 1.948(3) . ? Fe2 O7 1.948(3) . ? Fe2 O3 2.041(2) . ? Fe2 O1 2.061(3) . ? Fe2 O2 2.068(2) . ? Fe3 O1 1.955(3) . ? Fe3 O7 1.978(3) . ? Fe3 O16 1.986(3) . ? Fe3 O8 1.987(3) . ? Fe3 O18 2.055(3) . ? Fe3 N2 2.275(3) . ? Fe4 O1 1.972(2) . ? Fe4 O4 1.986(3) . ? Fe4 O11 1.990(3) . ? Fe4 O19 2.015(3) . ? Fe4 N5 2.066(3) . ? Fe4 O17 2.099(3) . ? Fe5 O2 1.957(2) . ? Fe5 O10 1.982(3) . ? Fe5 O11 1.983(3) . ? Fe5 O20 1.997(3) . ? Fe5 O22 2.033(3) . ? Fe5 N3 2.304(3) . ? Fe6 O2 1.952(3) . ? Fe6 O5 1.986(3) . ? Fe6 O14 1.986(3) . ? Fe6 O23 2.028(3) . ? Fe6 O21 2.068(3) . ? Fe6 N6 2.090(3) . ? Fe7 O3 1.974(3) . ? Fe7 O13 1.979(3) . ? Fe7 O14 1.988(3) . ? Fe7 O24 1.995(3) . ? Fe7 O26 2.042(3) . ? Fe7 N4 2.329(3) . ? Fe8 O3 1.970(3) . ? Fe8 O6 1.991(3) . ? Fe8 O8 2.000(3) . ? Fe8 O27 2.012(3) . ? Fe8 N7 2.055(4) . ? Fe8 O25 2.083(3) . ? N1 C5 1.470(6) . ? N1 C1 1.471(5) . ? N1 C3 1.476(5) . ? C1 C2 1.518(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O4 1.422(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.509(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O5 1.427(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.514(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O6 1.420(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N2 C11 1.478(6) . ? N2 C7 1.490(6) . ? N2 C9 1.498(5) . ? C7 C8 1.518(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O7 1.416(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.511(6) . ? C9 H9C 0.9900 . ? C9 H9D 0.9900 . ? C10 O8 1.436(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12B 1.29(3) . ? C11 C12A 1.466(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 H11C 0.9700 . ? C11 H11D 0.9702 . ? C12A O9A 1.416(9) . ? C12A H11D 0.6403 . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? O9A H9A 0.90(4) . ? C12B O9B 1.43(3) . ? C12B H12C 0.9900 . ? C12B H12D 0.9900 . ? N3 C17 1.485(5) . ? N3 C15 1.495(5) . ? N3 C13 1.508(5) . ? C13 C14 1.512(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O10 1.418(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.508(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O11 1.442(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.509(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O12 1.426(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? O12 H12 0.93(4) . ? N4 C23 1.486(5) . ? N4 C21 1.492(5) . ? N4 C19 1.497(5) . ? C19 C20 1.513(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O13 1.414(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.514(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O14 1.433(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.523(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O15 1.428(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? O15 H15 1.01(4) . ? O16 C25 1.279(5) . ? O17 C25 1.253(5) . ? C25 C26 1.521(6) . ? C26 C29 1.514(7) . ? C26 C27 1.515(6) . ? C26 C28 1.524(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? O18 C30 1.259(5) . ? O19 C30 1.272(5) . ? C30 C31 1.525(5) . ? C31 C33 1.523(7) . ? C31 C32 1.532(6) . ? C31 C34 1.535(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O20 C35 1.274(4) . ? O21 C35 1.255(4) . ? C35 C36 1.521(5) . ? C36 C39 1.529(7) . ? C36 C38 1.533(6) . ? C36 C37 1.535(6) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? O22 C40 1.267(5) . ? O23 C40 1.254(5) . ? C40 C41 1.518(6) . ? C41 C44 1.529(7) . ? C41 C42 1.531(6) . ? C41 C43 1.539(7) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? O24 C45 1.266(5) . ? O25 C45 1.251(6) . ? C45 C46 1.532(6) . ? C46 C48B 1.35(3) . ? C46 C49B 1.40(3) . ? C46 C48A 1.477(9) . ? C46 C47A 1.517(7) . ? C46 C49A 1.615(9) . ? C46 C47B 1.89(2) . ? C47A H47D 0.9800 . ? C47A H47E 0.9800 . ? C47A H47F 0.9800 . ? C48A H48A 0.9800 . ? C48A H48B 0.9800 . ? C48A H48C 0.9800 . ? C49A H49A 0.9800 . ? C49A H49B 0.9800 . ? C49A H49C 0.9800 . ? C47B H47A 0.9800 . ? C47B H47B 0.9800 . ? C47B H47C 0.9800 . ? C48B H48D 0.9800 . ? C48B H48E 0.9800 . ? C48B H48F 0.9800 . ? C49B H49D 0.9800 . ? C49B H49E 0.9800 . ? C49B H49F 0.9800 . ? O26 C50 1.252(5) . ? O27 C50 1.254(5) . ? C50 C51 1.528(5) . ? C51 C54 1.511(8) . ? C51 C53 1.529(7) . ? C51 C52 1.535(7) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? N5 C61 1.150(5) . ? C61 S1 1.625(4) . ? N6 C62 1.162(5) . ? C62 S2 1.618(5) . ? N7 C63 1.151(6) . ? C63 S3 1.618(5) . ? N71 C71 1.150(8) . ? C71 C72 1.474(10) . ? N73 C73 1.171(19) . ? C73 C74 1.59(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 O6 Fe1 O4 115.11(11) . . ? O6 Fe1 O5 112.59(11) . . ? O4 Fe1 O5 112.00(11) . . ? O6 Fe1 O3 75.54(10) . . ? O4 Fe1 O3 148.58(9) . . ? O5 Fe1 O3 87.92(10) . . ? O6 Fe1 O1 89.34(10) . . ? O4 Fe1 O1 75.54(10) . . ? O5 Fe1 O1 148.19(10) . . ? O3 Fe1 O1 75.13(9) . . ? O6 Fe1 O2 148.36(10) . . ? O4 Fe1 O2 86.97(10) . . ? O5 Fe1 O2 75.68(10) . . ? O3 Fe1 O2 74.30(9) . . ? O1 Fe1 O2 73.90(9) . . ? O6 Fe1 N1 74.39(11) . . ? O4 Fe1 N1 74.80(11) . . ? O5 Fe1 N1 74.69(11) . . ? O3 Fe1 N1 135.71(10) . . ? O1 Fe1 N1 135.54(11) . . ? O2 Fe1 N1 135.83(11) . . ? O6 Fe1 Fe2 105.20(7) . . ? O4 Fe1 Fe2 105.50(7) . . ? O5 Fe1 Fe2 105.43(8) . . ? O3 Fe1 Fe2 43.95(6) . . ? O1 Fe1 Fe2 44.43(7) . . ? O2 Fe1 Fe2 44.55(6) . . ? N1 Fe1 Fe2 179.58(9) . . ? O10 Fe2 O13 95.69(11) . . ? O10 Fe2 O7 94.59(11) . . ? O13 Fe2 O7 95.93(11) . . ? O10 Fe2 O3 159.77(11) . . ? O13 Fe2 O3 79.27(10) . . ? O7 Fe2 O3 105.37(11) . . ? O10 Fe2 O1 103.35(11) . . ? O13 Fe2 O1 160.76(11) . . ? O7 Fe2 O1 80.03(10) . . ? O3 Fe2 O1 83.67(10) . . ? O10 Fe2 O2 79.20(10) . . ? O13 Fe2 O2 104.03(11) . . ? O7 Fe2 O2 159.54(11) . . ? O3 Fe2 O2 83.03(10) . . ? O1 Fe2 O2 82.47(10) . . ? O10 Fe2 Fe1 121.63(8) . . ? O13 Fe2 Fe1 120.89(8) . . ? O7 Fe2 Fe1 121.51(8) . . ? O3 Fe2 Fe1 49.47(7) . . ? O1 Fe2 Fe1 49.91(7) . . ? O2 Fe2 Fe1 50.51(7) . . ? O1 Fe3 O7 81.96(11) . . ? O1 Fe3 O16 100.38(11) . . ? O7 Fe3 O16 174.46(12) . . ? O1 Fe3 O8 98.52(11) . . ? O7 Fe3 O8 93.97(11) . . ? O16 Fe3 O8 90.65(12) . . ? O1 Fe3 O18 99.86(11) . . ? O7 Fe3 O18 87.38(11) . . ? O16 Fe3 O18 87.27(12) . . ? O8 Fe3 O18 161.58(11) . . ? O1 Fe3 N2 161.13(12) . . ? O7 Fe3 N2 79.44(12) . . ? O16 Fe3 N2 98.43(12) . . ? O8 Fe3 N2 79.67(12) . . ? O18 Fe3 N2 82.54(11) . . ? O1 Fe4 O4 82.01(10) . . ? O1 Fe4 O11 94.22(11) . . ? O4 Fe4 O11 92.63(11) . . ? O1 Fe4 O19 101.02(11) . . ? O4 Fe4 O19 176.45(11) . . ? O11 Fe4 O19 89.00(12) . . ? O1 Fe4 N5 170.36(12) . . ? O4 Fe4 N5 90.16(12) . . ? O11 Fe4 N5 91.75(13) . . ? O19 Fe4 N5 86.64(12) . . ? O1 Fe4 O17 89.36(11) . . ? O4 Fe4 O17 90.10(11) . . ? O11 Fe4 O17 175.77(11) . . ? O19 Fe4 O17 88.10(12) . . ? N5 Fe4 O17 85.01(13) . . ? O2 Fe5 O10 80.81(10) . . ? O2 Fe5 O11 100.60(11) . . ? O10 Fe5 O11 94.41(11) . . ? O2 Fe5 O20 97.69(10) . . ? O10 Fe5 O20 176.27(12) . . ? O11 Fe5 O20 89.22(12) . . ? O2 Fe5 O22 101.56(11) . . ? O10 Fe5 O22 90.13(12) . . ? O11 Fe5 O22 157.82(11) . . ? O20 Fe5 O22 86.82(12) . . ? O2 Fe5 N3 159.67(11) . . ? O10 Fe5 N3 78.96(11) . . ? O11 Fe5 N3 79.07(11) . . ? O20 Fe5 N3 102.62(11) . . ? O22 Fe5 N3 80.52(12) . . ? O2 Fe6 O5 83.29(11) . . ? O2 Fe6 O14 93.55(11) . . ? O5 Fe6 O14 91.10(11) . . ? O2 Fe6 O23 99.63(11) . . ? O5 Fe6 O23 176.99(11) . . ? O14 Fe6 O23 89.42(12) . . ? O2 Fe6 O21 90.68(11) . . ? O5 Fe6 O21 89.29(11) . . ? O14 Fe6 O21 175.77(11) . . ? O23 Fe6 O21 89.98(12) . . ? O2 Fe6 N6 171.61(12) . . ? O5 Fe6 N6 90.59(12) . . ? O14 Fe6 N6 92.31(12) . . ? O23 Fe6 N6 86.43(12) . . ? O21 Fe6 N6 83.47(12) . . ? O3 Fe7 O13 80.18(10) . . ? O3 Fe7 O14 101.04(11) . . ? O13 Fe7 O14 94.76(11) . . ? O3 Fe7 O24 99.17(11) . . ? O13 Fe7 O24 176.53(13) . . ? O14 Fe7 O24 88.71(12) . . ? O3 Fe7 O26 102.26(12) . . ? O13 Fe7 O26 91.61(12) . . ? O14 Fe7 O26 156.57(12) . . ? O24 Fe7 O26 85.18(13) . . ? O3 Fe7 N4 157.99(11) . . ? O13 Fe7 N4 78.06(11) . . ? O14 Fe7 N4 77.63(11) . . ? O24 Fe7 N4 102.74(12) . . ? O26 Fe7 N4 81.69(12) . . ? O3 Fe8 O6 81.29(11) . . ? O3 Fe8 O8 96.60(11) . . ? O6 Fe8 O8 90.10(11) . . ? O3 Fe8 O27 97.26(12) . . ? O6 Fe8 O27 177.52(13) . . ? O8 Fe8 O27 88.06(13) . . ? O3 Fe8 N7 169.38(13) . . ? O6 Fe8 N7 90.88(13) . . ? O8 Fe8 N7 90.55(14) . . ? O27 Fe8 N7 90.81(14) . . ? O3 Fe8 O25 89.46(12) . . ? O6 Fe8 O25 91.77(13) . . ? O8 Fe8 O25 173.87(13) . . ? O27 Fe8 O25 90.22(15) . . ? N7 Fe8 O25 83.59(14) . . ? Fe3 O1 Fe4 113.22(13) . . ? Fe3 O1 Fe2 96.00(10) . . ? Fe4 O1 Fe2 134.29(14) . . ? Fe3 O1 Fe1 134.33(13) . . ? Fe4 O1 Fe1 96.47(10) . . ? Fe2 O1 Fe1 85.66(9) . . ? Fe6 O2 Fe5 114.03(13) . . ? Fe6 O2 Fe2 134.94(13) . . ? Fe5 O2 Fe2 96.31(10) . . ? Fe6 O2 Fe1 95.69(10) . . ? Fe5 O2 Fe1 133.68(13) . . ? Fe2 O2 Fe1 84.93(9) . . ? Fe8 O3 Fe7 115.20(11) . . ? Fe8 O3 Fe2 131.01(14) . . ? Fe7 O3 Fe2 96.44(11) . . ? Fe8 O3 Fe1 97.12(11) . . ? Fe7 O3 Fe1 131.88(13) . . ? Fe2 O3 Fe1 86.58(9) . . ? C5 N1 C1 113.6(3) . . ? C5 N1 C3 113.6(3) . . ? C1 N1 C3 113.2(3) . . ? C5 N1 Fe1 105.0(2) . . ? C1 N1 Fe1 105.4(2) . . ? C3 N1 Fe1 105.0(2) . . ? N1 C1 C2 108.7(3) . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? O4 C2 C1 107.7(3) . . ? O4 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? O4 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? C2 O4 Fe1 124.7(2) . . ? C2 O4 Fe4 123.3(2) . . ? Fe1 O4 Fe4 105.81(11) . . ? N1 C3 C4 108.2(3) . . ? N1 C3 H3A 110.1 . . ? C4 C3 H3A 110.1 . . ? N1 C3 H3B 110.1 . . ? C4 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? O5 C4 C3 108.1(3) . . ? O5 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? O5 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? C4 O5 Fe1 124.1(2) . . ? C4 O5 Fe6 124.7(2) . . ? Fe1 O5 Fe6 105.02(11) . . ? N1 C5 C6 108.5(3) . . ? N1 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? N1 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? O6 C6 C5 107.9(3) . . ? O6 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? O6 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? C6 O6 Fe1 124.9(2) . . ? C6 O6 Fe8 125.7(2) . . ? Fe1 O6 Fe8 106.05(12) . . ? C11 N2 C7 112.2(4) . . ? C11 N2 C9 111.4(4) . . ? C7 N2 C9 110.5(3) . . ? C11 N2 Fe3 113.1(3) . . ? C7 N2 Fe3 103.2(2) . . ? C9 N2 Fe3 106.0(2) . . ? N2 C7 C8 110.4(3) . . ? N2 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? N2 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? O7 C8 C7 107.9(3) . . ? O7 C8 H8A 110.1 . . ? C7 C8 H8A 110.1 . . ? O7 C8 H8B 110.1 . . ? C7 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? C8 O7 Fe2 135.4(3) . . ? C8 O7 Fe3 119.0(3) . . ? Fe2 O7 Fe3 98.98(11) . . ? N2 C9 C10 109.0(3) . . ? N2 C9 H9C 109.9 . . ? C10 C9 H9C 109.9 . . ? N2 C9 H9D 109.9 . . ? C10 C9 H9D 109.9 . . ? H9C C9 H9D 108.3 . . ? O8 C10 C9 108.2(3) . . ? O8 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? O8 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C10 O8 Fe3 111.2(2) . . ? C10 O8 Fe8 120.6(2) . . ? Fe3 O8 Fe8 128.11(14) . . ? C12B C11 N2 139.0(12) . . ? C12A C11 N2 120.4(5) . . ? C12A C11 H11A 107.2 . . ? N2 C11 H11A 107.2 . . ? C12A C11 H11B 107.2 . . ? N2 C11 H11B 107.2 . . ? H11A C11 H11B 106.9 . . ? C12B C11 H11C 102.2 . . ? C12A C11 H11C 105.2 . . ? N2 C11 H11C 102.3 . . ? C12B C11 H11D 102.6 . . ? N2 C11 H11D 102.2 . . ? H11C C11 H11D 104.8 . . ? O9A C12A C11 113.5(6) . . ? O9A C12A H12A 108.9 . . ? C11 C12A H12A 108.9 . . ? O9A C12A H12B 108.9 . . ? C11 C12A H12B 108.9 . . ? H12A C12A H12B 107.7 . . ? C12A O9A H9A 104(8) . . ? C11 C12B O9B 111.5(18) . . ? C11 C12B H12C 109.3 . . ? O9B C12B H12C 109.3 . . ? C11 C12B H12D 109.3 . . ? O9B C12B H12D 109.3 . . ? H12C C12B H12D 108.0 . . ? C17 N3 C15 112.3(3) . . ? C17 N3 C13 107.5(3) . . ? C15 N3 C13 110.4(3) . . ? C17 N3 Fe5 118.4(3) . . ? C15 N3 Fe5 105.3(2) . . ? C13 N3 Fe5 102.5(2) . . ? N3 C13 C14 110.9(3) . . ? N3 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? O10 C14 C13 107.1(3) . . ? O10 C14 H14A 110.3 . . ? C13 C14 H14A 110.3 . . ? O10 C14 H14B 110.3 . . ? C13 C14 H14B 110.3 . . ? H14A C14 H14B 108.6 . . ? C14 O10 Fe2 132.5(2) . . ? C14 O10 Fe5 119.8(2) . . ? Fe2 O10 Fe5 99.93(11) . . ? N3 C15 C16 109.8(3) . . ? N3 C15 H15A 109.7 . . ? C16 C15 H15A 109.7 . . ? N3 C15 H15B 109.7 . . ? C16 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? O11 C16 C15 107.4(3) . . ? O11 C16 H16A 110.2 . . ? C15 C16 H16A 110.2 . . ? O11 C16 H16B 110.2 . . ? C15 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? C16 O11 Fe5 112.0(2) . . ? C16 O11 Fe4 121.3(2) . . ? Fe5 O11 Fe4 126.68(12) . . ? N3 C17 C18 116.5(3) . . ? N3 C17 H17A 108.2 . . ? C18 C17 H17A 108.2 . . ? N3 C17 H17B 108.2 . . ? C18 C17 H17B 108.2 . . ? H17A C17 H17B 107.3 . . ? O12 C18 C17 111.5(4) . . ? O12 C18 H18A 109.3 . . ? C17 C18 H18A 109.3 . . ? O12 C18 H18B 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? C18 O12 H12 111(5) . . ? C23 N4 C21 110.8(3) . . ? C23 N4 C19 107.4(3) . . ? C21 N4 C19 110.9(3) . . ? C23 N4 Fe7 119.2(3) . . ? C21 N4 Fe7 106.0(2) . . ? C19 N4 Fe7 102.3(2) . . ? N4 C19 C20 110.4(3) . . ? N4 C19 H19A 109.6 . . ? C20 C19 H19A 109.6 . . ? N4 C19 H19B 109.6 . . ? C20 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? O13 C20 C19 107.3(3) . . ? O13 C20 H20A 110.3 . . ? C19 C20 H20A 110.3 . . ? O13 C20 H20B 110.3 . . ? C19 C20 H20B 110.3 . . ? H20A C20 H20B 108.5 . . ? C20 O13 Fe2 131.6(2) . . ? C20 O13 Fe7 120.7(2) . . ? Fe2 O13 Fe7 99.37(11) . . ? N4 C21 C22 109.0(3) . . ? N4 C21 H21A 109.9 . . ? C22 C21 H21A 109.9 . . ? N4 C21 H21B 109.9 . . ? C22 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? O14 C22 C21 107.0(3) . . ? O14 C22 H22A 110.3 . . ? C21 C22 H22A 110.3 . . ? O14 C22 H22B 110.3 . . ? C21 C22 H22B 110.3 . . ? H22A C22 H22B 108.6 . . ? C22 O14 Fe6 119.3(2) . . ? C22 O14 Fe7 113.9(2) . . ? Fe6 O14 Fe7 126.68(14) . . ? N4 C23 C24 113.7(3) . . ? N4 C23 H23A 108.8 . . ? C24 C23 H23A 108.8 . . ? N4 C23 H23B 108.8 . . ? C24 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? O15 C24 C23 106.9(4) . . ? O15 C24 H24A 110.3 . . ? C23 C24 H24A 110.3 . . ? O15 C24 H24B 110.3 . . ? C23 C24 H24B 110.3 . . ? H24A C24 H24B 108.6 . . ? C24 O15 H15 121(4) . . ? C25 O16 Fe3 130.0(3) . . ? C25 O17 Fe4 130.2(3) . . ? O17 C25 O16 124.2(4) . . ? O17 C25 C26 120.1(3) . . ? O16 C25 C26 115.7(3) . . ? C29 C26 C27 109.7(5) . . ? C29 C26 C25 106.5(4) . . ? C27 C26 C25 110.4(4) . . ? C29 C26 C28 110.3(5) . . ? C27 C26 C28 109.3(4) . . ? C25 C26 C28 110.6(4) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C30 O18 Fe3 127.8(3) . . ? C30 O19 Fe4 135.0(2) . . ? O18 C30 O19 123.6(3) . . ? O18 C30 C31 118.7(3) . . ? O19 C30 C31 117.6(3) . . ? C33 C31 C30 105.7(3) . . ? C33 C31 C32 110.3(4) . . ? C30 C31 C32 110.3(3) . . ? C33 C31 C34 109.4(4) . . ? C30 C31 C34 110.9(3) . . ? C32 C31 C34 110.1(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C35 O20 Fe5 132.0(2) . . ? C35 O21 Fe6 129.3(2) . . ? O21 C35 O20 124.3(3) . . ? O21 C35 C36 118.6(3) . . ? O20 C35 C36 117.0(3) . . ? C35 C36 C39 105.7(4) . . ? C35 C36 C38 110.6(4) . . ? C39 C36 C38 109.8(4) . . ? C35 C36 C37 111.3(3) . . ? C39 C36 C37 109.2(4) . . ? C38 C36 C37 110.1(4) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C40 O22 Fe5 127.9(3) . . ? C40 O23 Fe6 137.0(3) . . ? O23 C40 O22 123.5(4) . . ? O23 C40 C41 118.9(4) . . ? O22 C40 C41 117.6(3) . . ? C40 C41 C44 110.7(4) . . ? C40 C41 C42 110.0(4) . . ? C44 C41 C42 109.1(5) . . ? C40 C41 C43 106.4(4) . . ? C44 C41 C43 110.8(5) . . ? C42 C41 C43 109.8(4) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C45 O24 Fe7 128.6(3) . . ? C45 O25 Fe8 136.9(3) . . ? O25 C45 O24 124.4(4) . . ? O25 C45 C46 117.3(4) . . ? O24 C45 C46 118.2(4) . . ? C48B C46 C49B 128(2) . . ? C48A C46 C47A 113.6(5) . . ? C48B C46 C45 110.0(13) . . ? C49B C46 C45 112.4(15) . . ? C48A C46 C45 113.4(5) . . ? C47A C46 C45 108.6(4) . . ? C48A C46 C49A 108.7(5) . . ? C47A C46 C49A 105.6(5) . . ? C45 C46 C49A 106.5(5) . . ? C48B C46 C47B 99.9(16) . . ? C49B C46 C47B 102.0(18) . . ? C45 C46 C47B 99.2(8) . . ? C46 C47A H47D 109.5 . . ? C46 C47A H47E 109.5 . . ? H47D C47A H47E 109.5 . . ? C46 C47A H47F 109.5 . . ? H47D C47A H47F 109.5 . . ? H47E C47A H47F 109.5 . . ? C46 C48A H48A 109.5 . . ? C46 C48A H48B 109.5 . . ? H48A C48A H48B 109.5 . . ? C46 C48A H48C 109.5 . . ? H48A C48A H48C 109.5 . . ? H48B C48A H48C 109.5 . . ? C46 C49A H49A 109.5 . . ? C46 C49A H49B 109.5 . . ? H49A C49A H49B 109.5 . . ? C46 C49A H49C 109.5 . . ? H49A C49A H49C 109.5 . . ? H49B C49A H49C 109.5 . . ? C46 C47B H47A 109.5 . . ? C46 C47B H47B 109.5 . . ? H47A C47B H47B 109.5 . . ? C46 C47B H47C 109.5 . . ? H47A C47B H47C 109.5 . . ? H47B C47B H47C 109.5 . . ? C46 C48B H48D 109.5 . . ? C46 C48B H48E 109.5 . . ? H48D C48B H48E 109.5 . . ? C46 C48B H48F 109.5 . . ? H48D C48B H48F 109.5 . . ? H48E C48B H48F 109.5 . . ? C46 C49B H49D 109.5 . . ? C46 C49B H49E 109.5 . . ? H49D C49B H49E 109.5 . . ? C46 C49B H49F 109.5 . . ? H49D C49B H49F 109.5 . . ? H49E C49B H49F 109.5 . . ? C50 O26 Fe7 129.9(3) . . ? C50 O27 Fe8 136.6(3) . . ? O26 C50 O27 124.6(4) . . ? O26 C50 C51 119.0(4) . . ? O27 C50 C51 116.4(4) . . ? C54 C51 C50 109.5(4) . . ? C54 C51 C53 110.6(5) . . ? C50 C51 C53 111.6(4) . . ? C54 C51 C52 110.2(6) . . ? C50 C51 C52 106.8(4) . . ? C53 C51 C52 108.1(5) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C61 N5 Fe4 162.6(4) . . ? N5 C61 S1 179.2(6) . . ? C62 N6 Fe6 148.9(4) . . ? N6 C62 S2 179.0(5) . . ? C63 N7 Fe8 171.2(4) . . ? N7 C63 S3 179.3(5) . . ? N71 C71 C72 178.0(9) . . ? N73 C73 C74 130.2(19) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9A H9A S1 0.90(4) 2.45(4) 3.244(6) 147(7) 4_556 O12 H12 O15 0.93(4) 1.90(5) 2.760(6) 153(7) 1_545 O15 H15 N71 1.01(4) 1.89(4) 2.843(7) 155(5) . _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.738 _refine_diff_density_min -0.813 _refine_diff_density_rms 0.117 ########################################################################### data_232blue _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H48 N2 Ni O10' _chemical_formula_weight 559.33 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 12.9960(14) _cell_length_b 6.9495(7) _cell_length_c 16.1600(17) _cell_angle_alpha 90.00 _cell_angle_beta 102.368(2) _cell_angle_gamma 90.00 _cell_volume 1425.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3348 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.71 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 0.732 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.736 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6904 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.99 _reflns_number_total 3196 _reflns_number_gt 2386 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_data_reduction 'SAINT+ 6.0 (Bruker AXS Inc., 2000)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _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^)+(0.0283P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3196 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0649 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.000 _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 Ni1 Ni 0.5000 0.5000 0.5000 0.01471(9) Uani 1 2 d S . . N1 N 0.35673(10) 0.35014(18) 0.46369(8) 0.0160(3) Uani 1 1 d . . . C1 C 0.27692(12) 0.4666(2) 0.49564(10) 0.0185(4) Uani 1 1 d . . . H1A H 0.2764 0.4287 0.5546 0.022 Uiso 1 1 calc R . . H1B H 0.2060 0.4422 0.4602 0.022 Uiso 1 1 calc R . . C2 C 0.30312(12) 0.6780(2) 0.49274(10) 0.0189(4) Uani 1 1 d . . . H2A H 0.2954 0.7197 0.4332 0.023 Uiso 1 1 calc R . . H2B H 0.2539 0.7545 0.5186 0.023 Uiso 1 1 calc R . . O1 O 0.40943(8) 0.70986(15) 0.53822(7) 0.0170(3) Uani 1 1 d . . . H1 H 0.4086(15) 0.712(3) 0.5960(13) 0.048(6) Uiso 1 1 d . . . C3 C 0.37682(12) 0.1631(2) 0.50872(10) 0.0190(4) Uani 1 1 d . . . H3A H 0.4221 0.0825 0.4807 0.023 Uiso 1 1 calc R . . H3B H 0.3092 0.0947 0.5051 0.023 Uiso 1 1 calc R . . C4 C 0.43010(12) 0.1908(2) 0.60115(10) 0.0214(4) Uani 1 1 d . . . H4A H 0.3771 0.2291 0.6338 0.026 Uiso 1 1 calc R . . H4B H 0.4623 0.0680 0.6247 0.026 Uiso 1 1 calc R . . O2 O 0.51042(8) 0.33740(16) 0.60886(7) 0.0179(3) Uani 1 1 d . . . H2 H 0.5093(15) 0.398(3) 0.6549(13) 0.041(6) Uiso 1 1 d . . . C5 C 0.32810(12) 0.3230(2) 0.37038(10) 0.0201(4) Uani 1 1 d . . . H5A H 0.3925 0.2830 0.3515 0.024 Uiso 1 1 calc R . . H5B H 0.3072 0.4501 0.3444 0.024 Uiso 1 1 calc R . . C6 C 0.24193(12) 0.1815(3) 0.33417(11) 0.0248(4) Uani 1 1 d . . . H6A H 0.2354 0.1714 0.2722 0.030 Uiso 1 1 calc R . . H6B H 0.2606 0.0528 0.3592 0.030 Uiso 1 1 calc R . . O3 O 0.14416(10) 0.2409(2) 0.35138(9) 0.0376(4) Uani 1 1 d . . . H3 H 0.1006(15) 0.174(3) 0.3287(13) 0.037(7) Uiso 1 1 d . . . O4 O 0.50203(8) 0.49979(17) 0.75016(7) 0.0232(3) Uani 1 1 d . . . O5 O 0.39781(9) 0.73851(18) 0.69094(7) 0.0292(3) Uani 1 1 d . . . C7 C 0.44617(12) 0.6475(2) 0.75439(10) 0.0193(4) Uani 1 1 d . . . C8 C 0.43662(12) 0.7187(2) 0.84247(10) 0.0220(4) Uani 1 1 d . . . C9 C 0.38034(15) 0.9130(3) 0.83603(12) 0.0357(5) Uani 1 1 d . . . H9A H 0.3747 0.9556 0.8927 0.054 Uiso 1 1 calc R . . H9B H 0.3097 0.9001 0.8001 0.054 Uiso 1 1 calc R . . H9C H 0.4206 1.0079 0.8111 0.054 Uiso 1 1 calc R . . C10 C 0.37640(15) 0.5671(3) 0.88190(12) 0.0336(5) Uani 1 1 d . . . H10A H 0.3697 0.6100 0.9383 0.050 Uiso 1 1 calc R . . H10B H 0.4148 0.4449 0.8868 0.050 Uiso 1 1 calc R . . H10C H 0.3061 0.5495 0.8459 0.050 Uiso 1 1 calc R . . C11 C 0.54804(14) 0.7414(3) 0.89714(11) 0.0352(5) Uani 1 1 d . . . H11A H 0.5436 0.7859 0.9538 0.053 Uiso 1 1 calc R . . H11B H 0.5872 0.8358 0.8709 0.053 Uiso 1 1 calc R . . H11C H 0.5845 0.6172 0.9016 0.053 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 Ni1 0.01396(14) 0.01421(15) 0.01564(15) 0.00073(13) 0.00244(10) -0.00070(13) N1 0.0156(7) 0.0146(7) 0.0172(7) 0.0001(6) 0.0022(5) -0.0002(5) C1 0.0141(7) 0.0216(10) 0.0199(8) -0.0003(7) 0.0035(6) -0.0004(6) C2 0.0141(8) 0.0190(9) 0.0215(9) -0.0010(7) -0.0006(7) 0.0006(7) O1 0.0144(6) 0.0176(6) 0.0181(6) -0.0010(5) 0.0012(5) -0.0010(5) C3 0.0180(8) 0.0148(8) 0.0241(9) 0.0020(7) 0.0045(7) -0.0024(7) C4 0.0200(9) 0.0189(9) 0.0256(9) 0.0035(7) 0.0053(7) -0.0030(7) O2 0.0196(6) 0.0170(6) 0.0172(6) 0.0008(5) 0.0038(5) -0.0018(5) C5 0.0210(8) 0.0195(9) 0.0192(9) -0.0004(7) 0.0030(7) -0.0018(7) C6 0.0230(9) 0.0270(10) 0.0229(9) -0.0035(7) 0.0015(7) -0.0031(8) O3 0.0200(7) 0.0439(9) 0.0468(9) -0.0201(7) 0.0020(6) -0.0094(7) O4 0.0241(6) 0.0271(6) 0.0175(6) 0.0002(6) 0.0025(5) 0.0079(6) O5 0.0336(7) 0.0356(8) 0.0175(6) 0.0033(5) 0.0034(5) 0.0130(6) C7 0.0135(8) 0.0258(9) 0.0184(9) 0.0001(7) 0.0027(7) -0.0043(7) C8 0.0191(9) 0.0279(10) 0.0193(9) -0.0006(7) 0.0052(7) 0.0010(7) C9 0.0455(12) 0.0374(11) 0.0277(11) -0.0021(9) 0.0156(9) 0.0103(10) C10 0.0361(11) 0.0426(12) 0.0254(10) 0.0013(9) 0.0140(9) -0.0046(9) C11 0.0275(10) 0.0513(13) 0.0247(10) -0.0120(9) 0.0008(8) -0.0032(9) _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 Ni1 O1 2.0507(11) 3_666 ? Ni1 O1 2.0507(11) . ? Ni1 O2 2.0706(11) 3_666 ? Ni1 O2 2.0707(11) . ? Ni1 N1 2.1042(12) 3_666 ? Ni1 N1 2.1043(12) . ? N1 C3 1.4850(19) . ? N1 C5 1.486(2) . ? N1 C1 1.4924(19) . ? C1 C2 1.511(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O1 1.4362(18) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O1 H1 0.94(2) . ? C3 C4 1.518(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O2 1.4450(18) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O2 H2 0.86(2) . ? C5 C6 1.511(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O3 1.419(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O3 H3 0.764(19) . ? O4 C7 1.2678(19) . ? O5 C7 1.2529(19) . ? C7 C8 1.537(2) . ? C8 C9 1.529(2) . ? C8 C10 1.530(2) . ? C8 C11 1.534(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? 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 O1 Ni1 O1 180.0 3_666 . ? O1 Ni1 O2 93.99(5) 3_666 3_666 ? O1 Ni1 O2 86.01(5) . 3_666 ? O1 Ni1 O2 86.01(4) 3_666 . ? O1 Ni1 O2 93.99(5) . . ? O2 Ni1 O2 180.00(6) 3_666 . ? O1 Ni1 N1 84.56(4) 3_666 3_666 ? O1 Ni1 N1 95.44(4) . 3_666 ? O2 Ni1 N1 81.94(5) 3_666 3_666 ? O2 Ni1 N1 98.06(5) . 3_666 ? O1 Ni1 N1 95.44(4) 3_666 . ? O1 Ni1 N1 84.56(4) . . ? O2 Ni1 N1 98.06(5) 3_666 . ? O2 Ni1 N1 81.94(5) . . ? N1 Ni1 N1 180.0 3_666 . ? C3 N1 C5 111.46(12) . . ? C3 N1 C1 111.56(12) . . ? C5 N1 C1 112.24(12) . . ? C3 N1 Ni1 104.14(9) . . ? C5 N1 Ni1 111.10(9) . . ? C1 N1 Ni1 105.91(9) . . ? N1 C1 C2 109.80(12) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? O1 C2 C1 109.43(12) . . ? O1 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? O1 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? C2 O1 Ni1 106.71(9) . . ? C2 O1 H1 107.3(12) . . ? Ni1 O1 H1 116.4(12) . . ? N1 C3 C4 111.52(13) . . ? N1 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? N1 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? O2 C4 C3 110.05(13) . . ? O2 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? O2 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C4 O2 Ni1 113.39(9) . . ? C4 O2 H2 105.9(13) . . ? Ni1 O2 H2 117.4(14) . . ? N1 C5 C6 118.63(13) . . ? N1 C5 H5A 107.7 . . ? C6 C5 H5A 107.7 . . ? N1 C5 H5B 107.7 . . ? C6 C5 H5B 107.7 . . ? H5A C5 H5B 107.1 . . ? O3 C6 C5 110.80(14) . . ? O3 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? O3 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C6 O3 H3 109.3(15) . . ? O5 C7 O4 123.87(15) . . ? O5 C7 C8 118.02(15) . . ? O4 C7 C8 118.11(14) . . ? C9 C8 C10 110.89(14) . . ? C9 C8 C11 109.08(15) . . ? C10 C8 C11 109.58(15) . . ? C9 C8 C7 110.70(14) . . ? C10 C8 C7 108.32(14) . . ? C11 C8 C7 108.23(13) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O5 0.94(2) 1.58(2) 2.5125(16) 173.1(19) . O2 H2 O4 0.86(2) 1.72(2) 2.5703(16) 175(2) . O3 H3 O4 0.764(19) 2.00(2) 2.7553(17) 169(2) 4_565 _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.558 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.058