# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2139 ############################################################################## # IUMSC CIF Archive file # ############################################################################## data_MSC98127 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C22 H20 B2 F8 N4' _chemical_formula_moiety ? _chemical_formula_weight 514.037 _cell_length_a 9.341(7) _cell_length_b 11.460(14) _cell_length_c 5.383(6) _cell_angle_alpha 95.73(10) _cell_angle_beta 105.82(11) _cell_angle_gamma 90.06(5) _cell_volume 551.4(11) _cell_formula_units_Z 1 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 9.73 _cell_measurement_theta_max 10.47 _cell_measurement_temperature 173. _exptl_crystal_colour colorless _exptl_crystal_description irregular _exptl_crystal_size_max .30 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .25 _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 262 _exptl_absorpt_coefficient_mu 0.1394 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 173. _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4434 _diffrn_reflns_av_R_equivalents 0.097 _diffrn_reflns_theta_min 3.57475 _diffrn_reflns_theta_max 24.9983 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_standards_number 4 _diffrn_standards_decay_% 19.8 _diffrn_standards_interval_count 500 _reflns_number_total 1943 _reflns_number_gt 1016 _reflns_threshold_expression F^2^>2.33\s(F^2^) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source F F 0.014 0.01 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' B B 0 0.001 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 866 _refine_ls_number_parameters 164 _refine_ls_hydrogen_treatment ? _refine_ls_extinction_coef -0.000011(3) _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.07F)^2^ _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.0719 _refine_ls_goodness_of_fit_ref 1.6417 _refine_ls_shift/su_max 0.078 _refine_diff_density_max 0.38 _refine_diff_density_min -0.47 _computing_data_collection 'NPS, local program' _computing_cell_refinement 'XTEL, local package' _computing_data_reduction 'XTEL, local package' _computing_structure_solution MULTAN78 _computing_structure_refinement 'XTEL, local package' _computing_molecular_graphics 'XTEL, local package' _computing_publication_material 'XTEL, local package' 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_disorder_group _atom_site_disorder_assembly B1 B 0.2303(7) 0.6797(7) 0.1845(13) 0.050(3) Uani 1 0 . F2 F 0.1107(3) 0.6051(3) 0.1450(6) 0.0603(15) Uani 1 0 . F3 F 0.3441(3) 0.6254(3) 0.1020(6) 0.0541(13) Uani 1 0 . F4 F 0.2841(4) 0.7220(4) 0.4443(6) 0.0663(15) Uani 1 0 . F5 F 0.1867(4) 0.7775(3) 0.0426(7) 0.0671(15) Uani 1 0 . C6 C 0.9465(7) 1.0295(5) 0.3974(12) 0.056(3) Uani 1 0 . C7 C 0.8115(6) 0.9527(5) 0.2605(11) 0.044(2) Uani 1 0 . C8 C 0.6765(7) 0.9644(6) 0.3216(12) 0.053(3) Uani 1 0 . C9 C 0.5574(7) 0.8922(6) 0.1860(12) 0.054(3) Uani 1 0 . C10 C 0.5740(6) 0.8094(5) -0.0104(11) 0.044(2) Uani 1 0 . C11 C 0.7120(6) 0.8031(5) -0.0552(10) 0.036(2) Uani 1 0 . N12 N 0.8285(5) 0.8716(4) 0.0756(9) 0.0393(17) Uani 1 0 . C13 C 0.7435(5) 0.7176(4) -0.2598(9) 0.0332(19) Uani 1 0 . C14 C 0.6417(6) 0.6471(5) -0.4439(11) 0.043(2) Uani 1 0 . C15 C 0.6856(6) 0.5764(5) -0.6356(10) 0.045(2) Uani 1 0 . C16 C 0.8325(6) 0.5814(5) -0.6404(11) 0.041(2) Uani 1 0 . C17 C 0.9328(6) 0.6513(5) -0.4529(11) 0.042(2) Uani 1 0 . N18 N 0.8868(4) 0.7172(4) -0.2690(8) 0.0359(17) Uani 1 0 . H1 H 0.9818 1.0488 0.2561 0.0783 Uiso 1 0 . H2 H 0.9028 1.0955 0.468 0.0502 Uiso 1 0 . H3 H 0.667 1.0205 0.4576 0.0788 Uiso 1 0 . H4 H 0.4642 0.8996 0.2245 0.0802 Uiso 1 0 . H5 H 0.4959 0.7563 -0.1071 0.0682 Uiso 1 0 . H6 H 0.5408 0.6475 -0.4397 0.0669 Uiso 1 0 . H7 H 0.6181 0.5225 -0.7568 0.0702 Uiso 1 0 . H8 H 0.8599 0.5377 -0.779 0.0692 Uiso 1 0 . H9 H 1.035 0.6522 -0.4489 0.0653 Uiso 1 0 . H10 H 0.9579 0.7662 -0.1415 0.0626 Uiso 1 0 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 B1 0.031(6) 0.08(3) 0.042(5) 0.021(4) 0.021(3) 0.023(4) F2 0.041(7) 0.08(3) 0.062(5) 0.0080(19) 0.0213(16) 0.016(2) F3 0.037(6) 0.07(2) 0.057(4) 0.0191(17) 0.0188(15) -0.0045(19) F4 0.049(8) 0.11(4) 0.040(3) 0.024(2) 0.0046(16) -0.009(2) F5 0.057(9) 0.07(2) 0.072(5) 0.020(2) 0.0100(17) 0.025(2) C6 0.060(10) 0.050(17) 0.054(5) 0.021(4) 0.007(3) 0.005(4) C7 0.043(8) 0.037(13) 0.047(5) 0.011(3) 0.004(3) 0.010(3) C8 0.058(10) 0.056(19) 0.051(5) 0.017(4) 0.022(3) 0.002(4) C9 0.047(8) 0.07(2) 0.055(5) 0.012(4) 0.026(3) 0.003(4) C10 0.040(7) 0.046(15) 0.048(5) -0.001(3) 0.017(3) 0.006(3) C11 0.033(6) 0.039(13) 0.034(4) 0.011(3) 0.004(3) 0.013(3) N12 0.034(6) 0.036(12) 0.046(4) 0.014(2) 0.007(2) 0.004(3) C13 0.030(5) 0.036(12) 0.030(4) 0.013(3) 0.001(2) 0.005(3) C14 0.037(7) 0.050(17) 0.043(5) 0.019(3) 0.008(3) 0.005(3) C15 0.048(8) 0.040(14) 0.041(4) 0.010(3) 0.002(3) -0.001(3) C16 0.041(7) 0.043(15) 0.041(4) 0.018(3) 0.011(3) 0.009(3) C17 0.041(7) 0.043(14) 0.044(5) 0.019(3) 0.012(3) 0.011(3) N18 0.034(6) 0.034(12) 0.038(4) 0.013(2) 0.007(2) 0.007(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag F2 B1 1.366(9) . . no F3 B1 1.384(6) . . no F4 B1 1.387(8) . . no F5 B1 1.417(7) . . no N12 C7 1.337(7) . . no N12 C11 1.331(7) . . no N18 C13 1.351(6) . . no N18 C17 1.349(6) . . no C6 C6 1.497(10) . 2_776 no C6 C7 1.509(9) . . no C7 C8 1.388(8) . . no C8 C9 1.372(9) . . no C9 C10 1.393(8) . . no C10 C11 1.374(7) . . no C11 C13 1.492(7) . . no C13 C14 1.366(8) . . no C14 C15 1.396(8) . . no C15 C16 1.380(8) . . no C16 C17 1.362(8) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 N12 C11 118.5(5) . . . no C13 N18 C17 122.9(5) . . . no C6 C6 C7 111.7(7) 2_776 . . no N12 C7 C6 116.1(5) . . . no N12 C7 C8 121.2(6) . . . no C6 C7 C8 122.7(5) . . . no C7 C8 C9 119.7(6) . . . no C8 C9 C10 119.2(5) . . . no C9 C10 C11 117.2(6) . . . no N12 C11 C10 124.1(5) . . . no N12 C11 C13 113.7(4) . . . no C10 C11 C13 122.2(5) . . . no N18 C13 C11 115.1(5) . . . no N18 C13 C14 118.3(5) . . . no C11 C13 C14 126.5(5) . . . no C13 C14 C15 120.4(5) . . . no C14 C15 C16 119.2(6) . . . no C15 C16 C17 119.5(5) . . . no N18 C17 C16 119.8(5) . . . no F2 B1 F3 111.2(6) . . . no F2 B1 F4 111.3(5) . . . no F2 B1 F5 109.2(5) . . . no F3 B1 F4 109.1(5) . . . no F3 B1 F5 108.4(5) . . . no F4 B1 F5 107.5(6) . . . no #===END ############################################################################## # IUMSC CIF Archive file # ############################################################################## data_MSC98075 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C41 H35.5 Cl2 Fe2 N6.5 O5' _chemical_formula_moiety 'C36 H28 Cl2 Fe2 N4 O5, 2.5(C2 H3 N)' _chemical_formula_weight 881.87 _cell_length_a 11.459(6) _cell_length_b 16.457(8) _cell_length_c 11.376(6) _cell_angle_alpha 92.36(3) _cell_angle_beta 105.11(3) _cell_angle_gamma 74.40(3) _cell_volume 1993.9(18) _cell_formula_units_Z 2 _cell_measurement_reflns_used 66 _cell_measurement_theta_min 11.18 _cell_measurement_theta_max 15.84 _cell_measurement_temperature 108 _exptl_crystal_colour green _exptl_crystal_description 'triangular plate' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 906 _exptl_absorpt_coefficient_mu 0.9139 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _diffrn_crystal_treatment ; The sample consisted of transparent green crystals in the mother liquor of MeCN. The crystals had formed by cooling the solution in the freezer and had a tendency to redissolve in the mother liquor when warmed to room temperature. The first two data collection attempts came to a premature end due to ice problems. A third crystal was not diffracting well and finally a triangular shaped crystal was selected and mounted using a nylon loop and a lot of silicone grease. ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 108 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16730 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_theta_min 3.01717 _diffrn_reflns_theta_max 25.1048 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 4 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 300 _reflns_number_total 7057 _reflns_number_gt 5457 _reflns_threshold_expression F>3.0\s(F) _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogen geom loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.301 0.845 'International Tables Vol. IV (1974) Table 2.2B' Cl Cl 0.132 0.159 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_special_details ; The structure was solved by a combination of direct methods (SHELXS86) and Fourier techniques. The positions of the two iron atoms and some additional non-hydrogen atoms were obtained from the initial best solution. The remainder of the non-hydrogen atoms were located in several iterations of a least-squares refinemnet followed by a difference Fourier calculation. The asymmetric unit was found to contain the Fe-dimer complex as well as two and a half molecules of acetonitrile solvent from the crystallization. Two of the acetonitrile molecules were well behaved and the half molecule was modelled as three half weight carbon atoms near a center of inversion. Many hydrogen atoms were located, all were introduced in fixed idealized positions with individual isotropic thermal parameters equal to 1.0 plus the isotropic equivalent of the parent atom. The final least-squares refinement was carried out using anisotropic thermal parameters on the non-hydrogen atoms, except for the disordered solvent. The final R(F) was 0.0448 for 509 total variables and the full unique data set. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 7057 _refine_ls_number_parameters 509 _refine_ls_hydrogen_treatment ? _refine_ls_extinction_coef -0.00000046(9) _refine_ls_extinction_method Zachariasen _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.07F)^2^ _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.0457 _refine_ls_goodness_of_fit_ref 1.0395 _refine_ls_shift/su_max 0.0027 _refine_diff_density_max 0.86 _refine_diff_density_min -0.56 _computing_data_collection 'NPS, local program' _computing_cell_refinement 'XTEL, local package' _computing_data_reduction 'XTEL, local package' _computing_structure_solution SHELXS86 _computing_structure_refinement 'XTEL, local package' _computing_molecular_graphics 'XTEL, local package' _computing_publication_material 'XTEL, local package' 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_disorder_group _atom_site_disorder_assembly Fe1 Fe 0.13732(5) 0.16190(3) 0.33672(5) 0.02176(19) Uani 1 0 . Fe2 Fe 0.29647(5) 0.22310(3) 0.18632(5) 0.01939(19) Uani 1 0 . O3 O 0.2146(2) 0.15226(15) 0.2184(2) 0.0214(9) Uani 1 0 . Cl4 Cl -0.05255(8) 0.13324(6) 0.22738(9) 0.0309(3) Uani 1 0 . Cl5 Cl 0.24562(8) 0.20622(6) -0.02830(8) 0.0241(3) Uani 1 0 . O6 O 0.0626(2) 0.29086(15) 0.3141(2) 0.0267(10) Uani 1 0 . C7 C 0.0728(3) 0.3431(2) 0.2408(3) 0.0219(13) Uani 1 0 . O8 O 0.1554(2) 0.32983(15) 0.1816(2) 0.0237(9) Uani 1 0 . C9 C -0.0208(3) 0.4278(2) 0.2217(3) 0.0232(13) Uani 1 0 . C10 C -0.0075(4) 0.4899(2) 0.1511(4) 0.0263(14) Uani 1 0 . C11 C -0.0926(4) 0.5684(2) 0.1327(4) 0.0339(16) Uani 1 0 . C12 C -0.1935(4) 0.5860(3) 0.1838(4) 0.0393(18) Uani 1 0 . C13 C -0.2087(4) 0.5242(3) 0.2534(4) 0.0416(18) Uani 1 0 . C14 C -0.1228(4) 0.4453(3) 0.2736(4) 0.0346(16) Uani 1 0 . O15 O 0.2854(2) 0.18391(17) 0.4713(2) 0.0337(10) Uani 1 0 . C16 C 0.3505(3) 0.2332(2) 0.4621(3) 0.0235(13) Uani 1 0 . O17 O 0.3644(2) 0.25763(16) 0.3642(2) 0.0274(10) Uani 1 0 . C18 C 0.4163(3) 0.2652(2) 0.5794(3) 0.0213(13) Uani 1 0 . C19 C 0.4041(3) 0.2394(2) 0.6894(3) 0.0253(14) Uani 1 0 . C20 C 0.4691(4) 0.2645(3) 0.7984(3) 0.0296(14) Uani 1 0 . C21 C 0.5462(4) 0.3175(3) 0.7970(4) 0.0334(15) Uani 1 0 . C22 C 0.5566(4) 0.3444(3) 0.6874(4) 0.0343(15) Uani 1 0 . C23 C 0.4924(4) 0.3180(2) 0.5780(3) 0.0285(14) Uani 1 0 . N24 N 0.0688(3) 0.1639(2) 0.4977(3) 0.0303(12) Uani 1 0 . C25 C 0.0080(5) 0.2342(3) 0.5425(4) 0.0420(18) Uani 1 0 . C26 C -0.0247(5) 0.2351(3) 0.6508(4) 0.050(2) Uani 1 0 . C27 C 0.0055(5) 0.1592(4) 0.7144(4) 0.056(2) Uani 1 0 . C28 C 0.0669(4) 0.0866(3) 0.6699(4) 0.0424(17) Uani 1 0 . C29 C 0.0997(4) 0.0904(3) 0.5606(3) 0.0321(14) Uani 1 0 . C30 C 0.1709(3) 0.0153(3) 0.5087(3) 0.0317(14) Uani 1 0 . C31 C 0.1970(4) -0.0657(3) 0.5585(4) 0.0402(16) Uani 1 0 . C32 C 0.2626(4) -0.1335(3) 0.5057(4) 0.0439(17) Uani 1 0 . C33 C 0.3031(4) -0.1197(3) 0.4060(4) 0.0400(17) Uani 1 0 . C34 C 0.2794(4) -0.0374(2) 0.3621(4) 0.0323(15) Uani 1 0 . N35 N 0.2118(3) 0.02922(19) 0.4112(3) 0.0264(11) Uani 1 0 . C36 C 0.3386(4) -0.0222(2) 0.2635(4) 0.0303(15) Uani 1 0 . C37 C 0.4476(3) 0.0165(2) 0.3183(4) 0.0295(14) Uani 1 0 . N38 N 0.4827(3) 0.12785(19) 0.2055(3) 0.0217(11) Uani 1 0 . C39 C 0.5067(3) 0.0440(2) 0.2279(3) 0.0249(13) Uani 1 0 . C40 C 0.5897(3) -0.0138(2) 0.1762(4) 0.0282(14) Uani 1 0 . C41 C 0.6542(4) 0.0138(2) 0.1052(4) 0.0281(14) Uani 1 0 . C42 C 0.6398(3) 0.0991(2) 0.0942(3) 0.0269(14) Uani 1 0 . C43 C 0.5535(3) 0.1547(2) 0.1448(3) 0.0236(13) Uani 1 0 . C44 C 0.5328(3) 0.2475(2) 0.1399(3) 0.0217(13) Uani 1 0 . C45 C 0.6242(3) 0.2850(2) 0.1267(3) 0.0278(14) Uani 1 0 . C46 C 0.5965(4) 0.3721(3) 0.1234(4) 0.0342(15) Uani 1 0 . C47 C 0.4800(4) 0.4196(2) 0.1321(4) 0.0322(15) Uani 1 0 . C48 C 0.3941(4) 0.3781(2) 0.1466(3) 0.0265(14) Uani 1 0 . N49 N 0.4201(3) 0.29382(19) 0.1521(3) 0.0220(11) Uani 1 0 . C50 C -0.0949(4) 0.2770(3) -0.0129(4) 0.0431(17) Uani 1 0 . C51 C -0.1615(4) 0.3584(3) -0.0749(4) 0.0326(16) Uani 1 0 . N52 N -0.2154(4) 0.4207(3) -0.1232(4) 0.0577(18) Uani 1 0 . C53 C 0.7610(8) 0.5088(4) 0.5841(5) 0.097(3) Uani 1 0 . C54 C 0.7125(6) 0.4485(5) 0.5100(5) 0.078(3) Uani 1 0 . N55 N 0.6777(8) 0.3999(6) 0.4511(6) 0.183(5) Uani 1 0 . C56 C 0.1487(10) -0.0983(6) 0.0965(9) 0.048(2) Uiso 0.5 0 . C57 C 0.0667(11) -0.0433(7) 0.0436(10) 0.058(3) Uiso 0.5 0 . C58 C -0.0483(17) -0.0474(11) 0.0081(16) 0.112(6) Uiso 0.5 0 . H1 H 0.0613 0.4776 0.1131 0.0388 Uiso 1 0 . H2 H -0.081 0.6115 0.0839 0.0439 Uiso 1 0 . H3 H -0.2552 0.6406 0.1714 0.0508 Uiso 1 0 . H4 H -0.2759 0.5366 0.2913 0.0543 Uiso 1 0 . H5 H -0.1333 0.4021 0.3214 0.0457 Uiso 1 0 . H6 H 0.3528 0.2021 0.6885 0.0348 Uiso 1 0 . H7 H 0.4604 0.2447 0.8746 0.0391 Uiso 1 0 . H8 H 0.5907 0.3361 0.8728 0.0434 Uiso 1 0 . H9 H 0.6066 0.3823 0.6871 0.0434 Uiso 1 0 . H10 H 0.5022 0.3343 0.5018 0.039 Uiso 1 0 . H11 H -0.0144 0.2869 0.496 0.0523 Uiso 1 0 . H12 H -0.0681 0.2878 0.68 0.061 Uiso 1 0 . H13 H -0.018 0.1569 0.7884 0.0677 Uiso 1 0 . H14 H 0.0908 0.0333 0.714 0.05 Uiso 1 0 . H15 H 0.1654 -0.0746 0.6288 0.0478 Uiso 1 0 . H16 H 0.2793 -0.19 0.5363 0.0481 Uiso 1 0 . H17 H 0.3495 -0.1663 0.3691 0.0491 Uiso 1 0 . H18 H 0.3685 -0.0749 0.2258 0.0413 Uiso 1 0 . H19 H 0.2774 0.0152 0.2007 0.0413 Uiso 1 0 . H20 H 0.4184 0.0639 0.364 0.0396 Uiso 1 0 . H21 H 0.5121 -0.0251 0.3733 0.0396 Uiso 1 0 . H22 H 0.603 -0.0734 0.1896 0.0398 Uiso 1 0 . H23 H 0.7068 -0.0265 0.0651 0.0406 Uiso 1 0 . H24 H 0.6885 0.1198 0.0522 0.036 Uiso 1 0 . H25 H 0.7033 0.251 0.1172 0.0396 Uiso 1 0 . H26 H 0.6586 0.399 0.1191 0.0414 Uiso 1 0 . H27 H 0.4565 0.4804 0.1266 0.0393 Uiso 1 0 . H28 H 0.3132 0.4108 0.1526 0.0393 Uiso 1 0 . H29 H -0.0979 0.2786 0.0691 0.0502 Uiso 1 0 . H30 H -0.1291 0.2335 -0.0531 0.0502 Uiso 1 0 . H31 H -0.0074 0.2631 -0.0152 0.0502 Uiso 1 0 . H32 H 0.8519 0.4953 0.6015 0.0972 Uiso 1 0 . H33 H 0.741 0.5117 0.6618 0.0972 Uiso 1 0 . H34 H 0.7282 0.5639 0.5466 0.0972 Uiso 1 0 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.017(2) 0.020(5) 0.021(3) -0.0070(2) 0.0049(2) 0.0047(2) Fe2 0.0151(19) 0.018(5) 0.020(2) -0.0043(2) 0.0049(2) 0.0041(2) O3 0.016(2) 0.019(5) 0.024(3) -0.0062(10) 0.0044(11) 0.0029(11) Cl4 0.018(2) 0.033(8) 0.028(3) -0.0094(4) 0.0014(4) 0.0110(4) Cl5 0.022(3) 0.024(6) 0.021(3) -0.0047(4) 0.0042(4) 0.0016(4) O6 0.029(4) 0.021(5) 0.028(4) -0.0044(12) 0.0161(12) 0.0044(11) C7 0.021(3) 0.021(6) 0.021(3) -0.0101(16) 0.0075(16) -0.0018(15) O8 0.021(3) 0.019(5) 0.026(3) -0.0032(11) 0.0084(12) 0.0051(11) C9 0.022(3) 0.022(6) 0.023(3) -0.0080(16) 0.0076(16) -0.0016(15) C10 0.025(4) 0.024(6) 0.028(4) -0.0051(16) 0.0098(17) 0.0004(16) C11 0.036(5) 0.020(6) 0.039(5) -0.0027(18) 0.014(2) 0.0070(18) C12 0.039(6) 0.027(7) 0.048(6) 0.005(2) 0.017(2) 0.005(2) C13 0.037(5) 0.040(11) 0.052(7) 0.002(2) 0.030(2) 0.000(2) C14 0.033(5) 0.029(8) 0.039(5) -0.0079(19) 0.016(2) 0.0018(19) O15 0.031(4) 0.036(9) 0.022(3) -0.0216(13) 0.0025(12) 0.0050(12) C16 0.021(3) 0.024(6) 0.021(3) -0.0033(16) 0.0053(16) 0.0015(15) O17 0.029(4) 0.028(7) 0.020(3) -0.0146(12) 0.0079(12) 0.0005(11) C18 0.018(3) 0.019(5) 0.021(3) -0.0018(15) 0.0028(15) 0.0021(15) C19 0.020(3) 0.023(6) 0.027(4) -0.0042(16) 0.0049(16) 0.0031(16) C20 0.027(4) 0.033(9) 0.020(3) -0.0057(18) 0.0056(17) 0.0049(17) C21 0.030(4) 0.040(10) 0.025(4) -0.0141(19) 0.0048(18) -0.0044(18) C22 0.030(4) 0.035(9) 0.032(5) -0.0169(19) 0.0071(19) -0.0032(18) C23 0.027(4) 0.028(7) 0.023(3) -0.0092(17) 0.0059(17) 0.0040(16) N24 0.026(4) 0.034(9) 0.025(4) -0.0163(15) 0.0090(15) -0.0002(15) C25 0.050(7) 0.040(10) 0.039(5) -0.020(2) 0.027(2) -0.004(2) C26 0.065(9) 0.051(13) 0.041(6) -0.023(3) 0.032(3) -0.013(2) C27 0.062(8) 0.072(19) 0.030(4) -0.032(3) 0.022(2) -0.004(2) C28 0.037(5) 0.052(13) 0.023(4) -0.020(2) 0.0040(19) 0.007(2) C29 0.022(3) 0.041(11) 0.021(3) -0.0180(18) -0.0016(16) 0.0043(17) C30 0.016(3) 0.038(10) 0.023(3) -0.0124(17) -0.0040(16) 0.0124(17) C31 0.026(4) 0.042(11) 0.031(4) -0.014(2) 0.0006(18) 0.0186(19) C32 0.025(4) 0.031(8) 0.053(7) -0.0051(19) 0.004(2) 0.025(2) C33 0.026(4) 0.028(7) 0.054(7) -0.0043(18) 0.010(2) 0.013(2) C34 0.018(3) 0.030(8) 0.035(5) -0.0056(17) 0.0007(17) 0.0102(18) N35 0.014(2) 0.028(7) 0.026(4) -0.0083(14) 0.0014(13) 0.0084(14) C36 0.025(4) 0.024(7) 0.037(5) -0.0033(17) 0.0111(18) 0.0050(18) C37 0.019(3) 0.023(6) 0.036(5) -0.0004(16) 0.0066(18) 0.0116(17) N38 0.013(2) 0.023(6) 0.021(3) -0.0043(13) 0.0015(13) 0.0055(13) C39 0.016(3) 0.025(7) 0.024(4) -0.0034(16) 0.0015(16) 0.0059(16) C40 0.019(3) 0.020(5) 0.036(5) 0.0002(16) 0.0027(17) 0.0064(17) C41 0.022(3) 0.030(8) 0.028(4) -0.0022(17) 0.0066(17) -0.0002(17) C42 0.018(3) 0.034(9) 0.024(4) -0.0095(17) 0.0061(16) 0.0009(17) C43 0.014(3) 0.027(7) 0.020(3) -0.0051(15) 0.0007(15) 0.0070(15) C44 0.018(3) 0.027(7) 0.013(2) -0.0075(16) 0.0019(15) 0.0026(15) C45 0.020(3) 0.031(8) 0.027(4) -0.0074(17) 0.0039(17) 0.0008(17) C46 0.026(4) 0.036(9) 0.033(5) -0.0176(19) 0.0057(18) -0.0002(18) C47 0.034(5) 0.026(7) 0.032(5) -0.0138(18) 0.0114(19) -0.0001(17) C48 0.023(4) 0.023(6) 0.027(4) -0.0051(16) 0.0056(17) 0.0035(16) N49 0.021(3) 0.026(7) 0.013(2) -0.0088(14) 0.0028(13) 0.0018(12) C50 0.026(4) 0.041(11) 0.046(6) -0.009(2) 0.002(2) 0.011(2) C51 0.024(4) 0.036(9) 0.034(5) -0.0154(19) 0.0068(18) -0.004(2) N52 0.034(5) 0.038(10) 0.076(10) -0.0159(19) -0.008(2) 0.010(2) C53 0.144(19) 0.063(17) 0.038(6) -0.021(4) -0.022(4) 0.002(3) C54 0.069(10) 0.11(3) 0.042(6) -0.055(4) 0.019(3) -0.008(3) N55 0.23(3) 0.25(6) 0.063(9) -0.202(8) 0.072(5) -0.046(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 Cl4 2.3658(15) . . no Fe1 O3 1.775(3) . . no Fe1 O6 2.063(3) . . no Fe1 O15 2.070(3) . . no Fe1 N24 2.169(3) . . no Fe1 N35 2.233(3) . . no Fe2 Cl5 2.3806(16) . . no Fe2 O3 1.781(2) . . no Fe2 O8 2.034(3) . . no Fe2 O17 2.085(3) . . no Fe2 N38 2.246(3) . . no Fe2 N49 2.174(3) . . no O6 C7 1.270(4) . . no O8 C7 1.267(4) . . no O15 C16 1.264(4) . . no O17 C16 1.261(4) . . no N24 C25 1.337(5) . . no N24 C29 1.345(5) . . no N35 C30 1.360(5) . . no N35 C34 1.354(5) . . no N38 C39 1.353(5) . . no N38 C43 1.357(5) . . no N49 C44 1.349(5) . . no N49 C48 1.339(5) . . no N52 C51 1.124(5) . . no N55 C54 1.112(8) . . no C7 C9 1.497(5) . . no C9 C10 1.389(5) . . no C9 C14 1.400(5) . . no C10 C11 1.380(5) . . no C10 H1 0.966(4) . . no C11 C12 1.383(6) . . no C11 H2 0.974(4) . . no C12 C13 1.388(6) . . no C12 H3 0.972(4) . . no C13 C14 1.388(6) . . no C13 H4 0.949(4) . . no C14 H5 0.963(4) . . no C16 C18 1.503(5) . . no C18 C19 1.390(5) . . no C18 C23 1.391(5) . . no C19 C20 1.380(5) . . no C19 H6 0.956(4) . . no C20 C21 1.403(6) . . no C20 H7 0.975(4) . . no C21 C22 1.383(6) . . no C21 H8 0.965(4) . . no C22 C23 1.389(5) . . no C22 H9 0.955(4) . . no C23 H10 0.960(4) . . no C25 C26 1.376(6) . . no C25 H11 0.972(4) . . no C26 C27 1.384(7) . . no C26 H12 0.970(5) . . no C27 C28 1.365(7) . . no C27 H13 0.954(4) . . no C28 C29 1.398(6) . . no C28 H14 0.965(4) . . no C29 C30 1.480(6) . . no C30 C31 1.395(5) . . no C31 C32 1.379(6) . . no C31 H15 0.990(4) . . no C32 C33 1.380(6) . . no C32 H16 0.959(4) . . no C33 C34 1.393(5) . . no C33 H17 0.958(5) . . no C34 C36 1.514(5) . . no C36 C37 1.531(5) . . no C36 H18 0.969(4) . . no C36 H19 0.961(4) . . no C37 C39 1.512(5) . . no C37 H20 0.953(4) . . no C37 H21 0.964(4) . . no C39 C40 1.384(5) . . no C40 C41 1.388(5) . . no C40 H22 0.963(4) . . no C41 C42 1.376(5) . . no C41 H23 0.957(4) . . no C42 C43 1.383(5) . . no C42 H24 0.953(4) . . no C43 C44 1.483(5) . . no C44 C45 1.393(5) . . no C45 C46 1.382(6) . . no C45 H25 0.959(4) . . no C46 C47 1.380(6) . . no C46 H26 0.946(4) . . no C47 C48 1.384(5) . . no C47 H27 0.964(4) . . no C48 H28 0.955(4) . . no C50 C51 1.457(6) . . no C50 H29 0.942(5) . . no C50 H30 0.952(5) . . no C50 H31 0.973(4) . . no C53 C54 1.409(8) . . no C53 H32 0.973(9) . . no C53 H33 0.966(7) . . no C53 H34 0.954(6) . . no C56 C57 1.165(14) . . no C57 C57 1.87(2) . 2_555 no C57 C58 1.292(19) . . no C57 C58 1.566(19) . 2_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl4 Fe1 O3 99.70(9) . . . no Cl4 Fe1 O6 93.19(9) . . . no Cl4 Fe1 O15 164.90(8) . . . no Cl4 Fe1 N24 86.45(9) . . . no Cl4 Fe1 N35 90.54(9) . . . no O3 Fe1 O6 95.20(11) . . . no O3 Fe1 O15 95.14(12) . . . no O3 Fe1 N24 171.79(12) . . . no O3 Fe1 N35 98.81(12) . . . no O6 Fe1 O15 88.22(11) . . . no O6 Fe1 N24 89.85(12) . . . no O6 Fe1 N35 164.68(11) . . . no O15 Fe1 N24 78.51(12) . . . no O15 Fe1 N35 84.40(11) . . . no N24 Fe1 N35 75.55(12) . . . no Cl5 Fe2 O3 95.70(9) . . . no Cl5 Fe2 O8 95.09(8) . . . no Cl5 Fe2 O17 166.05(7) . . . no Cl5 Fe2 N38 90.20(9) . . . no Cl5 Fe2 N49 84.80(8) . . . no O3 Fe2 O8 95.95(11) . . . no O3 Fe2 O17 98.25(11) . . . no O3 Fe2 N38 96.94(12) . . . no O3 Fe2 N49 171.68(11) . . . no O8 Fe2 O17 83.64(11) . . . no O8 Fe2 N38 165.51(11) . . . no O8 Fe2 N49 92.28(11) . . . no O17 Fe2 N38 87.98(11) . . . no O17 Fe2 N49 81.38(10) . . . no N38 Fe2 N49 74.74(12) . . . no Fe1 O3 Fe2 125.80(14) . . . no Fe1 O6 C7 130.8(2) . . . no Fe2 O8 C7 127.2(2) . . . no Fe1 O15 C16 126.1(2) . . . no Fe2 O17 C16 129.1(2) . . . no Fe1 N24 C25 123.9(3) . . . no Fe1 N24 C29 116.9(3) . . . no C25 N24 C29 119.0(3) . . . no Fe1 N35 C30 113.8(3) . . . no Fe1 N35 C34 126.9(3) . . . no C30 N35 C34 118.8(3) . . . no Fe2 N38 C39 125.6(2) . . . no Fe2 N38 C43 111.0(2) . . . no C39 N38 C43 118.6(3) . . . no Fe2 N49 C44 116.0(2) . . . no Fe2 N49 C48 125.0(3) . . . no C44 N49 C48 119.0(3) . . . no O6 C7 O8 125.8(3) . . . no O6 C7 C9 117.5(3) . . . no O8 C7 C9 116.8(3) . . . no C7 C9 C10 119.8(3) . . . no C7 C9 C14 120.8(3) . . . no C10 C9 C14 119.3(3) . . . no C9 C10 C11 120.8(4) . . . no C9 C10 H1 119.6(4) . . . no C11 C10 H1 119.6(4) . . . no C10 C11 C12 120.1(4) . . . no C10 C11 H2 119.6(4) . . . no C12 C11 H2 120.3(4) . . . no C11 C12 C13 119.7(4) . . . no C11 C12 H3 121.6(4) . . . no C13 C12 H3 118.7(4) . . . no C12 C13 C14 120.6(4) . . . no C12 C13 H4 120.0(4) . . . no C14 C13 H4 119.3(4) . . . no C9 C14 C13 119.5(4) . . . no C9 C14 H5 119.6(4) . . . no C13 C14 H5 120.9(4) . . . no O15 C16 O17 126.0(3) . . . no O15 C16 C18 116.2(3) . . . no O17 C16 C18 117.9(3) . . . no C16 C18 C19 119.7(3) . . . no C16 C18 C23 120.0(3) . . . no C19 C18 C23 120.2(3) . . . no C18 C19 C20 120.6(3) . . . no C18 C19 H6 118.9(4) . . . no C20 C19 H6 120.5(4) . . . no C19 C20 C21 119.2(3) . . . no C19 C20 H7 119.2(4) . . . no C21 C20 H7 121.6(4) . . . no C20 C21 C22 120.2(4) . . . no C20 C21 H8 119.7(4) . . . no C22 C21 H8 120.1(4) . . . no C21 C22 C23 120.4(4) . . . no C21 C22 H9 119.7(4) . . . no C23 C22 H9 119.9(4) . . . no C18 C23 C22 119.4(3) . . . no C18 C23 H10 119.8(4) . . . no C22 C23 H10 120.8(4) . . . no N24 C25 C26 122.9(4) . . . no N24 C25 H11 118.2(4) . . . no C26 C25 H11 118.8(4) . . . no C25 C26 C27 118.0(4) . . . no C25 C26 H12 119.9(5) . . . no C27 C26 H12 122.1(4) . . . no C26 C27 C28 120.0(4) . . . no C26 C27 H13 120.5(5) . . . no C28 C27 H13 119.5(5) . . . no C27 C28 C29 119.1(4) . . . no C27 C28 H14 121.2(4) . . . no C29 C28 H14 119.6(5) . . . no N24 C29 C28 121.0(4) . . . no N24 C29 C30 116.5(3) . . . no C28 C29 C30 122.5(4) . . . no N35 C30 C29 116.7(3) . . . no N35 C30 C31 121.5(4) . . . no C29 C30 C31 121.7(4) . . . no C30 C31 C32 119.2(4) . . . no C30 C31 H15 120.3(4) . . . no C32 C31 H15 120.4(4) . . . no C31 C32 C33 119.3(4) . . . no C31 C32 H16 121.0(4) . . . no C33 C32 H16 119.6(5) . . . no C32 C33 C34 119.5(4) . . . no C32 C33 H17 120.0(4) . . . no C34 C33 H17 120.4(4) . . . no N35 C34 C33 121.4(4) . . . no N35 C34 C36 119.5(3) . . . no C33 C34 C36 118.9(4) . . . no C34 C36 C37 109.8(3) . . . no C34 C36 H18 110.1(3) . . . no C34 C36 H19 110.2(3) . . . no C37 C36 H18 110.0(3) . . . no C37 C36 H19 109.6(3) . . . no H18 C36 H19 107.2(4) . . . no C36 C37 C39 115.6(3) . . . no C36 C37 H20 108.4(3) . . . no C36 C37 H21 107.8(3) . . . no C39 C37 H20 108.9(3) . . . no C39 C37 H21 107.6(3) . . . no H20 C37 H21 108.4(4) . . . no N38 C39 C37 117.7(3) . . . no N38 C39 C40 120.7(3) . . . no C37 C39 C40 121.4(3) . . . no C39 C40 C41 120.1(3) . . . no C39 C40 H22 120.0(4) . . . no C41 C40 H22 119.9(4) . . . no C40 C41 C42 118.6(4) . . . no C40 C41 H23 119.5(4) . . . no C42 C41 H23 121.8(4) . . . no C41 C42 C43 119.1(3) . . . no C41 C42 H24 120.6(4) . . . no C43 C42 H24 120.4(4) . . . no N38 C43 C42 122.2(3) . . . no N38 C43 C44 114.7(3) . . . no C42 C43 C44 123.2(3) . . . no N49 C44 C43 115.7(3) . . . no N49 C44 C45 121.8(3) . . . no C43 C44 C45 122.5(3) . . . no C44 C45 C46 118.4(4) . . . no C44 C45 H25 120.4(4) . . . no C46 C45 H25 121.1(4) . . . no C45 C46 C47 119.8(4) . . . no C45 C46 H26 119.9(4) . . . no C47 C46 H26 120.1(4) . . . no C46 C47 C48 118.7(4) . . . no C46 C47 H27 121.8(4) . . . no C48 C47 H27 119.5(4) . . . no N49 C48 C47 122.3(4) . . . no N49 C48 H28 118.8(4) . . . no C47 C48 H28 118.9(4) . . . no C51 C50 H29 110.7(4) . . . no C51 C50 H30 110.7(4) . . . no C51 C50 H31 109.4(4) . . . no H29 C50 H30 110.1(4) . . . no H29 C50 H31 108.5(4) . . . no H30 C50 H31 107.3(5) . . . no N52 C51 C50 178.5(4) . . . no C54 C53 H32 112.0(6) . . . no C54 C53 H33 111.3(7) . . . no C54 C53 H34 111.7(6) . . . no H32 C53 H33 106.5(5) . . . no H32 C53 H34 107.3(8) . . . no H33 C53 H34 107.7(7) . . . no N55 C54 C53 177.8(9) . . . no C56 C57 C57 178.8(14) . . 2_555 no C56 C57 C58 123.3(15) . . . no C56 C57 C58 138.0(14) . . 2_555 no C57 C57 C58 55.8(10) 2_555 . . no C57 C57 C58 43.0(8) 2_555 . 2_555 no C58 C57 C58 98.8(13) . . 2_555 no C57 C58 C57 81.2(13) 2_555 . . no #===END ############################################################################## # IUMSC CIF Archive file # ############################################################################## data_MSC98140 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C12 H20 Cl4 Fe1 N4 O4' _chemical_formula_moiety ? _chemical_formula_weight 481.973 _cell_length_a 14.343(9) _cell_length_b 17.631(11) _cell_length_c 14.465(9) _cell_angle_alpha 90 _cell_angle_beta 90.12(3) _cell_angle_gamma 90 _cell_volume 3658(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 53 _cell_measurement_theta_min 7.74 _cell_measurement_theta_max 10.21 _cell_measurement_temperature 104. _exptl_crystal_colour red/green? _exptl_crystal_description 'elongated octahedron' _exptl_crystal_size_max .30 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .25 _exptl_crystal_density_diffrn 0.875 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.7165 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2+y,z -x,y,1/2-z 1/2-x,1/2+y,1/2-z x,-y,1/2+z 1/2+x,1/2-y,1/2+z -x,-y,-z 1/2-x,1/2-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 104. _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3348 _diffrn_reflns_av_R_equivalents 0.084 _diffrn_reflns_theta_min 3.35702 _diffrn_reflns_theta_max 24.9933 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 4 _diffrn_standards_decay_% 3 _diffrn_standards_interval_count 300 _reflns_number_total 3211 _reflns_number_gt 2302 _reflns_threshold_expression F^2^>2.33\s(F^2^) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.301 0.845 'International Tables Vol. IV (1974) Table 2.2B' Cl Cl 0.132 0.159 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 2575 _refine_ls_number_parameters 234 _refine_ls_hydrogen_treatment ? _refine_ls_extinction_coef 0.00000021(4) _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.03F)^2^ _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.0573 _refine_ls_goodness_of_fit_ref 2.322 _refine_ls_shift/su_max 0.0036 _refine_diff_density_max 0.83 _refine_diff_density_min -0.74 _computing_data_collection 'NPS, local program' _computing_cell_refinement 'XTEL, local package' _computing_data_reduction 'XTEL, local package' _computing_structure_solution MULTAN78 _computing_structure_refinement 'XTEL, local package' _computing_molecular_graphics 'XTEL, local package' _computing_publication_material 'XTEL, local package' 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_disorder_group _atom_site_disorder_assembly Fe1 Fe 0.04860(6) 0.16036(4) 0.85150(5) 0.0178(3) Uani 1 0 . Cl2 Cl 0.90404(11) 0.15838(9) 0.93018(10) 0.0332(5) Uani 1 0 . O3 O 0.1820(3) 0.1617(2) 0.7827(3) 0.0271(13) Uani 1 0 . O4 O 0 0.1990(3) 0.75 0.0237(18) Uani 1 0 . N5 N 0.1186(3) 0.1360(2) 0.9776(3) 0.0176(14) Uani 1 0 . C6 C 0.1395(4) 0.0659(3) 1.0065(4) 0.0221(18) Uani 1 0 . C7 C 0.1815(4) 0.0521(3) 1.0907(4) 0.0234(19) Uani 1 0 . C8 C 0.2056(4) 0.1137(3) 1.1450(4) 0.0213(18) Uani 1 0 . C9 C 0.1857(4) 0.1856(3) 1.1164(4) 0.0203(17) Uani 1 0 . C10 C 0.1404(4) 0.1964(3) 1.0317(4) 0.0167(16) Uani 1 0 . C11 C 0.1125(4) 0.2712(3) 0.9962(4) 0.0167(17) Uani 1 0 . C12 C 0.1153(4) 0.3355(3) 1.0501(4) 0.0241(18) Uani 1 0 . C13 C 0.0906(5) 0.4046(3) 1.0117(4) 0.027(2) Uani 1 0 . C14 C 0.0662(4) 0.4077(3) 0.9197(4) 0.0249(19) Uani 1 0 . C15 C 0.0646(4) 0.3419(3) 0.8677(4) 0.0261(19) Uani 1 0 . N16 N 0.0846(3) 0.2736(2) 0.9059(3) 0.0224(16) Uani 1 0 . C17 C 0.0512(5) 0.3477(3) 0.7624(4) 0.033(2) Uani 1 0 . O18 O 0.0401(3) 0.04974(19) 0.8173(3) 0.0222(13) Uani 1 0 . C19 C 0 0.0164(4) 0.75 0.019(2) Uani 1 0 . C20 C 0 0.9324(4) 0.75 0.022(3) Uani 1 0 . C21 C 0.9570(4) 0.8930(3) 0.6785(4) 0.0236(18) Uani 1 0 . C22 C 0.9570(5) 0.8142(3) 0.6786(4) 0.030(2) Uani 1 0 . C23 C 0 0.7741(4) 0.75 0.030(3) Uani 1 0 . Cl24 Cl 0 0.43722(11) 0.25 0.0282(7) Uani 1 0 . O25 O 0.2123(3) 0.4605(2) 0.2279(3) 0.0324(15) Uani 1 0 . N26 N 0.7144(4) 0.0766(4) 1.0884(4) 0.047(2) Uani 1 0 . C27 C 0.6875(5) 0.1092(4) 1.0301(5) 0.041(3) Uani 1 0 . C28 C 0.6520(5) 0.1554(4) 0.9502(5) 0.050(3) Uani 1 0 . H1 H 0.2213 0.1189 0.7881 0.0271 Uiso 1 0 . H2 H 0.182 0.1693 0.718 0.1105 Uiso 1 0 . H3 H 0.1252 0.0241 0.9677 0.0466 Uiso 1 0 . H4 H 0.1932 0.0019 1.111 0.0491 Uiso 1 0 . H5 H 0.2364 0.1062 1.202 0.0476 Uiso 1 0 . H6 H 0.2024 0.2275 1.1532 0.0457 Uiso 1 0 . H7 H 0.1335 0.3325 1.1129 0.0497 Uiso 1 0 . H8 H 0.0906 0.4491 1.0484 0.0528 Uiso 1 0 . H9 H 0.0509 0.4549 0.8925 0.0499 Uiso 1 0 . H10 H 0.0786 0.3932 0.7408 0.0572 Uiso 1 0 . H11 H 0.0804 0.3054 0.7335 0.0572 Uiso 1 0 . H12 H 0.9274 0.9198 0.6296 0.0482 Uiso 1 0 . H13 H 0.9282 0.7874 0.6297 0.0556 Uiso 1 0 . H14 H 0 0.7204 0.75 0.055 Uiso 1 0 . H15 H 0.1483 0.4583 0.2422 0.0159 Uiso 1 0 . H16 H 0.2315 0.4906 0.1766 0.0625 Uiso 1 0 . H17 H 0.7055 0.1745 0.9173 0.0747 Uiso 1 0 . H18 H 0.6165 0.1248 0.9112 0.0747 Uiso 1 0 . H19 H 0.6174 0.1966 0.9731 0.0747 Uiso 1 0 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.029(7) 0.009(3) 0.016(4) 0.0009(4) -0.0117(3) -0.0013(3) Cl2 0.036(9) 0.035(13) 0.029(7) -0.0022(8) -0.0021(7) -0.0040(7) O3 0.032(8) 0.020(8) 0.030(8) 0.0047(19) -0.0018(18) -0.0005(19) O4 0.043(11) 0.010(5) 0.019(6) 0 -0.018(3) 0 N5 0.022(6) 0.013(5) 0.018(5) 0.0008(19) -0.007(2) -0.0016(19) C6 0.027(8) 0.016(7) 0.023(7) 0.005(3) -0.008(3) 0.003(2) C7 0.032(9) 0.018(7) 0.020(6) -0.001(3) -0.006(3) 0.003(2) C8 0.025(7) 0.024(10) 0.014(5) 0.003(3) -0.011(2) 0.004(2) C9 0.027(7) 0.018(8) 0.016(5) -0.003(2) -0.008(2) -0.001(2) C10 0.018(5) 0.015(6) 0.018(5) 0.000(2) -0.002(2) 0.001(2) C11 0.024(7) 0.013(6) 0.013(4) -0.001(2) -0.003(2) 0.000(2) C12 0.035(9) 0.017(7) 0.021(6) 0.002(3) -0.014(3) -0.005(3) C13 0.045(12) 0.016(7) 0.020(6) 0.002(3) -0.009(3) -0.006(2) C14 0.039(10) 0.010(5) 0.026(8) -0.000(3) -0.010(3) 0.001(2) C15 0.043(12) 0.014(6) 0.021(6) 0.001(3) -0.015(3) 0.000(2) N16 0.038(10) 0.012(5) 0.018(5) -0.000(2) -0.011(2) -0.0017(19) C17 0.045(12) 0.015(6) 0.038(10) 0.000(3) -0.007(3) 0.005(3) O18 0.034(9) 0.010(4) 0.023(6) 0.0003(17) -0.0143(18) -0.0019(16) C19 0.024(8) 0.017(8) 0.016(6) 0 -0.000(3) 0 C20 0.034(10) 0.009(5) 0.022(7) 0 -0.002(4) 0 C21 0.032(9) 0.014(6) 0.025(7) -0.003(3) -0.005(3) 0.001(2) C22 0.052(14) 0.014(6) 0.026(7) -0.002(3) -0.004(3) -0.006(2) C23 0.057(16) 0.007(5) 0.026(8) 0 0.010(4) 0 Cl24 0.036(9) 0.017(7) 0.031(8) 0 -0.0029(10) 0 O25 0.035(9) 0.026(10) 0.035(9) 0.004(2) -0.009(2) -0.0050(19) N26 0.058(15) 0.043(17) 0.040(11) 0.025(3) -0.015(3) 0.002(3) C27 0.047(13) 0.024(10) 0.051(14) 0.001(3) -0.001(4) -0.006(3) C28 0.054(14) 0.040(16) 0.057(15) 0.010(4) 0.001(4) 0.016(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 Cl2 2.368(2) . 1_455 no Fe1 O3 2.158(4) . . no Fe1 O4 1.761(2) . . no Fe1 O4 1.761(2) . 3_556 no Fe1 O18 2.016(4) . . no Fe1 N5 2.123(5) . . no Fe1 N16 2.207(4) . . no O3 H1 0.946(4) . . no O3 H2 0.945(4) . . no O18 C19 1.274(5) . . no O18 C19 1.274(5) . 3_556 no O25 H15 0.942(4) . . no O25 H16 0.954(4) . . no N5 C6 1.339(7) . . no N5 C10 1.358(7) . . no N16 C11 1.366(7) . . no N16 C15 1.355(7) . . no N26 C27 1.090(8) . . no C6 C7 1.378(8) . . no C6 H3 0.949(6) . . no C7 C8 1.383(8) . . no C7 H4 0.948(5) . . no C8 C9 1.363(8) . . no C8 H5 0.944(5) . . no C9 C10 1.398(7) . . no C9 H6 0.942(5) . . no C10 C11 1.470(7) . . no C11 C12 1.376(7) . . no C12 C13 1.386(8) . . no C12 H7 0.945(5) . . no C13 C14 1.376(8) . . no C13 H8 0.947(5) . . no C14 C15 1.383(8) . . no C14 H9 0.945(5) . . no C15 C17 1.538(8) . . no C17 C17 1.512(13) . 3_556 no C17 H10 0.947(6) . . no C17 H11 0.952(6) . . no C19 C20 1.479(10) . 1_545 no C19 C20 1.479(10) . 3_546 no C20 C21 1.391(7) . 1_455 no C20 C21 1.391(7) . 3_656 no C21 C22 1.389(8) . . no C21 H12 0.950(6) . . no C22 C23 1.394(7) . 1_655 no C22 C23 1.394(7) . 3_656 no C22 H13 0.945(6) . . no C23 H14 0.947(8) . . no C23 H14 0.947(8) . 3_556 no C27 C28 1.502(10) . . no C28 H17 0.965(8) . . no C28 H18 0.931(8) . . no C28 H19 0.941(8) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Fe1 O3 178.69(12) 1_455 . . no Cl2 Fe1 O4 93.50(6) 1_455 . . no Cl2 Fe1 O4 93.50(6) 1_455 . 3_556 no Cl2 Fe1 O18 92.95(13) 1_455 . . no Cl2 Fe1 N5 89.82(14) 1_455 . . no Cl2 Fe1 N16 92.64(14) 1_455 . . no O3 Fe1 O4 87.78(12) . . . no O3 Fe1 O4 87.78(12) . . 3_556 no O3 Fe1 O18 87.15(16) . . . no O3 Fe1 N5 88.87(17) . . . no O3 Fe1 N16 87.01(17) . . . no O4 Fe1 O18 98.39(19) . . . no O4 Fe1 O18 98.39(19) 3_556 . . no O4 Fe1 N5 168.45(19) . . . no O4 Fe1 N5 168.45(19) 3_556 . . no O4 Fe1 N16 92.26(19) . . . no O4 Fe1 N16 92.26(19) 3_556 . . no O18 Fe1 N5 92.47(16) . . . no O18 Fe1 N16 167.64(17) . . . no N5 Fe1 N16 76.53(17) . . . no Fe1 O3 H1 118.8(3) . . . no Fe1 O3 H2 117.4(3) . . . no H1 O3 H2 101.1(4) . . . no Fe1 O4 Fe1 134.5(3) . . 3_556 no Fe1 O4 Fe1 134.5(3) 3_556 . . no Fe1 O18 C19 131.4(4) . . . no Fe1 O18 C19 131.4(4) . . 3_556 no H15 O25 H16 118.5(4) . . . no Fe1 N5 C6 124.1(4) . . . no Fe1 N5 C10 116.4(3) . . . no C6 N5 C10 119.5(5) . . . no Fe1 N16 C11 112.4(3) . . . no Fe1 N16 C15 127.5(4) . . . no C11 N16 C15 118.6(4) . . . no N5 C6 C7 122.4(5) . . . no N5 C6 H3 118.9(5) . . . no C7 C6 H3 118.7(5) . . . no C6 C7 C8 118.1(5) . . . no C6 C7 H4 121.0(6) . . . no C8 C7 H4 120.8(5) . . . no C7 C8 C9 120.3(5) . . . no C7 C8 H5 120.1(5) . . . no C9 C8 H5 119.6(5) . . . no C8 C9 C10 119.3(5) . . . no C8 C9 H6 120.4(5) . . . no C10 C9 H6 120.3(5) . . . no N5 C10 C9 120.3(5) . . . no N5 C10 C11 116.1(4) . . . no C9 C10 C11 123.6(5) . . . no N16 C11 C10 116.2(4) . . . no N16 C11 C12 121.6(5) . . . no C10 C11 C12 122.2(5) . . . no C11 C12 C13 119.4(5) . . . no C11 C12 H7 120.4(5) . . . no C13 C12 H7 120.2(5) . . . no C12 C13 C14 119.1(5) . . . no C12 C13 H8 120.3(5) . . . no C14 C13 H8 120.6(6) . . . no C13 C14 C15 119.8(5) . . . no C13 C14 H9 119.7(5) . . . no C15 C14 H9 120.5(6) . . . no N16 C15 C14 121.4(5) . . . no N16 C15 C17 119.3(5) . . . no C14 C15 C17 119.0(5) . . . no C15 C17 C17 110.8(7) . . 3_556 no C15 C17 H10 109.4(6) . . . no C15 C17 H11 109.2(5) . . . no C17 C17 H10 109.0(4) 3_556 . . no C17 C17 H11 108.9(5) 3_556 . . no H10 C17 H11 109.5(7) . . . no O18 C19 O18 125.0(7) . . 3_556 no O18 C19 O18 125.0(7) 3_556 . . no O18 C19 C20 117.5(3) . . 1_545 no O18 C19 C20 117.5(3) . . 3_546 no O18 C19 C20 117.5(3) 3_556 . 1_545 no O18 C19 C20 117.5(3) 3_556 . 3_546 no O18 C19 C20 117.5(3) . . 1_545 no O18 C19 C20 117.5(3) . . 3_546 no O18 C19 C20 117.5(3) 3_556 . 1_545 no O18 C19 C20 117.5(3) 3_556 . 3_546 no C19 C20 C21 120.1(3) 1_565 . 1_455 no C19 C20 C21 120.1(3) 1_565 . 3_656 no C19 C20 C21 120.1(3) 3_566 . 1_455 no C19 C20 C21 120.1(3) 3_566 . 3_656 no C19 C20 C21 120.1(3) 1_565 . 1_455 no C19 C20 C21 120.1(3) 1_565 . 3_656 no C19 C20 C21 120.1(3) 3_566 . 1_455 no C19 C20 C21 120.1(3) 3_566 . 3_656 no C21 C20 C21 119.9(7) 1_455 . 3_656 no C21 C20 C21 119.9(7) 3_656 . 1_455 no C20 C21 C22 120.0(6) 1_655 . . no C20 C21 C22 120.0(6) 3_656 . . no C20 C21 H12 120.1(5) 1_655 . . no C20 C21 H12 120.1(5) 3_656 . . no C22 C21 H12 119.9(6) . . . no C21 C22 C23 120.6(6) . . 1_655 no C21 C22 C23 120.6(6) . . 3_656 no C21 C22 H13 119.9(6) . . . no C23 C22 H13 119.5(6) 1_655 . . no C23 C22 H13 119.5(6) 3_656 . . no C22 C23 C22 119.1(7) 1_455 . 3_656 no C22 C23 C22 119.1(7) 3_656 . 1_455 no C22 C23 H14 120.5(4) 1_455 . . no C22 C23 H14 120.5(4) 1_455 . 3_556 no C22 C23 H14 120.5(4) 3_656 . . no C22 C23 H14 120.5(4) 3_656 . 3_556 no C22 C23 H14 120.5(4) 1_455 . . no C22 C23 H14 120.5(4) 1_455 . 3_556 no C22 C23 H14 120.5(4) 3_656 . . no C22 C23 H14 120.5(4) 3_656 . 3_556 no N26 C27 C28 178.8(8) . . . no C27 C28 H17 107.4(7) . . . no C27 C28 H18 109.7(6) . . . no C27 C28 H19 108.9(7) . . . no H17 C28 H18 109.8(8) . . . no H17 C28 H19 109.0(7) . . . no H18 C28 H19 111.9(8) . . . no #===END ############################################################################## # IUMSC CIF Archive file # ############################################################################## data_MSC99001 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C87 H111 Cl3 Fe6 N12 O33' _chemical_formula_moiety 'C87 H71 Fe6 N12 O14 3+, 3(Cl 1-), 19(H2 O1 )' _chemical_formula_weight 2294.34 _cell_length_a 18.272(3) _cell_length_b 20.688(3) _cell_length_c 15.284(2) _cell_angle_alpha 102.498(7) _cell_angle_beta 95.013(8) _cell_angle_gamma 101.045(8) _cell_volume 5486.0(20) _cell_formula_units_Z 2 _cell_measurement_reflns_used 128 _cell_measurement_theta_min 10.98 _cell_measurement_theta_max 15.27 _cell_measurement_temperature 105 _exptl_crystal_colour brown _exptl_crystal_description 'hexagonal prism' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 0.9234 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.81 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 105 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22929 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_theta_min 3.03271 _diffrn_reflns_theta_max 25.0649 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 4 _diffrn_standards_decay_% 2.4 _diffrn_standards_interval_count 300 _reflns_number_total 19353 _reflns_number_gt 11187 _reflns_threshold_expression F^2^>2.0\s(F^2^) _atom_sites_location_primary DIRDIF-96 _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogen geom loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.301 0.845 'International Tables Vol. IV (1974) Table 2.2B' Cl Cl 0.132 0.159 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 11187 _refine_ls_number_parameters 1247 _refine_ls_hydrogen_treatment noref _refine_ls_extinction_coef 0.00000032(5) _refine_ls_extinction_method Zachariasen _refine_special_details ; The structure was solved by locating a large part of the molecule using DIRDIF-96. The remainder of the atoms in the molecule of interest were located in iterations of a least-squares refinement followed by a difference Fourier. When the molecule of interest had been completed the process of locating the anions and water molecules began. The expected three chloride anions were again not visible in the difference map, probably due to a disorder between anions and water molecules. The six largest peaks were assigned to be 50% Cl and the remaining peaks were added as full or 50% oxygen as they were located. New peaks were added until the largest peaks in the difference map were seen to be residuals of already included atoms. For the final cycles of full-matrix least-squares refinement hydrogen atoms were added to the cation in fixed calculated positions with isotropic thermal parameters equal to 1.0 plus the isotropic equivalent of the parent atom. The 119 atoms of the cation and the six partial chlorine atoms were refined using anisotropic thermal parameters, while the remainder of the solvent atoms were refined with isotropic thermal parameters. The final R(F) was 0.0945 for 1247 parameters. ; _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.07F)^2^ _refine_ls_R_factor_gt 0.0945 _refine_ls_wR_factor_ref 0.1034 _refine_ls_goodness_of_fit_ref 2.2981 _refine_ls_shift/su_max 1.1936 _refine_diff_density_max 1.51 _refine_diff_density_min -0.84 _computing_data_collection 'NPS, local program' _computing_cell_refinement 'XTEL, local package' _computing_data_reduction 'XTEL, local package' _computing_structure_solution DIRDIF-96 _computing_structure_refinement 'XTEL, local package' _computing_molecular_graphics 'XTEL, local package' _computing_publication_material 'XTEL, local package' 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_disorder_group _atom_site_disorder_assembly Fe1 Fe 0.19067(6) 0.13949(6) 0.06163(7) 0.0308(4) Uani 1 0 . Fe2 Fe 0.32121(6) 0.08635(6) 0.00573(7) 0.0322(4) Uani 1 0 . Fe3 Fe 0.18282(6) 0.27447(6) 0.26242(7) 0.0301(4) Uani 1 0 . Fe4 Fe 0.30352(6) 0.19977(5) 0.22808(7) 0.0284(4) Uani 1 0 . Fe5 Fe 0.18650(7) 0.42119(7) 0.45707(9) 0.0520(5) Uani 1 0 . Fe6 Fe 0.29228(6) 0.33077(6) 0.43234(7) 0.0301(4) Uani 1 0 . O7 O 0.2093(3) 0.0603(3) -0.0305(3) 0.0347(19) Uani 1 0 . O8 O 0.2948(2) 0.1357(2) 0.1108(3) 0.0282(18) Uani 1 0 . O9 O 0.2078(3) 0.2142(2) 0.1628(3) 0.0314(19) Uani 1 0 . O10 O 0.2896(3) 0.2752(2) 0.3155(3) 0.0318(19) Uani 1 0 . O11 O 0.1942(3) 0.3429(3) 0.3757(3) 0.036(2) Uani 1 0 . O12 O 0.2615(3) 0.3949(3) 0.5364(3) 0.039(2) Uani 1 0 . O13 O 0.3349(3) 0.0167(3) -0.1133(3) 0.042(2) Uani 1 0 . O14 O 0.1890(4) 0.5072(4) 0.5634(5) 0.099(4) Uani 1 0 . N15 N 0.0793(3) 0.1528(3) 0.0253(4) 0.035(2) Uani 1 0 . C16 C 0.0664(5) 0.1994(4) -0.0204(5) 0.044(3) Uani 1 0 . C17 C -0.0052(6) 0.2166(5) -0.0267(7) 0.066(4) Uani 1 0 . C18 C -0.0602(5) 0.1875(5) 0.0196(6) 0.047(4) Uani 1 0 . C19 C -0.0448(4) 0.1409(4) 0.0645(6) 0.044(3) Uani 1 0 . C20 C 0.0242(4) 0.1216(4) 0.0638(5) 0.035(3) Uani 1 0 . C21 C 0.0418(4) 0.0659(4) 0.1018(5) 0.035(3) Uani 1 0 . C22 C -0.0142(4) 0.0196(5) 0.1230(5) 0.044(3) Uani 1 0 . C23 C 0.0024(5) -0.0350(4) 0.1532(6) 0.045(3) Uani 1 0 . C24 C 0.0739(5) -0.0419(4) 0.1608(5) 0.041(3) Uani 1 0 . C25 C 0.1317(5) 0.0085(4) 0.1406(5) 0.042(3) Uani 1 0 . N26 N 0.1136(3) 0.0613(3) 0.1107(4) 0.033(2) Uani 1 0 . C27 C 0.2113(4) 0.0009(4) 0.1522(5) 0.040(3) Uani 1 0 . C28 C 0.2329(4) -0.0492(4) 0.0731(5) 0.038(3) Uani 1 0 . N29 N 0.3603(4) 0.0123(3) 0.0725(4) 0.038(3) Uani 1 0 . C30 C 0.3174(5) -0.0423(4) 0.0896(5) 0.040(3) Uani 1 0 . C31 C 0.3492(5) -0.0869(4) 0.1271(6) 0.052(4) Uani 1 0 . C32 C 0.4257(5) -0.0753(5) 0.1493(6) 0.049(4) Uani 1 0 . C33 C 0.4683(4) -0.0203(5) 0.1327(6) 0.047(4) Uani 1 0 . C34 C 0.4364(4) 0.0231(4) 0.0946(5) 0.042(3) Uani 1 0 . C35 C 0.4811(4) 0.0865(4) 0.0733(5) 0.033(3) Uani 1 0 . C36 C 0.5589(5) 0.1062(5) 0.0965(6) 0.045(3) Uani 1 0 . C37 C 0.5956(5) 0.1641(5) 0.0782(6) 0.057(4) Uani 1 0 . C38 C 0.5565(5) 0.2021(5) 0.0320(6) 0.052(4) Uani 1 0 . C39 C 0.4803(5) 0.1790(5) 0.0120(6) 0.048(4) Uani 1 0 . N40 N 0.4430(3) 0.1214(3) 0.0320(4) 0.037(3) Uani 1 0 . O41 O 0.3249(3) 0.1576(3) -0.0676(3) 0.038(2) Uani 1 0 . C42 C 0.2796(4) 0.1960(4) -0.0731(5) 0.039(3) Uani 1 0 . O43 O 0.2238(3) 0.1972(3) -0.0278(3) 0.039(2) Uani 1 0 . C44 C 0.2923(5) 0.2424(4) -0.1338(5) 0.047(3) Uani 1 0 . C45 C 0.3489(5) 0.2370(5) -0.1868(5) 0.051(4) Uani 1 0 . C46 C 0.3563(7) 0.2831(7) -0.2468(6) 0.088(5) Uani 1 0 . C47 C 0.3135(7) 0.3280(6) -0.2517(8) 0.076(5) Uani 1 0 . C48 C 0.2588(6) 0.3308(5) -0.1973(8) 0.073(5) Uani 1 0 . C49 C 0.2468(5) 0.2904(5) -0.1363(6) 0.053(4) Uani 1 0 . N50 N 0.0645(3) 0.2775(3) 0.2369(4) 0.037(3) Uani 1 0 . C51 C 0.0113(4) 0.2488(4) 0.2801(6) 0.046(3) Uani 1 0 . C52 C -0.0607(5) 0.2587(5) 0.2772(6) 0.054(4) Uani 1 0 . C53 C -0.0787(5) 0.2995(5) 0.2254(7) 0.063(4) Uani 1 0 . C54 C -0.0251(6) 0.3311(5) 0.1800(6) 0.055(4) Uani 1 0 . C55 C 0.0458(4) 0.3183(4) 0.1891(5) 0.040(3) Uani 1 0 . C56 C 0.1065(5) 0.3513(4) 0.1467(6) 0.049(3) Uani 1 0 . C57 C 0.0969(6) 0.3900(5) 0.0819(7) 0.067(5) Uani 1 0 . C58 C 0.1545(6) 0.4226(6) 0.0482(8) 0.081(6) Uani 1 0 . C59 C 0.2248(6) 0.4196(5) 0.0834(7) 0.069(5) Uani 1 0 . C60 C 0.2365(5) 0.3819(4) 0.1466(5) 0.043(3) Uani 1 0 . N61 N 0.1778(4) 0.3482(3) 0.1769(4) 0.040(3) Uani 1 0 . C62 C 0.3136(4) 0.3771(4) 0.1799(5) 0.038(3) Uani 1 0 . C63 C 0.3435(5) 0.3235(4) 0.1158(5) 0.044(3) Uani 1 0 . N64 N 0.4102(3) 0.2619(3) 0.2034(4) 0.033(2) Uani 1 0 . C65 C 0.4157(4) 0.3123(4) 0.1595(5) 0.036(3) Uani 1 0 . C66 C 0.4821(5) 0.3563(4) 0.1606(6) 0.048(4) Uani 1 0 . C67 C 0.5472(5) 0.3461(5) 0.2072(7) 0.061(4) Uani 1 0 . C68 C 0.5441(4) 0.2934(5) 0.2463(6) 0.054(4) Uani 1 0 . C69 C 0.4734(4) 0.2502(4) 0.2445(5) 0.044(3) Uani 1 0 . C70 C 0.4643(4) 0.1905(4) 0.2837(5) 0.034(3) Uani 1 0 . C71 C 0.5274(4) 0.1678(4) 0.3137(5) 0.040(3) Uani 1 0 . C72 C 0.5140(5) 0.1084(5) 0.3445(6) 0.057(4) Uani 1 0 . C73 C 0.4396(5) 0.0752(4) 0.3472(6) 0.052(4) Uani 1 0 . C74 C 0.3802(4) 0.1022(4) 0.3170(5) 0.042(3) Uani 1 0 . N75 N 0.3928(3) 0.1616(3) 0.2872(4) 0.034(3) Uani 1 0 . O76 O 0.2366(3) 0.1366(2) 0.2911(3) 0.0300(19) Uani 1 0 . C77 C 0.1731(4) 0.1416(4) 0.3139(5) 0.032(3) Uani 1 0 . O78 O 0.1418(3) 0.1910(2) 0.3120(3) 0.0307(19) Uani 1 0 . C79 C 0.1298(4) 0.0855(4) 0.3488(5) 0.039(3) Uani 1 0 . C80 C 0.1654(4) 0.0368(4) 0.3767(5) 0.042(3) Uani 1 0 . C81 C 0.1281(5) -0.0146(5) 0.4059(6) 0.049(4) Uani 1 0 . C82 C 0.0531(6) -0.0214(5) 0.4093(6) 0.060(4) Uani 1 0 . C83 C 0.0168(5) 0.0264(5) 0.3850(6) 0.054(4) Uani 1 0 . C84 C 0.0551(4) 0.0800(4) 0.3563(5) 0.038(3) Uani 1 0 . N85 N 0.1115(6) 0.4599(5) 0.3754(7) 0.091(5) Uani 1 0 . C86 C 0.1340(8) 0.4943(7) 0.3133(9) 0.099(7) Uani 1 0 . C87 C 0.0736(12) 0.5169(7) 0.2682(10) 0.129(9) Uani 1 0 . C88 C 0.0053(14) 0.5061(11) 0.2809(15) 0.162(12) Uani 1 0 . C89 C -0.0172(10) 0.4714(9) 0.3445(13) 0.151(10) Uani 1 0 . C90 C 0.0379(8) 0.4477(7) 0.3904(10) 0.099(7) Uani 1 0 . C91 C 0.0200(6) 0.4086(7) 0.4560(10) 0.093(6) Uani 1 0 . C92 C -0.0533(11) 0.3932(12) 0.4725(13) 0.138(11) Uani 1 0 . C93 C -0.0686(8) 0.3593(10) 0.5288(13) 0.149(10) Uani 1 0 . C94 C -0.0125(6) 0.3279(8) 0.5789(9) 0.132(7) Uani 1 0 . C95 C 0.0599(5) 0.3480(6) 0.5507(8) 0.080(5) Uani 1 0 . N96 N 0.0751(4) 0.3847(5) 0.4924(6) 0.069(4) Uani 1 0 . C97 C 0.1205(5) 0.3130(6) 0.5868(6) 0.066(4) Uani 1 0 . C98 C 0.1306(5) 0.2552(5) 0.5107(6) 0.055(4) Uani 1 0 . N99 N 0.2632(4) 0.2500(3) 0.5057(4) 0.041(3) Uani 1 0 . C100 C 0.1954(5) 0.2242(5) 0.5296(5) 0.049(4) Uani 1 0 . C101 C 0.1864(6) 0.1692(6) 0.5669(6) 0.064(4) Uani 1 0 . C102 C 0.2439(9) 0.1384(6) 0.5820(7) 0.087(6) Uani 1 0 . C103 C 0.3122(6) 0.1651(5) 0.5636(7) 0.066(5) Uani 1 0 . C104 C 0.3218(5) 0.2191(4) 0.5244(5) 0.046(3) Uani 1 0 . C105 C 0.3977(4) 0.2566(5) 0.5090(5) 0.043(3) Uani 1 0 . C106 C 0.4620(5) 0.2323(5) 0.5266(6) 0.057(4) Uani 1 0 . C107 C 0.5267(6) 0.2675(7) 0.5129(7) 0.079(5) Uani 1 0 . C108 C 0.5330(5) 0.3279(6) 0.4814(7) 0.068(5) Uani 1 0 . C109 C 0.4652(5) 0.3473(5) 0.4661(6) 0.053(4) Uani 1 0 . N110 N 0.3984(3) 0.3112(3) 0.4806(4) 0.033(2) Uani 1 0 . O111 O 0.3540(3) 0.4154(3) 0.4055(4) 0.047(2) Uani 1 0 . C112 C 0.3356(7) 0.4668(5) 0.3962(6) 0.066(5) Uani 1 0 . O113 O 0.2703(4) 0.4833(3) 0.4147(4) 0.069(3) Uani 1 0 . C114 C 0.3828(9) 0.5189(6) 0.3562(7) 0.091(6) Uani 1 0 . C115 C 0.4580(9) 0.5090(6) 0.3436(8) 0.101(6) Uani 1 0 . C116 C 0.5000(10) 0.5498(9) 0.2971(9) 0.135(8) Uani 1 0 . C117 C 0.4688(19) 0.6027(16) 0.2750(15) 0.193(17) Uani 1 0 . C118 C 0.4058(16) 0.6037(13) 0.2776(16) 0.198(15) Uani 1 0 . C119 C 0.3538(10) 0.5696(5) 0.3285(8) 0.120(8) Uani 1 0 . Cl120 Cl 0.2364(3) -0.1145(3) -0.1586(4) 0.078(2) Uani 0.5 0 . Cl121 Cl 0.1727(2) 0.0677(3) -0.2275(3) 0.065(2) Uani 0.5 0 . Cl122 Cl -0.2714(3) 0.2414(3) 0.2959(4) 0.075(2) Uani 0.5 0 . Cl123 Cl 0.2780(4) 0.5042(3) 0.7278(4) 0.094(3) Uani 0.5 0 . Cl124 Cl -0.0966(4) 0.1604(3) 0.4673(5) 0.090(3) Uani 0.5 0 . Cl125 Cl 0.0561(4) 0.3274(4) -0.1818(4) 0.106(3) Uani 0.5 0 . O126 O 0.3037(4) -0.0750(3) 0.3793(4) 0.0696(19) Uiso 1 0 . O127 O 0.3220(4) 0.0484(4) -0.2737(5) 0.085(2) Uiso 1 0 . O128 O 0.1599(5) 0.4564(5) 0.7575(6) 0.112(3) Uiso 1 0 . O129 O -0.1276(5) 0.0844(4) 0.2698(6) 0.101(3) Uiso 1 0 . O130 O 0.0912(5) 0.1627(4) -0.2508(6) 0.113(3) Uiso 1 0 . O131 O 0.7337(6) 0.3401(5) 0.1704(7) 0.128(3) Uiso 1 0 . O132 O 0.4539(6) 0.1260(5) 0.6877(7) 0.132(3) Uiso 1 0 . O133 O 0.5515(6) 0.2340(5) -0.1991(7) 0.144(4) Uiso 1 0 . O134 O 0.4721(6) -0.0674(6) 0.4418(7) 0.153(4) Uiso 1 0 . O135 O -0.2547(8) 0.3081(7) 0.6296(9) 0.072(4) Uiso 0.5 0 . O136 O 0.2713(7) 0.6384(7) 0.5389(9) 0.067(4) Uiso 0.5 0 . O137 O -0.2002(9) 0.2473(8) -0.1036(11) 0.105(5) Uiso 0.5 0 . O138 O 0.2785(9) 0.6102(8) 0.6204(11) 0.096(5) Uiso 0.5 0 . O139 O -0.0461(9) 0.1900(8) 0.6949(11) 0.096(5) Uiso 0.5 0 . O140 O -0.0680(11) 0.3951(10) -0.0734(14) 0.135(7) Uiso 0.5 0 . O141 O 0.3603(9) 0.5054(8) 0.6352(11) 0.095(5) Uiso 0.5 0 . O142 O 0.1454(9) 0.4612(8) -0.1594(11) 0.092(5) Uiso 0.5 0 . O143 O 0.1782(9) -0.1484(8) 0.2411(10) 0.091(5) Uiso 0.5 0 . O144 O -0.2930(9) 0.0535(8) 0.4167(11) 0.097(5) Uiso 0.5 0 . O145 O -0.0842(10) 0.4416(9) 0.0397(12) 0.118(6) Uiso 0.5 0 . O146 O 0.2287(11) -0.2227(9) -0.0561(13) 0.122(6) Uiso 0.5 0 . O147 O 0.5085(14) 0.4307(12) -0.0304(17) 0.171(9) Uiso 0.5 0 . O148 O 0.6700(12) 0.4965(10) 0.1906(15) 0.137(7) Uiso 0.5 0 . O149 O 0.6979(13) 0.1682(12) 0.3219(16) 0.161(8) Uiso 0.5 0 . O150 O -0.1718(15) 0.1938(13) 0.5984(18) 0.193(10) Uiso 0.5 0 . O151 O -0.1941(15) 0.1571(14) 0.4101(18) 0.073(8) Uiso 0.25 0 . O152 O -0.0796(11) 0.3330(10) -0.1566(14) 0.125(6) Uiso 0.5 0 . O153 O 0.3240(13) -0.2240(12) 0.2723(16) 0.163(9) Uiso 0.5 0 . O154 O 0.4197(15) 0.4916(13) -0.0275(17) 0.183(10) Uiso 0.5 0 . O155 O 0.7193(15) 0.2984(15) 0.4488(19) 0.196(11) Uiso 0.5 0 . H1 H 0.1054 0.2215 -0.0475 0.0565 Uiso 1 0 . H2 H -0.0152 0.2475 -0.062 0.0746 Uiso 1 0 . H3 H -0.1071 0.2014 0.0196 0.0592 Uiso 1 0 . H4 H -0.0819 0.1207 0.0952 0.0573 Uiso 1 0 . H5 H -0.0649 0.0245 0.118 0.0566 Uiso 1 0 . H6 H -0.0365 -0.0675 0.1674 0.0574 Uiso 1 0 . H7 H 0.0865 -0.0799 0.1804 0.0539 Uiso 1 0 . H8 H 0.2427 0.0437 0.16 0.0536 Uiso 1 0 . H9 H 0.2187 -0.0155 0.2058 0.0536 Uiso 1 0 . H10 H 0.2078 -0.0946 0.0706 0.0504 Uiso 1 0 . H11 H 0.2189 -0.0383 0.0174 0.0504 Uiso 1 0 . H12 H 0.3177 -0.1258 0.1386 0.0657 Uiso 1 0 . H13 H 0.4477 -0.1054 0.1773 0.0626 Uiso 1 0 . H14 H 0.5216 -0.0101 0.1486 0.06 Uiso 1 0 . H15 H 0.5855 0.0788 0.1244 0.0573 Uiso 1 0 . H16 H 0.6474 0.1801 0.0983 0.0708 Uiso 1 0 . H17 H 0.5815 0.2404 0.0155 0.064 Uiso 1 0 . H18 H 0.4518 0.2044 -0.0155 0.0604 Uiso 1 0 . H19 H 0.3801 0.2054 -0.1846 0.0632 Uiso 1 0 . H20 H 0.3952 0.2813 -0.2837 0.0967 Uiso 1 0 . H21 H 0.3207 0.3565 -0.2909 0.0878 Uiso 1 0 . H22 H 0.2277 0.3617 -0.2012 0.0862 Uiso 1 0 . H23 H 0.2097 0.2948 -0.0978 0.0641 Uiso 1 0 . H24 H 0.0248 0.2192 0.3159 0.0579 Uiso 1 0 . H25 H -0.096 0.2369 0.3113 0.0662 Uiso 1 0 . H26 H -0.1285 0.3062 0.2221 0.0784 Uiso 1 0 . H27 H -0.0374 0.3609 0.1426 0.0692 Uiso 1 0 . H28 H 0.0464 0.3922 0.0624 0.0791 Uiso 1 0 . H29 H 0.1465 0.4481 0.0063 0.0926 Uiso 1 0 . H30 H 0.2668 0.4444 0.0638 0.0805 Uiso 1 0 . H31 H 0.3464 0.4202 0.1862 0.0493 Uiso 1 0 . H32 H 0.3134 0.3666 0.2373 0.0493 Uiso 1 0 . H33 H 0.3069 0.282 0.1013 0.0556 Uiso 1 0 . H34 H 0.3527 0.338 0.0625 0.0556 Uiso 1 0 . H35 H 0.4842 0.3915 0.1305 0.0616 Uiso 1 0 . H36 H 0.594 0.3776 0.2121 0.0732 Uiso 1 0 . H37 H 0.5892 0.2864 0.2754 0.0674 Uiso 1 0 . H38 H 0.577 0.1918 0.313 0.053 Uiso 1 0 . H39 H 0.5547 0.09 0.3631 0.0691 Uiso 1 0 . H40 H 0.4295 0.0353 0.3697 0.064 Uiso 1 0 . H41 H 0.33 0.0797 0.3174 0.0545 Uiso 1 0 . H42 H 0.2181 0.041 0.3736 0.057 Uiso 1 0 . H43 H 0.1537 -0.0462 0.4253 0.0637 Uiso 1 0 . H44 H 0.0251 -0.0594 0.4292 0.0728 Uiso 1 0 . H45 H -0.0349 0.023 0.3907 0.0669 Uiso 1 0 . H46 H 0.0292 0.1129 0.3402 0.05 Uiso 1 0 . H47 H 0.1869 0.5027 0.3 0.118 Uiso 1 0 . H48 H 0.0922 0.5427 0.2205 0.1441 Uiso 1 0 . H49 H -0.0248 0.526 0.2452 0.1764 Uiso 1 0 . H50 H -0.0693 0.4635 0.3564 0.168 Uiso 1 0 . H51 H -0.0903 0.4093 0.4373 0.1572 Uiso 1 0 . H52 H -0.1181 0.3538 0.5407 0.17 Uiso 1 0 . H53 H -0.024 0.3009 0.6207 0.1549 Uiso 1 0 . H54 H 0.1669 0.3435 0.6081 0.0788 Uiso 1 0 . H55 H 0.1032 0.2936 0.6356 0.0788 Uiso 1 0 . H56 H 0.0858 0.2207 0.4986 0.0671 Uiso 1 0 . H57 H 0.1369 0.2732 0.4593 0.0671 Uiso 1 0 . H58 H 0.1383 0.1512 0.5821 0.0768 Uiso 1 0 . H59 H 0.2368 0.0992 0.6058 0.1011 Uiso 1 0 . H60 H 0.355 0.147 0.5783 0.0779 Uiso 1 0 . H61 H 0.4595 0.1919 0.5464 0.0686 Uiso 1 0 . H62 H 0.5702 0.2511 0.526 0.0895 Uiso 1 0 . H63 H 0.5798 0.3524 0.4733 0.0824 Uiso 1 0 . H64 H 0.4651 0.3869 0.4458 0.0661 Uiso 1 0 . H65 H 0.4784 0.4743 0.3647 0.1098 Uiso 1 0 . H66 H 0.5479 0.5419 0.2839 0.1498 Uiso 1 0 . H67 H 0.5001 0.639 0.2633 0.2188 Uiso 1 0 . H68 H 0.3854 0.6311 0.2437 0.2149 Uiso 1 0 . H69 H 0.3083 0.5802 0.3426 0.1327 Uiso 1 0 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.029(3) 0.041(5) 0.0257(17) 0.0135(5) 0.0044(5) 0.0090(5) Fe2 0.029(3) 0.045(6) 0.0266(18) 0.0165(5) 0.0073(5) 0.0086(5) Fe3 0.025(2) 0.038(5) 0.0298(19) 0.0149(5) 0.0024(5) 0.0074(5) Fe4 0.026(2) 0.039(5) 0.0258(17) 0.0142(5) 0.0072(5) 0.0109(5) Fe5 0.045(4) 0.063(8) 0.044(3) 0.0352(7) -0.0065(6) -0.0089(7) Fe6 0.024(2) 0.039(5) 0.0284(19) 0.0124(5) 0.0043(5) 0.0066(5) O7 0.028(4) 0.044(7) 0.031(3) 0.012(2) 0.003(2) 0.005(3) O8 0.029(4) 0.035(5) 0.023(3) 0.016(2) 0.008(2) 0.005(2) O9 0.031(4) 0.044(7) 0.023(3) 0.018(2) 0.003(2) 0.008(2) O10 0.028(4) 0.040(6) 0.027(3) 0.009(2) 0.001(2) 0.006(2) O11 0.027(4) 0.050(7) 0.028(3) 0.017(2) -0.004(2) 0.002(3) O12 0.029(4) 0.056(8) 0.035(4) 0.024(3) 0.003(2) 0.007(3) O13 0.036(5) 0.053(8) 0.037(4) 0.020(3) 0.013(2) -0.002(3) O14 0.089(10) 0.099(14) 0.091(8) 0.078(5) -0.022(4) -0.047(5) N15 0.032(5) 0.040(7) 0.032(4) 0.010(3) -0.004(3) 0.009(3) C16 0.042(6) 0.050(9) 0.039(5) 0.015(4) 0.003(4) 0.006(4) C17 0.074(10) 0.050(9) 0.065(8) 0.029(5) -0.041(6) -0.001(5) C18 0.031(5) 0.055(9) 0.054(7) 0.011(4) 0.009(4) 0.006(5) C19 0.035(6) 0.047(8) 0.046(6) 0.009(4) 0.008(4) -0.002(4) C20 0.031(5) 0.041(7) 0.032(5) 0.010(4) 0.002(3) 0.003(4) C21 0.033(5) 0.048(8) 0.022(4) 0.007(4) 0.008(3) 0.003(4) C22 0.035(6) 0.059(10) 0.030(5) 0.009(4) 0.001(4) -0.004(4) C23 0.037(6) 0.051(9) 0.041(6) 0.001(4) 0.015(4) 0.005(4) C24 0.048(7) 0.038(7) 0.035(5) 0.002(4) 0.016(4) 0.005(4) C25 0.053(7) 0.055(9) 0.022(4) 0.020(4) 0.013(4) 0.004(4) N26 0.037(5) 0.035(6) 0.031(4) 0.014(3) 0.015(3) 0.007(3) C27 0.040(6) 0.042(7) 0.042(5) 0.018(4) 0.009(4) 0.009(4) C28 0.037(6) 0.047(8) 0.035(5) 0.017(4) 0.003(4) 0.013(4) N29 0.040(5) 0.044(7) 0.037(4) 0.020(3) 0.012(3) 0.012(3) C30 0.052(7) 0.050(8) 0.031(5) 0.034(4) 0.017(4) 0.011(4) C31 0.075(10) 0.045(8) 0.043(6) 0.026(5) 0.018(5) 0.010(4) C32 0.052(8) 0.061(10) 0.047(6) 0.040(5) 0.003(4) 0.017(5) C33 0.033(6) 0.070(11) 0.050(6) 0.029(5) 0.011(4) 0.021(5) C34 0.039(6) 0.055(9) 0.031(5) 0.026(4) 0.002(4) -0.005(4) C35 0.034(5) 0.037(7) 0.027(4) 0.016(4) 0.004(3) 0.001(4) C36 0.036(6) 0.056(9) 0.046(6) 0.024(4) 0.003(4) 0.007(4) C37 0.033(6) 0.071(12) 0.056(7) 0.010(5) 0.005(4) -0.008(5) C38 0.033(6) 0.068(11) 0.047(6) 0.008(5) 0.004(4) -0.003(5) C39 0.043(7) 0.063(10) 0.044(6) 0.021(5) 0.015(4) 0.013(5) N40 0.030(5) 0.044(7) 0.036(4) 0.009(3) 0.006(3) 0.006(3) O41 0.037(5) 0.054(8) 0.030(3) 0.013(3) 0.016(2) 0.018(3) C42 0.043(6) 0.041(7) 0.036(5) 0.016(4) 0.006(4) 0.010(4) O43 0.044(5) 0.050(7) 0.032(4) 0.019(3) 0.007(3) 0.015(3) C44 0.050(7) 0.054(9) 0.031(5) -0.003(4) 0.001(4) 0.013(4) C45 0.062(8) 0.060(10) 0.027(5) 0.002(5) 0.009(4) 0.011(4) C46 0.087(12) 0.111(18) 0.033(6) -0.055(8) 0.012(6) 0.008(6) C47 0.094(13) 0.077(13) 0.061(8) 0.014(7) -0.014(7) 0.035(6) C48 0.077(11) 0.069(12) 0.079(9) 0.019(6) -0.003(6) 0.031(6) C49 0.054(8) 0.063(10) 0.051(6) 0.010(5) 0.004(4) 0.036(5) N50 0.027(4) 0.041(7) 0.043(5) 0.020(3) 0.002(3) 0.003(3) C51 0.029(5) 0.053(9) 0.053(6) 0.018(4) -0.001(4) -0.001(5) C52 0.031(6) 0.066(11) 0.066(8) 0.030(5) 0.003(4) 0.004(5) C53 0.040(7) 0.081(13) 0.062(8) 0.033(5) 0.001(5) -0.005(6) C54 0.066(9) 0.055(9) 0.045(6) 0.035(5) -0.009(5) -0.001(5) C55 0.033(6) 0.051(9) 0.037(5) 0.018(4) -0.004(4) 0.007(4) C56 0.050(7) 0.036(7) 0.055(7) 0.025(4) -0.022(4) 0.002(4) C57 0.064(9) 0.080(13) 0.061(8) 0.037(6) -0.018(5) 0.016(6) C58 0.066(10) 0.105(16) 0.103(11) 0.035(7) 0.003(6) 0.078(8) C59 0.062(9) 0.073(12) 0.080(9) 0.012(6) 0.002(6) 0.040(6) C60 0.049(7) 0.043(8) 0.037(5) 0.013(4) 0.003(4) 0.012(4) N61 0.053(7) 0.035(6) 0.039(5) 0.023(3) 0.002(3) 0.013(3) C62 0.039(6) 0.037(7) 0.042(5) 0.012(4) 0.007(4) 0.015(4) C63 0.050(7) 0.046(8) 0.037(5) 0.003(4) 0.006(4) 0.019(4) N64 0.026(4) 0.038(6) 0.034(4) 0.014(3) 0.001(3) 0.000(3) C65 0.037(6) 0.037(7) 0.036(5) 0.007(4) 0.015(4) 0.008(4) C66 0.044(7) 0.056(9) 0.055(7) 0.016(4) 0.022(4) 0.022(5) C67 0.048(7) 0.063(11) 0.076(8) 0.007(5) 0.033(5) 0.023(6) C68 0.025(5) 0.073(12) 0.064(7) 0.010(4) 0.016(4) 0.013(5) C69 0.032(5) 0.059(10) 0.036(5) 0.017(4) 0.002(4) -0.003(4) C70 0.034(6) 0.040(7) 0.032(5) 0.015(4) 0.011(4) 0.010(4) C71 0.034(6) 0.046(8) 0.040(5) 0.013(4) 0.007(4) 0.007(4) C72 0.043(7) 0.082(13) 0.047(6) 0.039(5) -0.003(4) 0.002(5) C73 0.059(8) 0.048(8) 0.058(7) 0.025(5) 0.004(5) 0.021(5) C74 0.032(5) 0.064(10) 0.032(5) 0.021(4) -0.004(3) 0.010(4) N75 0.035(5) 0.045(7) 0.031(4) 0.023(3) 0.007(3) 0.013(3) O76 0.023(3) 0.038(6) 0.034(4) 0.010(2) 0.005(2) 0.014(2) C77 0.028(5) 0.051(8) 0.023(4) 0.015(4) 0.004(3) 0.013(4) O78 0.024(3) 0.044(7) 0.029(3) 0.015(2) 0.007(2) 0.010(2) C79 0.038(6) 0.044(8) 0.032(5) 0.012(4) 0.005(4) 0.005(4) C80 0.040(6) 0.060(10) 0.035(5) 0.017(4) 0.013(4) 0.020(4) C81 0.053(7) 0.057(10) 0.053(6) 0.021(5) 0.011(4) 0.033(5) C82 0.064(9) 0.065(11) 0.059(7) 0.005(5) 0.030(5) 0.027(5) C83 0.043(7) 0.069(11) 0.055(7) 0.011(5) 0.028(4) 0.017(5) C84 0.044(6) 0.054(9) 0.023(4) 0.017(4) 0.013(4) 0.014(4) N85 0.082(10) 0.092(14) 0.088(9) 0.075(6) -0.037(6) -0.030(6) C86 0.145(19) 0.094(16) 0.072(9) 0.078(9) -0.018(8) 0.016(7) C87 0.21(3) 0.083(15) 0.092(12) 0.075(13) -0.043(13) 0.005(8) C88 0.17(3) 0.15(3) 0.14(2) 0.120(17) -0.095(17) -0.052(13) C89 0.130(19) 0.13(2) 0.148(18) 0.100(13) -0.104(14) -0.079(12) C90 0.097(14) 0.088(15) 0.092(11) 0.070(9) -0.037(8) -0.042(8) C91 0.034(7) 0.099(16) 0.114(13) 0.049(6) -0.024(7) -0.056(8) C92 0.083(16) 0.18(3) 0.127(18) 0.065(13) 0.007(11) -0.042(13) C93 0.026(7) 0.17(3) 0.17(2) 0.036(9) -0.013(10) -0.128(15) C94 0.040(7) 0.19(3) 0.112(13) 0.027(8) 0.023(7) -0.080(10) C95 0.024(6) 0.110(17) 0.068(9) 0.009(6) 0.002(5) -0.047(7) N96 0.038(6) 0.096(14) 0.056(7) 0.022(5) 0.008(4) -0.025(5) C97 0.041(7) 0.104(16) 0.040(6) -0.000(5) 0.019(4) 0.000(5) C98 0.036(6) 0.080(13) 0.047(6) 0.001(5) 0.022(4) 0.013(5) N99 0.040(5) 0.055(8) 0.030(4) 0.017(3) 0.008(3) 0.012(3) C100 0.045(7) 0.067(11) 0.035(5) -0.001(5) 0.013(4) 0.021(5) C101 0.067(9) 0.075(12) 0.044(6) -0.013(6) 0.004(5) 0.022(5) C102 0.136(18) 0.064(11) 0.055(8) -0.006(8) -0.002(7) 0.033(6) C103 0.090(12) 0.055(10) 0.054(7) 0.007(6) -0.005(6) 0.025(5) C104 0.050(7) 0.054(9) 0.038(5) 0.023(4) 0.003(4) 0.014(4) C105 0.039(6) 0.056(9) 0.034(5) 0.021(4) 0.002(4) 0.004(4) C106 0.048(7) 0.076(12) 0.042(6) 0.035(5) -0.018(4) -0.003(5) C107 0.055(9) 0.124(19) 0.047(7) 0.058(8) -0.010(5) -0.025(7) C108 0.022(5) 0.100(16) 0.064(8) 0.019(5) -0.002(4) -0.019(6) C109 0.035(6) 0.058(10) 0.048(6) 0.013(4) -0.007(4) -0.020(5) N110 0.024(4) 0.045(7) 0.032(4) 0.012(3) 0.007(3) 0.006(3) O111 0.054(6) 0.033(5) 0.056(5) 0.008(3) 0.015(3) 0.014(3) C112 0.087(12) 0.053(10) 0.043(6) -0.006(6) -0.007(6) 0.004(5) O113 0.097(11) 0.038(6) 0.064(6) 0.015(4) -0.010(4) 0.006(3) C114 0.145(18) 0.062(11) 0.033(6) -0.041(8) 0.005(7) -0.001(5) C115 0.135(17) 0.080(14) 0.054(8) -0.052(9) 0.007(8) 0.012(6) C116 0.17(2) 0.12(2) 0.069(10) -0.079(12) 0.038(10) 0.012(9) C117 0.28(5) 0.15(3) 0.070(12) -0.15(3) -0.037(19) 0.053(12) C118 0.28(4) 0.14(2) 0.117(17) -0.12(2) -0.11(2) 0.095(13) C119 0.25(3) 0.034(8) 0.063(9) -0.001(8) -0.023(9) 0.029(6) Cl120 0.054(6) 0.102(14) 0.063(5) 0.017(3) 0.008(3) -0.015(3) Cl121 0.044(5) 0.091(12) 0.040(4) -0.001(3) 0.011(2) -0.017(3) Cl122 0.036(4) 0.091(12) 0.087(7) 0.027(3) 0.007(3) -0.012(3) Cl123 0.116(12) 0.078(11) 0.074(6) -0.001(4) 0.003(4) 0.013(3) Cl124 0.089(9) 0.074(10) 0.113(9) 0.022(3) 0.021(4) 0.026(4) Cl125 0.128(13) 0.128(18) 0.054(5) -0.008(5) 0.010(4) 0.037(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 Fe2 2.9295(15) . . no Fe1 O7 2.020(5) . . no Fe1 O8 2.005(4) . . no Fe1 O9 1.890(5) . . no Fe1 O43 2.058(5) . . no Fe1 N15 2.147(6) . . no Fe1 N26 2.236(6) . . no Fe2 O7 2.008(5) . . no Fe2 O8 1.862(4) . . no Fe2 O13 2.129(5) . . no Fe2 O41 2.032(5) . . no Fe2 N29 2.205(6) . . no Fe2 N40 2.176(6) . . no Fe3 Fe4 2.9471(14) . . no Fe3 Fe6 2.9986(15) . . no Fe3 O9 1.897(5) . . no Fe3 O10 2.043(5) . . no Fe3 O11 1.951(5) . . no Fe3 O78 2.071(5) . . no Fe3 N50 2.178(6) . . no Fe3 N61 2.223(6) . . no Fe4 O8 1.959(5) . . no Fe4 O9 2.042(5) . . no Fe4 O10 1.896(5) . . no Fe4 O76 2.065(5) . . no Fe4 N64 2.230(6) . . no Fe4 N75 2.156(6) . . no Fe5 Fe6 2.9301(16) . . no Fe5 O11 1.854(5) . . no Fe5 O12 1.980(5) . . no Fe5 O14 2.125(6) . . no Fe5 O113 2.048(7) . . no Fe5 N85 2.152(8) . . no Fe5 N96 2.187(9) . . no Fe6 O10 1.894(5) . . no Fe6 O11 2.005(5) . . no Fe6 O12 2.034(5) . . no Fe6 O111 2.035(6) . . no Fe6 N99 2.216(6) . . no Fe6 N110 2.156(6) . . no Cl122 O149 1.66(2) . 1_455 no Cl122 O155 2.41(3) . 1_455 no Cl123 O128 2.321(11) . . no Cl123 O141 2.154(17) . . no Cl123 O148 1.50(2) . 2_666 no Cl124 O151 1.90(3) . . no O41 C42 1.260(8) . . no O43 C42 1.284(9) . . no O76 C77 1.258(8) . . no O78 C77 1.268(8) . . no O111 C112 1.208(12) . . no O113 C112 1.337(12) . . no O128 O142 1.307(16) . 1_556 no O136 O138 1.492(19) . . no O136 O155 1.26(3) . 2_666 no O140 O145 1.87(3) . . no O140 O152 1.57(2) . . no O147 O154 1.86(3) . 2_665 no O147 O154 1.86(3) . 2_665 no N15 C16 1.350(10) . . no N15 C20 1.339(9) . . no N26 C21 1.332(9) . . no N26 C25 1.356(10) . . no N29 C30 1.336(10) . . no N29 C34 1.366(9) . . no N40 C35 1.313(9) . . no N40 C39 1.363(10) . . no N50 C51 1.339(10) . . no N50 C55 1.302(9) . . no N61 C56 1.361(9) . . no N61 C60 1.338(10) . . no N64 C65 1.349(9) . . no N64 C69 1.356(9) . . no N75 C70 1.339(9) . . no N75 C74 1.387(10) . . no N85 C86 1.352(15) . . no N85 C90 1.368(17) . . no N96 C91 1.333(13) . . no N96 C95 1.305(14) . . no N99 C100 1.364(10) . . no N99 C104 1.385(9) . . no N110 C105 1.293(10) . . no N110 C109 1.368(10) . . no C16 C17 1.421(12) . . no C16 H1 0.946(8) . . no C17 C18 1.398(13) . . no C17 H2 0.955(9) . . no C18 C19 1.355(12) . . no C18 H3 0.954(8) . . no C19 C20 1.392(10) . . no C19 H4 0.942(8) . . no C20 C21 1.472(10) . . no C21 C22 1.374(11) . . no C22 C23 1.383(11) . . no C22 H5 0.950(8) . . no C23 C24 1.340(11) . . no C23 H6 0.955(8) . . no C24 C25 1.439(11) . . no C24 H7 0.958(8) . . no C25 C27 1.492(11) . . no C27 C28 1.547(10) . . no C27 H8 0.936(8) . . no C27 H9 0.961(8) . . no C28 C30 1.516(10) . . no C28 H10 0.954(8) . . no C28 H11 0.953(7) . . no C30 C31 1.377(11) . . no C31 C32 1.370(12) . . no C31 H12 0.956(9) . . no C32 C33 1.336(12) . . no C32 H13 0.954(8) . . no C33 C34 1.360(11) . . no C33 H14 0.954(8) . . no C34 C35 1.520(11) . . no C35 C36 1.391(10) . . no C36 C37 1.355(12) . . no C36 H15 0.955(8) . . no C37 C38 1.412(13) . . no C37 H16 0.941(8) . . no C38 C39 1.366(11) . . no C38 H17 0.931(9) . . no C39 H18 0.941(8) . . no C42 C44 1.475(11) . . no C44 C45 1.374(11) . . no C44 C49 1.415(12) . . no C45 C46 1.456(14) . . no C45 H19 0.949(9) . . no C46 C47 1.334(16) . . no C46 H20 0.947(11) . . no C47 C48 1.357(15) . . no C47 H21 0.927(10) . . no C48 C49 1.385(13) . . no C48 H22 0.940(10) . . no C49 H23 0.941(9) . . no C51 C52 1.368(10) . . no C51 H24 0.955(9) . . no C52 C53 1.343(13) . . no C52 H25 0.969(9) . . no C53 C54 1.392(13) . . no C53 H26 0.945(8) . . no C54 C55 1.373(11) . . no C54 H27 0.967(9) . . no C55 C56 1.465(12) . . no C56 C57 1.420(12) . . no C57 C58 1.343(14) . . no C57 H28 0.958(9) . . no C58 C59 1.367(13) . . no C58 H29 0.932(9) . . no C59 C60 1.393(12) . . no C59 H30 0.948(10) . . no C60 C62 1.484(11) . . no C62 C63 1.532(11) . . no C62 H31 0.955(8) . . no C62 H32 0.949(7) . . no C63 C65 1.507(11) . . no C63 H33 0.951(8) . . no C63 H34 0.945(7) . . no C65 C66 1.366(11) . . no C66 C67 1.407(12) . . no C66 H35 0.939(8) . . no C67 C68 1.346(12) . . no C67 H36 0.957(9) . . no C68 C69 1.418(11) . . no C68 H37 0.952(9) . . no C69 C70 1.473(11) . . no C70 C71 1.401(10) . . no C71 C72 1.396(12) . . no C71 H38 0.950(8) . . no C72 C73 1.408(12) . . no C72 H39 0.947(8) . . no C73 C74 1.400(10) . . no C73 H40 0.954(8) . . no C74 H41 0.947(8) . . no C77 C79 1.500(10) . . no C79 C80 1.417(10) . . no C79 C84 1.364(10) . . no C80 C81 1.332(11) . . no C80 H42 0.957(8) . . no C81 C82 1.358(12) . . no C81 H43 0.956(8) . . no C82 C83 1.387(12) . . no C82 H44 0.974(9) . . no C83 C84 1.371(11) . . no C83 H45 0.947(8) . . no C84 H46 0.960(8) . . no C86 C87 1.455(18) . . no C86 H47 0.995(15) . . no C87 C88 1.26(3) . . no C87 H48 1.037(18) . . no C88 C89 1.37(3) . . no C88 H49 0.950(17) . . no C89 C90 1.400(16) . . no C89 H50 0.98(2) . . no C90 C91 1.442(18) . . no C91 C92 1.37(2) . . no C92 C93 1.24(3) . . no C92 H51 0.98(2) . . no C93 C94 1.55(2) . . no C93 H52 0.928(14) . . no C94 C95 1.441(15) . . no C94 H53 0.947(18) . . no C95 C97 1.559(15) . . no C97 C98 1.529(12) . . no C97 H54 0.939(9) . . no C97 H55 0.968(9) . . no C98 C100 1.485(12) . . no C98 H56 0.952(8) . . no C98 H57 0.947(9) . . no C100 C101 1.369(12) . . no C101 C102 1.356(15) . . no C101 H58 0.955(10) . . no C102 C103 1.344(15) . . no C102 H59 0.952(10) . . no C103 C104 1.369(12) . . no C103 H60 0.960(11) . . no C104 C105 1.518(12) . . no C105 C106 1.391(11) . . no C106 C107 1.323(15) . . no C106 H61 0.942(10) . . no C107 C108 1.421(15) . . no C107 H62 0.946(9) . . no C108 C109 1.390(12) . . no C108 H63 0.939(10) . . no C109 H64 0.937(10) . . no C112 C114 1.517(14) . . no C114 C115 1.452(18) . . no C114 C119 1.387(17) . . no C115 C116 1.383(16) . . no C115 H65 0.969(15) . . no C116 C117 1.41(4) . . no C116 H66 0.951(19) . . no C117 C118 1.16(6) . . no C117 H67 0.913(18) . . no C118 C119 1.45(3) . . no C118 H68 0.95(2) . . no C119 H69 0.930(18) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Fe2 Fe1 O7 43.18(13) . . . no Fe2 Fe1 O8 38.96(13) . . . no Fe2 Fe1 O9 117.54(14) . . . no Fe2 Fe1 O43 79.42(14) . . . no Fe2 Fe1 N15 148.36(17) . . . no Fe2 Fe1 N26 109.25(16) . . . no O7 Fe1 O8 79.00(19) . . . no O7 Fe1 O9 160.26(19) . . . no O7 Fe1 O43 86.1(2) . . . no O7 Fe1 N15 108.3(2) . . . no O7 Fe1 N26 85.5(2) . . . no O8 Fe1 O9 81.31(19) . . . no O8 Fe1 O43 95.90(19) . . . no O8 Fe1 N15 172.6(2) . . . no O8 Fe1 N26 105.2(2) . . . no O9 Fe1 O43 94.7(2) . . . no O9 Fe1 N15 91.4(2) . . . no O9 Fe1 N26 101.0(2) . . . no O43 Fe1 N15 86.1(2) . . . no O43 Fe1 N26 155.3(2) . . . no N15 Fe1 N26 74.6(2) . . . no Fe1 Fe2 O7 43.50(14) . . . no Fe1 Fe2 O8 42.63(14) . . . no Fe1 Fe2 O13 131.67(14) . . . no Fe1 Fe2 O41 81.14(14) . . . no Fe1 Fe2 N29 119.36(16) . . . no Fe1 Fe2 N40 136.37(17) . . . no O7 Fe2 O8 82.7(2) . . . no O7 Fe2 O13 89.54(19) . . . no O7 Fe2 O41 88.3(2) . . . no O7 Fe2 N29 110.9(2) . . . no O7 Fe2 N40 172.9(2) . . . no O8 Fe2 O13 170.0(2) . . . no O8 Fe2 O41 98.0(2) . . . no O8 Fe2 N29 94.2(2) . . . no O8 Fe2 N40 99.8(2) . . . no O13 Fe2 O41 88.1(2) . . . no O13 Fe2 N29 82.6(2) . . . no O13 Fe2 N40 88.6(2) . . . no O41 Fe2 N29 158.5(2) . . . no O41 Fe2 N40 84.9(2) . . . no N29 Fe2 N40 75.6(2) . . . no Fe4 Fe3 Fe6 77.32(4) . . . no Fe4 Fe3 O9 43.48(14) . . . no Fe4 Fe3 O10 39.71(14) . . . no Fe4 Fe3 O11 118.68(14) . . . no Fe4 Fe3 O78 80.54(13) . . . no Fe4 Fe3 N50 148.54(17) . . . no Fe4 Fe3 N61 113.03(17) . . . no Fe6 Fe3 O9 120.32(14) . . . no Fe6 Fe3 O10 38.57(13) . . . no Fe6 Fe3 O11 41.40(13) . . . no Fe6 Fe3 O78 89.06(13) . . . no Fe6 Fe3 N50 129.81(17) . . . no Fe6 Fe3 N61 113.40(18) . . . no O9 Fe3 O10 81.83(19) . . . no O9 Fe3 O11 160.45(19) . . . no O9 Fe3 O78 88.0(2) . . . no O9 Fe3 N50 109.1(2) . . . no O9 Fe3 N61 88.9(2) . . . no O10 Fe3 O11 79.34(19) . . . no O10 Fe3 O78 90.05(19) . . . no O10 Fe3 N50 167.3(2) . . . no O10 Fe3 N61 113.6(2) . . . no O11 Fe3 O78 97.1(2) . . . no O11 Fe3 N50 90.3(2) . . . no O11 Fe3 N61 93.9(2) . . . no O78 Fe3 N50 84.0(2) . . . no O78 Fe3 N61 155.4(2) . . . no N50 Fe3 N61 74.0(3) . . . no Fe3 Fe4 O8 118.31(13) . . . no Fe3 Fe4 O9 39.73(13) . . . no Fe3 Fe4 O10 43.50(14) . . . no Fe3 Fe4 O76 79.99(13) . . . no Fe3 Fe4 N64 114.49(15) . . . no Fe3 Fe4 N75 146.13(16) . . . no O8 Fe4 O9 78.77(18) . . . no O8 Fe4 O10 159.24(19) . . . no O8 Fe4 O76 97.93(19) . . . no O8 Fe4 N64 91.5(2) . . . no O8 Fe4 N75 93.0(2) . . . no O9 Fe4 O10 81.87(19) . . . no O9 Fe4 O76 88.44(19) . . . no O9 Fe4 N64 114.9(2) . . . no O9 Fe4 N75 167.6(2) . . . no O10 Fe4 O76 88.9(2) . . . no O10 Fe4 N64 89.9(2) . . . no O10 Fe4 N75 107.3(2) . . . no O76 Fe4 N64 156.2(2) . . . no O76 Fe4 N75 83.4(2) . . . no N64 Fe4 N75 74.3(2) . . . no Fe6 Fe5 O11 42.57(14) . . . no Fe6 Fe5 O12 43.86(14) . . . no Fe6 Fe5 O14 129.57(18) . . . no Fe6 Fe5 O113 81.6(2) . . . no Fe6 Fe5 N85 138.7(3) . . . no Fe6 Fe5 N96 119.8(3) . . . no O11 Fe5 O12 83.5(2) . . . no O11 Fe5 O14 171.7(2) . . . no O11 Fe5 O113 94.9(2) . . . no O11 Fe5 N85 100.7(3) . . . no O11 Fe5 N96 98.3(3) . . . no O12 Fe5 O14 88.2(2) . . . no O12 Fe5 O113 90.8(2) . . . no O12 Fe5 N85 174.3(3) . . . no O12 Fe5 N96 107.8(3) . . . no O14 Fe5 O113 85.3(3) . . . no O14 Fe5 N85 87.6(3) . . . no O14 Fe5 N96 84.0(3) . . . no O113 Fe5 N85 85.0(4) . . . no O113 Fe5 N96 158.1(3) . . . no N85 Fe5 N96 75.6(4) . . . no Fe3 Fe6 Fe5 78.41(4) . . . no Fe3 Fe6 O10 42.27(14) . . . no Fe3 Fe6 O11 40.05(14) . . . no Fe3 Fe6 O12 118.07(14) . . . no Fe3 Fe6 O111 101.75(17) . . . no Fe3 Fe6 N99 100.79(17) . . . no Fe3 Fe6 N110 134.33(17) . . . no Fe5 Fe6 O10 118.19(14) . . . no Fe5 Fe6 O11 38.70(14) . . . no Fe5 Fe6 O12 42.41(13) . . . no Fe5 Fe6 O111 79.34(17) . . . no Fe5 Fe6 N99 109.95(17) . . . no Fe5 Fe6 N110 146.65(17) . . . no O10 Fe6 O11 81.66(19) . . . no O10 Fe6 O12 160.10(19) . . . no O10 Fe6 O111 94.8(2) . . . no O10 Fe6 N99 98.7(2) . . . no O10 Fe6 N110 92.7(2) . . . no O11 Fe6 O12 78.45(19) . . . no O11 Fe6 O111 94.3(2) . . . no O11 Fe6 N99 106.0(2) . . . no O11 Fe6 N110 174.3(2) . . . no O12 Fe6 O111 86.1(2) . . . no O12 Fe6 N99 87.4(2) . . . no O12 Fe6 N110 107.2(2) . . . no O111 Fe6 N99 157.0(2) . . . no O111 Fe6 N110 86.2(2) . . . no N99 Fe6 N110 74.6(2) . . . no O149 Cl122 O155 88.5(11) 1_455 . 1_455 no O128 Cl123 O141 148.2(6) . . . no O128 Cl123 O148 103.7(9) . . 2_666 no O141 Cl123 O148 97.0(10) . . 2_666 no Fe1 O7 Fe2 93.3(2) . . . no Fe1 O8 Fe2 98.4(2) . . . no Fe1 O8 Fe4 98.37(19) . . . no Fe2 O8 Fe4 160.7(3) . . . no Fe1 O9 Fe3 156.7(3) . . . no Fe1 O9 Fe4 99.4(2) . . . no Fe3 O9 Fe4 96.8(2) . . . no Fe3 O10 Fe4 96.8(2) . . . no Fe3 O10 Fe6 99.2(2) . . . no Fe4 O10 Fe6 157.1(3) . . . no Fe3 O11 Fe5 160.1(3) . . . no Fe3 O11 Fe6 98.5(2) . . . no Fe5 O11 Fe6 98.7(2) . . . no Fe5 O12 Fe6 93.7(2) . . . no Fe2 O41 C42 127.8(5) . . . no Fe1 O43 C42 128.2(5) . . . no Fe4 O76 C77 127.1(5) . . . no Fe3 O78 C77 126.0(4) . . . no Fe6 O111 C112 129.8(7) . . . no Fe5 O113 C112 123.6(6) . . . no Cl123 O128 O142 120.8(9) . . 1_556 no O138 O136 O155 117.6(18) . . 2_666 no O145 O140 O152 155.6(16) . . . no Cl122 O155 O136 113.6(18) 1_655 . 2_666 no Fe1 N15 C16 122.1(5) . . . no Fe1 N15 C20 116.7(5) . . . no C16 N15 C20 120.2(7) . . . no Fe1 N26 C21 114.1(5) . . . no Fe1 N26 C25 127.0(5) . . . no C21 N26 C25 118.7(7) . . . no Fe2 N29 C30 126.4(5) . . . no Fe2 N29 C34 115.4(5) . . . no C30 N29 C34 118.1(7) . . . no Fe2 N40 C35 117.2(5) . . . no Fe2 N40 C39 123.5(5) . . . no C35 N40 C39 119.2(7) . . . no Fe3 N50 C51 123.3(5) . . . no Fe3 N50 C55 118.7(5) . . . no C51 N50 C55 117.0(7) . . . no Fe3 N61 C56 113.8(6) . . . no Fe3 N61 C60 125.7(5) . . . no C56 N61 C60 120.0(7) . . . no Fe4 N64 C65 126.0(5) . . . no Fe4 N64 C69 114.3(5) . . . no C65 N64 C69 119.4(7) . . . no Fe4 N75 C70 119.0(5) . . . no Fe4 N75 C74 122.9(5) . . . no C70 N75 C74 117.3(6) . . . no Fe5 N85 C86 123.5(9) . . . no Fe5 N85 C90 115.5(10) . . . no C86 N85 C90 121.0(11) . . . no Fe5 N96 C91 114.9(10) . . . no Fe5 N96 C95 126.3(7) . . . no C91 N96 C95 118.5(11) . . . no Fe6 N99 C100 129.0(6) . . . no Fe6 N99 C104 114.2(5) . . . no C100 N99 C104 116.6(7) . . . no Fe6 N110 C105 118.2(5) . . . no Fe6 N110 C109 121.4(6) . . . no C105 N110 C109 119.2(7) . . . no N15 C16 C17 120.3(8) . . . no N15 C16 H1 120.2(8) . . . no C17 C16 H1 119.5(9) . . . no C16 C17 C18 118.8(8) . . . no C16 C17 H2 120.4(11) . . . no C18 C17 H2 120.9(10) . . . no C17 C18 C19 118.6(8) . . . no C17 C18 H3 119.4(9) . . . no C19 C18 H3 122.0(9) . . . no C18 C19 C20 120.9(8) . . . no C18 C19 H4 119.1(8) . . . no C20 C19 H4 120.0(9) . . . no N15 C20 C19 120.8(7) . . . no N15 C20 C21 115.2(7) . . . no C19 C20 C21 124.0(7) . . . no N26 C21 C20 116.8(7) . . . no N26 C21 C22 122.1(7) . . . no C20 C21 C22 121.0(7) . . . no C21 C22 C23 120.5(7) . . . no C21 C22 H5 121.0(9) . . . no C23 C22 H5 118.5(9) . . . no C22 C23 C24 118.6(8) . . . no C22 C23 H6 120.6(8) . . . no C24 C23 H6 120.8(9) . . . no C23 C24 C25 119.6(8) . . . no C23 C24 H7 120.0(8) . . . no C25 C24 H7 120.4(8) . . . no N26 C25 C24 120.3(7) . . . no N26 C25 C27 121.0(7) . . . no C24 C25 C27 118.7(7) . . . no C25 C27 C28 114.8(6) . . . no C25 C27 H8 108.1(7) . . . no C25 C27 H9 107.4(7) . . . no C28 C27 H8 109.1(7) . . . no C28 C27 H9 107.7(7) . . . no H8 C27 H9 109.7(8) . . . no C27 C28 C30 107.4(6) . . . no C27 C28 H10 110.6(7) . . . no C27 C28 H11 109.7(7) . . . no C30 C28 H10 110.0(7) . . . no C30 C28 H11 110.4(7) . . . no H10 C28 H11 108.9(8) . . . no N29 C30 C28 116.9(6) . . . no N29 C30 C31 120.8(8) . . . no C28 C30 C31 122.1(8) . . . no C30 C31 C32 120.6(8) . . . no C30 C31 H12 119.7(10) . . . no C32 C31 H12 119.7(9) . . . no C31 C32 C33 118.4(7) . . . no C31 C32 H13 120.6(10) . . . no C33 C32 H13 121.0(9) . . . no C32 C33 C34 120.8(8) . . . no C32 C33 H14 120.7(8) . . . no C34 C33 H14 118.6(9) . . . no N29 C34 C33 121.5(8) . . . no N29 C34 C35 114.7(7) . . . no C33 C34 C35 123.8(7) . . . no N40 C35 C34 116.9(7) . . . no N40 C35 C36 121.8(7) . . . no C34 C35 C36 121.4(7) . . . no C35 C36 C37 118.9(8) . . . no C35 C36 H15 120.0(9) . . . no C37 C36 H15 121.1(9) . . . no C36 C37 C38 120.8(8) . . . no C36 C37 H16 119.6(10) . . . no C38 C37 H16 119.6(10) . . . no C37 C38 C39 116.2(9) . . . no C37 C38 H17 121.6(8) . . . no C39 C38 H17 122.2(9) . . . no N40 C39 C38 123.1(8) . . . no N40 C39 H18 118.0(8) . . . no C38 C39 H18 118.9(9) . . . no O41 C42 O43 123.4(7) . . . no O41 C42 C44 118.1(7) . . . no O43 C42 C44 118.5(7) . . . no C42 C44 C45 117.7(8) . . . no C42 C44 C49 120.0(7) . . . no C45 C44 C49 122.2(8) . . . no C44 C45 C46 114.4(9) . . . no C44 C45 H19 122.5(8) . . . no C46 C45 H19 123.1(9) . . . no C45 C46 C47 124.7(10) . . . no C45 C46 H20 116.9(15) . . . no C47 C46 H20 118.4(13) . . . no C46 C47 C48 117.8(10) . . . no C46 C47 H21 121.4(14) . . . no C48 C47 H21 120.8(13) . . . no C47 C48 C49 123.0(10) . . . no C47 C48 H22 118.4(12) . . . no C49 C48 H22 118.6(12) . . . no C44 C49 C48 117.8(9) . . . no C44 C49 H23 121.3(8) . . . no C48 C49 H23 120.9(10) . . . no N50 C51 C52 125.1(8) . . . no N50 C51 H24 117.5(7) . . . no C52 C51 H24 117.4(9) . . . no C51 C52 C53 116.5(9) . . . no C51 C52 H25 120.7(9) . . . no C53 C52 H25 122.8(8) . . . no C52 C53 C54 120.5(8) . . . no C52 C53 H26 117.3(11) . . . no C54 C53 H26 122.1(11) . . . no C53 C54 C55 117.8(8) . . . no C53 C54 H27 121.4(9) . . . no C55 C54 H27 120.8(10) . . . no N50 C55 C54 123.1(8) . . . no N50 C55 C56 115.2(7) . . . no C54 C55 C56 121.6(8) . . . no N61 C56 C55 116.8(7) . . . no N61 C56 C57 118.2(9) . . . no C55 C56 C57 124.9(8) . . . no C56 C57 C58 123.2(9) . . . no C56 C57 H28 116.8(11) . . . no C58 C57 H28 119.9(10) . . . no C57 C58 C59 115.9(9) . . . no C57 C58 H29 121.3(10) . . . no C59 C58 H29 122.7(11) . . . no C58 C59 C60 122.5(9) . . . no C58 C59 H30 118.1(10) . . . no C60 C59 H30 119.4(9) . . . no N61 C60 C59 120.1(8) . . . no N61 C60 C62 118.9(7) . . . no C59 C60 C62 120.9(8) . . . no C60 C62 C63 113.0(7) . . . no C60 C62 H31 108.2(7) . . . no C60 C62 H32 109.0(7) . . . no C63 C62 H31 108.4(7) . . . no C63 C62 H32 109.0(7) . . . no H31 C62 H32 109.1(8) . . . no C62 C63 C65 110.9(6) . . . no C62 C63 H33 108.8(7) . . . no C62 C63 H34 109.4(7) . . . no C65 C63 H33 109.1(7) . . . no C65 C63 H34 108.9(7) . . . no H33 C63 H34 109.8(8) . . . no N64 C65 C63 117.1(6) . . . no N64 C65 C66 122.9(8) . . . no C63 C65 C66 119.7(7) . . . no C65 C66 C67 117.4(8) . . . no C65 C66 H35 121.1(9) . . . no C67 C66 H35 121.4(9) . . . no C66 C67 C68 120.9(8) . . . no C66 C67 H36 119.4(10) . . . no C68 C67 H36 119.7(10) . . . no C67 C68 C69 119.1(8) . . . no C67 C68 H37 119.6(9) . . . no C69 C68 H37 121.3(10) . . . no N64 C69 C68 120.0(8) . . . no N64 C69 C70 116.8(7) . . . no C68 C69 C70 123.2(8) . . . no N75 C70 C69 114.5(6) . . . no N75 C70 C71 124.9(7) . . . no C69 C70 C71 120.6(7) . . . no C70 C71 C72 117.2(7) . . . no C70 C71 H38 121.4(8) . . . no C72 C71 H38 121.4(8) . . . no C71 C72 C73 119.9(7) . . . no C71 C72 H39 120.4(10) . . . no C73 C72 H39 119.7(10) . . . no C72 C73 C74 118.9(8) . . . no C72 C73 H40 121.1(9) . . . no C74 C73 H40 120.0(9) . . . no N75 C74 C73 121.6(7) . . . no N75 C74 H41 118.9(7) . . . no C73 C74 H41 119.5(8) . . . no O76 C77 O78 126.0(7) . . . no O76 C77 C79 118.4(6) . . . no O78 C77 C79 115.6(6) . . . no C77 C79 C80 121.0(7) . . . no C77 C79 C84 121.4(7) . . . no C80 C79 C84 117.6(7) . . . no C79 C80 C81 122.5(7) . . . no C79 C80 H42 118.3(8) . . . no C81 C80 H42 119.2(8) . . . no C80 C81 C82 119.6(8) . . . no C80 C81 H43 120.8(9) . . . no C82 C81 H43 119.6(9) . . . no C81 C82 C83 119.4(8) . . . no C81 C82 H44 120.2(10) . . . no C83 C82 H44 120.4(10) . . . no C82 C83 C84 121.3(8) . . . no C82 C83 H45 119.3(9) . . . no C84 C83 H45 119.4(9) . . . no C79 C84 C83 119.5(8) . . . no C79 C84 H46 120.4(8) . . . no C83 C84 H46 120.1(8) . . . no N85 C86 C87 113.4(14) . . . no N85 C86 H47 122.5(11) . . . no C87 C86 H47 124.1(15) . . . no C86 C87 C88 126(2) . . . no C86 C87 H48 111.8(19) . . . no C88 C87 H48 122(2) . . . no C87 C88 C89 119.8(17) . . . no C87 C88 H49 113(3) . . . no C89 C88 H49 127(3) . . . no C88 C89 C90 117(2) . . . no C88 C89 H50 121.2(17) . . . no C90 C89 H50 122(2) . . . no N85 C90 C89 122.3(17) . . . no N85 C90 C91 116.2(10) . . . no C89 C90 C91 121.6(16) . . . no N96 C91 C90 117.3(11) . . . no N96 C91 C92 123.4(17) . . . no C90 C91 C92 119.0(15) . . . no C91 C92 C93 119(2) . . . no C91 C92 H51 117(2) . . . no C93 C92 H51 124(2) . . . no C92 C93 C94 125.3(17) . . . no C92 C93 H52 115(3) . . . no C94 C93 H52 120(2) . . . no C93 C94 C95 107.2(15) . . . no C93 C94 H53 125.9(12) . . . no C95 C94 H53 127.0(14) . . . no N96 C95 C94 126.5(12) . . . no N96 C95 C97 120.0(8) . . . no C94 C95 C97 113.0(13) . . . no C95 C97 C98 108.9(7) . . . no C95 C97 H54 112.0(10) . . . no C95 C97 H55 109.5(9) . . . no C98 C97 H54 109.5(8) . . . no C98 C97 H55 108.0(9) . . . no H54 C97 H55 108.9(9) . . . no C97 C98 C100 115.3(8) . . . no C97 C98 H56 107.8(7) . . . no C97 C98 H57 106.8(9) . . . no C100 C98 H56 108.4(9) . . . no C100 C98 H57 108.8(7) . . . no H56 C98 H57 109.6(9) . . . no N99 C100 C98 118.8(7) . . . no N99 C100 C101 120.7(9) . . . no C98 C100 C101 120.5(8) . . . no C100 C101 C102 121.8(9) . . . no C100 C101 H58 119.7(11) . . . no C102 C101 H58 118.5(11) . . . no C101 C102 C103 118.5(10) . . . no C101 C102 H59 121.5(14) . . . no C103 C102 H59 120.0(15) . . . no C102 C103 C104 120.3(10) . . . no C102 C103 H60 120.7(11) . . . no C104 C103 H60 119.0(11) . . . no N99 C104 C103 121.9(9) . . . no N99 C104 C105 113.6(7) . . . no C103 C104 C105 124.0(8) . . . no N110 C105 C104 116.5(7) . . . no N110 C105 C106 123.4(8) . . . no C104 C105 C106 120.1(8) . . . no C105 C106 C107 117.3(10) . . . no C105 C106 H61 121.3(10) . . . no C107 C106 H61 121.4(10) . . . no C106 C107 C108 123.4(9) . . . no C106 C107 H62 116.7(14) . . . no C108 C107 H62 119.9(13) . . . no C107 C108 C109 114.4(9) . . . no C107 C108 H63 121.6(11) . . . no C109 C108 H63 124.0(13) . . . no N110 C109 C108 122.4(9) . . . no N110 C109 H64 118.4(8) . . . no C108 C109 H64 119.2(10) . . . no O111 C112 O113 125.0(10) . . . no O111 C112 C114 123.2(12) . . . no O113 C112 C114 111.7(11) . . . no C112 C114 C115 115.2(12) . . . no C112 C114 C119 121.8(14) . . . no C115 C114 C119 122.8(12) . . . no C114 C115 C116 117.6(15) . . . no C114 C115 H65 122.3(12) . . . no C116 C115 H65 120.1(18) . . . no C115 C116 C117 117(2) . . . no C115 C116 H66 119(2) . . . no C117 C116 H66 124.3(19) . . . no C116 C117 C118 122(2) . . . no C116 C117 H67 119(4) . . . no C118 C117 H67 119(5) . . . no C117 C118 C119 128(3) . . . no C117 C118 H68 117(3) . . . no C119 C118 H68 115(3) . . . no C114 C119 C118 109.9(19) . . . no C114 C119 H69 123.8(13) . . . no C118 C119 H69 126.3(18) . . . no #===END ############################################################################## # IUMSC CIF Archive file # ############################################################################## data_MSC98201 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C22 H18 Fe2 N8 O13' _chemical_formula_moiety 'C22 H18 Fe2 N8 O13' _chemical_formula_weight 714.125 _cell_length_a 8.759(2) _cell_length_b 18.811(6) _cell_length_c 16.618(5) _cell_angle_alpha 90 _cell_angle_beta 104.750(15) _cell_angle_gamma 90 _cell_volume 2647.7(22) _cell_formula_units_Z 4 _cell_measurement_reflns_used 60 _cell_measurement_theta_min 9.65 _cell_measurement_theta_max 15.15 _cell_measurement_temperature 107 _exptl_crystal_colour red _exptl_crystal_description prism _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 1.1808 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa _exptl_absorpt_correction_T_min 0.882 _exptl_absorpt_correction_T_max 0.945 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z x,1/2-y,1/2+z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 107 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5921 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_min 3.01745 _diffrn_reflns_theta_max 25.0521 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 4 _diffrn_standards_number 4 _diffrn_standards_decay_% -0.6 _diffrn_standards_interval_count 300 _reflns_number_total 4689 _reflns_number_gt 3121 _reflns_threshold_expression F^2^>2.0\s(F^2^) _atom_sites_solution_primary direct _atom_sites_solution_hydrogen geom loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.301 0.845 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_special_details ; The structure was solved using DIRDIF-96. The solution contained all of the non-hydrogen atoms in the molecule. Hydrogen atoms were introduced in fixed calculated positions and assigned isotropic thermal parameters equal to 1.0 plus the isotropic equivalent of the parent atom. The full matrix least-squares refinement was completed usimg anisotropic thermal parameters on all of the non-hydrogen atoms. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 3121 _refine_ls_number_parameters 407 _refine_ls_hydrogen_treatment noref _refine_ls_extinction_coef 0.00000013(6) _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.07F)^2^ _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.0476 _refine_ls_goodness_of_fit_ref 0.9517 _refine_ls_shift/su_max 0.0036 _refine_diff_density_max 0.31 _refine_diff_density_min -0.39 _computing_data_collection 'NPS, local program' _computing_cell_refinement 'XTEL, local package' _computing_data_reduction 'XTEL, local package' _computing_structure_solution DIRDIF-96 _computing_structure_refinement 'XTEL, local package' _computing_molecular_graphics 'XTEL, local package' _computing_publication_material 'XTEL, local package' 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_disorder_group _atom_site_disorder_assembly Fe1 Fe 0.12186(10) 0.11859(4) 0.32507(5) 0.0127(3) Uani 1 0 . Fe2 Fe 0.36620(10) 0.10299(4) 0.19031(5) 0.0129(3) Uani 1 0 . O3 O 0.2168(4) 0.1000(2) 0.2446(2) 0.0158(14) Uani 1 0 . N4 N 0.0056(5) 0.1349(2) 0.4212(3) 0.0132(16) Uani 1 0 . C5 C 0.0249(7) 0.1934(3) 0.4691(4) 0.0176(19) Uani 1 0 . C6 C -0.0525(7) 0.2034(3) 0.5309(3) 0.0159(19) Uani 1 0 . C7 C -0.1572(7) 0.1517(3) 0.5421(3) 0.018(2) Uani 1 0 . C8 C -0.1785(6) 0.0910(3) 0.4933(3) 0.0143(18) Uani 1 0 . C9 C -0.0939(6) 0.0839(3) 0.4338(3) 0.0133(18) Uani 1 0 . C10 C -0.1040(7) 0.0195(3) 0.3808(3) 0.0145(19) Uani 1 0 . C11 C -0.2043(7) -0.0364(3) 0.3861(4) 0.018(2) Uani 1 0 . C12 C -0.2009(7) -0.0970(3) 0.3397(4) 0.0180(19) Uani 1 0 . C13 C -0.0993(7) -0.0997(3) 0.2878(3) 0.0150(18) Uani 1 0 . C14 C -0.0040(7) -0.0417(3) 0.2831(4) 0.0164(19) Uani 1 0 . N15 N -0.0057(5) 0.0174(2) 0.3287(3) 0.0135(16) Uani 1 0 . C16 C 0.1069(7) -0.0466(3) 0.2263(4) 0.019(2) Uani 1 0 . C17 C 0.2804(7) -0.0539(3) 0.2761(4) 0.017(2) Uani 1 0 . N18 N 0.4463(6) -0.0071(2) 0.1879(3) 0.0140(16) Uani 1 0 . C19 C 0.3912(7) -0.0646(3) 0.2212(4) 0.0162(19) Uani 1 0 . C20 C 0.4370(7) -0.1330(3) 0.2068(4) 0.0176(19) Uani 1 0 . C21 C 0.5433(7) -0.1441(3) 0.1589(4) 0.020(2) Uani 1 0 . C22 C 0.6031(7) -0.0851(3) 0.1268(4) 0.019(2) Uani 1 0 . C23 C 0.5520(7) -0.0173(3) 0.1418(3) 0.0152(19) Uani 1 0 . C24 C 0.6063(6) 0.0466(3) 0.1060(3) 0.0132(18) Uani 1 0 . C25 C 0.7223(7) 0.0457(3) 0.0624(4) 0.022(2) Uani 1 0 . C26 C 0.7556(7) 0.1069(3) 0.0239(4) 0.025(2) Uani 1 0 . C27 C 0.6754(7) 0.1682(3) 0.0313(4) 0.022(2) Uani 1 0 . C28 C 0.5662(7) 0.1675(3) 0.0786(4) 0.020(2) Uani 1 0 . N29 N 0.5320(6) 0.1078(2) 0.1153(3) 0.0162(16) Uani 1 0 . O30 O 0.3180(5) 0.1773(2) 0.4045(3) 0.0193(14) Uani 1 0 . N31 N 0.3694(6) 0.1249(3) 0.4524(3) 0.0188(18) Uani 1 0 . O32 O 0.2996(5) 0.0660(2) 0.4289(2) 0.0188(14) Uani 1 0 . O33 O 0.4742(5) 0.1308(2) 0.5165(3) 0.0274(16) Uani 1 0 . O34 O 0.0624(5) 0.2285(2) 0.2923(2) 0.0193(14) Uani 1 0 . N35 N -0.0754(6) 0.2138(3) 0.2468(3) 0.0189(18) Uani 1 0 . O36 O -0.1102(5) 0.1478(2) 0.2408(2) 0.0196(14) Uani 1 0 . O37 O -0.1681(5) 0.2598(2) 0.2111(3) 0.0240(15) Uani 1 0 . O38 O 0.5628(5) 0.1057(2) 0.3014(2) 0.0175(13) Uani 1 0 . N39 N 0.5677(6) 0.1736(3) 0.3006(3) 0.0151(16) Uani 1 0 . O40 O 0.4665(5) 0.20299(19) 0.2400(2) 0.0160(14) Uani 1 0 . O41 O 0.6610(5) 0.2084(2) 0.3528(2) 0.0200(14) Uani 1 0 . O42 O 0.2068(5) 0.0631(2) 0.0729(2) 0.0179(14) Uani 1 0 . N43 N 0.1738(6) 0.1255(3) 0.0441(3) 0.0171(17) Uani 1 0 . O44 O 0.2322(5) 0.1759(2) 0.0936(2) 0.0184(14) Uani 1 0 . O45 O 0.0966(5) 0.1361(2) -0.0274(3) 0.0234(15) Uani 1 0 . H1 H 0.095 0.2294 0.4601 0.0305 Uiso 1 0 . H2 H -0.0342 0.2448 0.565 0.0285 Uiso 1 0 . H3 H -0.2149 0.1578 0.583 0.0307 Uiso 1 0 . H4 H -0.2505 0.0552 0.5003 0.027 Uiso 1 0 . H5 H -0.2743 -0.0331 0.4213 0.0304 Uiso 1 0 . H6 H -0.2674 -0.1361 0.343 0.0309 Uiso 1 0 . H7 H -0.0949 -0.1412 0.2558 0.0276 Uiso 1 0 . H8 H 0.0788 -0.0867 0.1911 0.0315 Uiso 1 0 . H9 H 0.0962 -0.0046 0.1933 0.0315 Uiso 1 0 . H10 H 0.3106 -0.012 0.308 0.03 Uiso 1 0 . H11 H 0.2891 -0.0936 0.3123 0.03 Uiso 1 0 . H12 H 0.3954 -0.1725 0.2299 0.0306 Uiso 1 0 . H13 H 0.5747 -0.1908 0.1482 0.0324 Uiso 1 0 . H14 H 0.6783 -0.0908 0.0949 0.0318 Uiso 1 0 . H15 H 0.7785 0.0031 0.0589 0.0351 Uiso 1 0 . H16 H 0.8327 0.1064 -0.0072 0.0378 Uiso 1 0 . H17 H 0.6951 0.2107 0.0046 0.0345 Uiso 1 0 . H18 H 0.5131 0.2104 0.0852 0.0322 Uiso 1 0 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.0128(7) 0.012(3) 0.015(2) -0.0006(4) 0.0058(3) -0.0006(3) Fe2 0.0141(7) 0.011(2) 0.014(2) 0.0001(4) 0.0052(3) -0.0003(3) O3 0.015(2) 0.018(4) 0.016(3) 0.0011(17) 0.0053(18) -0.0012(17) N4 0.014(3) 0.014(4) 0.014(3) 0.002(2) 0.007(2) 0.000(2) C5 0.015(3) 0.015(4) 0.021(5) -0.002(2) 0.000(3) 0.000(2) C6 0.013(3) 0.018(5) 0.015(4) 0.001(2) -0.000(2) -0.003(2) C7 0.016(3) 0.025(6) 0.013(4) 0.010(3) 0.003(2) 0.007(3) C8 0.010(3) 0.015(4) 0.016(4) 0.001(2) 0.001(2) -0.002(2) C9 0.009(3) 0.020(5) 0.009(3) 0.003(2) -0.001(2) 0.000(2) C10 0.011(3) 0.016(5) 0.017(4) 0.004(2) 0.006(2) 0.005(2) C11 0.015(3) 0.024(6) 0.016(4) 0.003(3) 0.007(3) 0.007(3) C12 0.014(3) 0.018(5) 0.020(4) 0.001(2) 0.000(3) 0.002(3) C13 0.013(3) 0.015(4) 0.015(4) 0.001(2) 0.000(2) 0.000(2) C14 0.018(3) 0.013(4) 0.015(4) 0.003(2) -0.003(2) 0.000(2) N15 0.012(3) 0.013(4) 0.015(3) 0.0039(19) 0.004(2) 0.003(2) C16 0.018(3) 0.016(5) 0.021(5) -0.001(3) 0.004(3) -0.002(3) C17 0.025(4) 0.011(4) 0.017(4) 0.003(2) 0.009(3) -0.000(2) N18 0.015(3) 0.015(4) 0.011(3) -0.000(2) 0.002(2) -0.004(2) C19 0.013(3) 0.016(5) 0.019(4) 0.002(2) 0.004(2) -0.000(2) C20 0.015(3) 0.018(5) 0.019(4) -0.003(2) 0.003(2) -0.002(2) C21 0.023(4) 0.015(4) 0.019(4) 0.007(3) -0.001(3) -0.001(2) C22 0.015(3) 0.025(6) 0.019(4) 0.002(3) 0.008(3) -0.008(3) C23 0.011(3) 0.019(5) 0.014(4) 0.004(2) 0.002(2) -0.001(2) C24 0.012(3) 0.014(4) 0.012(3) -0.002(2) -0.000(2) -0.004(2) C25 0.026(4) 0.024(6) 0.020(5) -0.009(3) 0.009(3) -0.010(3) C26 0.019(3) 0.035(8) 0.022(5) -0.006(3) 0.007(3) -0.007(3) C27 0.021(4) 0.022(6) 0.022(5) -0.007(3) 0.003(3) 0.003(3) C28 0.017(3) 0.023(6) 0.017(4) -0.006(3) 0.002(3) 0.000(3) N29 0.014(3) 0.020(5) 0.013(3) -0.005(2) 0.001(2) -0.001(2) O30 0.018(2) 0.020(5) 0.023(4) -0.0025(19) 0.0094(19) -0.0025(19) N31 0.014(3) 0.026(6) 0.019(4) 0.003(2) 0.008(2) -0.001(2) O32 0.015(2) 0.021(5) 0.019(4) -0.0006(18) 0.0026(18) 0.0005(18) O33 0.017(3) 0.041(9) 0.020(4) 0.000(2) -0.0029(19) -0.003(2) O34 0.016(2) 0.020(5) 0.020(4) -0.0057(18) 0.0025(19) 0.0003(18) N35 0.021(3) 0.022(5) 0.016(4) 0.004(2) 0.008(2) 0.001(2) O36 0.019(2) 0.014(4) 0.024(5) -0.0025(18) 0.0028(19) -0.0006(18) O37 0.023(3) 0.026(6) 0.023(4) 0.007(2) 0.007(2) 0.007(2) O38 0.021(2) 0.009(3) 0.021(4) 0.0016(17) 0.0039(18) 0.0002(17) N39 0.012(3) 0.020(5) 0.015(3) 0.005(2) 0.006(2) 0.003(2) O40 0.017(2) 0.012(3) 0.018(4) 0.0002(17) 0.0033(18) 0.0023(17) O41 0.017(2) 0.022(5) 0.018(4) -0.0040(18) -0.0006(19) -0.0040(18) O42 0.021(3) 0.015(4) 0.018(4) 0.0014(18) 0.0050(18) -0.0014(17) N43 0.014(3) 0.023(6) 0.017(4) -0.000(2) 0.009(2) 0.001(2) O44 0.018(2) 0.018(4) 0.019(4) -0.0036(18) 0.0042(18) -0.0031(18) O45 0.018(3) 0.033(8) 0.017(3) 0.0009(19) 0.0003(19) 0.0011(19) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 Fe2 3.482(1) . . no Fe1 O3 1.779(4) . . no Fe1 O30 2.182(4) . . no Fe1 O32 2.239(4) . . no Fe1 O34 2.167(4) . . no Fe1 O36 2.223(4) . . no Fe1 N4 2.124(4) . . no Fe1 N15 2.217(5) . . no Fe2 O3 1.770(4) . . no Fe2 O38 2.181(4) . . no Fe2 O40 2.150(4) . . no Fe2 O42 2.221(4) . . no Fe2 O44 2.210(4) . . no Fe2 N18 2.190(5) . . no Fe2 N29 2.143(5) . . no O30 N31 1.275(6) . . no O32 N31 1.278(6) . . no O33 N31 1.221(6) . . no O34 N35 1.281(6) . . no O36 N35 1.276(6) . . no O37 N35 1.231(6) . . no O38 N39 1.279(6) . . no O40 N39 1.284(6) . . no O41 N39 1.220(6) . . no O42 N43 1.273(6) . . no O44 N43 1.274(6) . . no O45 N43 1.224(6) . . no N4 C5 1.344(7) . . no N4 C9 1.348(7) . . no N15 C10 1.368(7) . . no N15 C14 1.347(7) . . no N18 C19 1.358(7) . . no N18 C23 1.358(7) . . no N29 C24 1.350(7) . . no N29 C28 1.347(7) . . no C5 C6 1.380(8) . . no C5 H1 0.951(6) . . no C6 C7 1.381(8) . . no C6 H2 0.951(6) . . no C7 C8 1.385(8) . . no C7 H3 0.952(6) . . no C8 C9 1.385(8) . . no C8 H4 0.951(5) . . no C9 C10 1.486(8) . . no C10 C11 1.387(8) . . no C11 C12 1.381(8) . . no C11 H5 0.951(6) . . no C12 C13 1.389(8) . . no C12 H6 0.949(6) . . no C13 C14 1.389(8) . . no C13 H7 0.951(6) . . no C14 C16 1.519(8) . . no C16 C17 1.540(8) . . no C16 H8 0.949(6) . . no C16 H9 0.952(6) . . no C17 C19 1.504(8) . . no C17 H10 0.950(6) . . no C17 H11 0.950(6) . . no C19 C20 1.387(8) . . no C20 C21 1.387(8) . . no C20 H12 0.951(6) . . no C21 C22 1.391(8) . . no C21 H13 0.951(6) . . no C22 C23 1.394(8) . . no C22 H14 0.951(6) . . no C23 C24 1.473(8) . . no C24 C25 1.391(8) . . no C25 C26 1.383(9) . . no C25 H15 0.950(6) . . no C26 C27 1.371(9) . . no C26 H16 0.950(6) . . no C27 C28 1.384(8) . . no C27 H17 0.952(6) . . no C28 H18 0.952(6) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Fe2 Fe1 O30 85.04(11) . . . no Fe2 Fe1 O32 92.15(11) . . . no Fe2 Fe1 O34 93.83(11) . . . no Fe2 Fe1 O36 103.22(11) . . . no Fe2 Fe1 N4 170.71(13) . . . no Fe2 Fe1 N15 109.99(12) . . . no Fe1 Fe2 O38 86.32(11) . . . no Fe1 Fe2 O40 86.39(11) . . . no Fe1 Fe2 O42 103.99(11) . . . no Fe1 Fe2 O44 96.65(11) . . . no Fe1 Fe2 N18 110.10(12) . . . no Fe1 Fe2 N29 171.52(13) . . . no O3 Fe1 O30 96.17(16) . . . no O3 Fe1 O32 97.24(16) . . . no O3 Fe1 O34 97.29(17) . . . no O3 Fe1 O36 95.87(16) . . . no O3 Fe1 N4 176.95(18) . . . no O3 Fe1 N15 100.79(17) . . . no O30 Fe1 O32 58.10(15) . . . no O30 Fe1 O34 76.74(15) . . . no O30 Fe1 O36 135.10(15) . . . no O30 Fe1 N4 85.78(16) . . . no O30 Fe1 N15 138.03(17) . . . no O32 Fe1 O34 133.68(15) . . . no O32 Fe1 O36 159.96(15) . . . no O32 Fe1 N4 81.78(16) . . . no O32 Fe1 N15 81.72(16) . . . no O34 Fe1 O36 58.89(14) . . . no O34 Fe1 N4 85.42(16) . . . no O34 Fe1 N15 137.36(16) . . . no O36 Fe1 N4 84.34(17) . . . no O36 Fe1 N15 80.98(16) . . . no N4 Fe1 N15 76.23(17) . . . no O3 Fe2 O38 95.52(16) . . . no O3 Fe2 O40 96.57(16) . . . no O3 Fe2 O42 93.23(16) . . . no O3 Fe2 O44 93.75(16) . . . no O3 Fe2 N18 105.16(18) . . . no O3 Fe2 N29 175.27(18) . . . no O38 Fe2 O40 59.81(14) . . . no O38 Fe2 O42 159.35(15) . . . no O38 Fe2 O44 139.47(15) . . . no O38 Fe2 N18 81.35(16) . . . no O38 Fe2 N29 89.15(17) . . . no O40 Fe2 O42 137.47(15) . . . no O40 Fe2 O44 79.97(15) . . . no O40 Fe2 N18 137.11(17) . . . no O40 Fe2 N29 85.14(16) . . . no O42 Fe2 O44 58.11(14) . . . no O42 Fe2 N18 78.32(16) . . . no O42 Fe2 N29 82.58(16) . . . no O44 Fe2 N18 133.41(16) . . . no O44 Fe2 N29 82.18(16) . . . no N18 Fe2 N29 76.22(18) . . . no Fe1 O3 Fe2 157.6(2) . . . no Fe1 O30 N31 94.8(3) . . . no Fe1 O32 N31 92.1(3) . . . no Fe1 O34 N35 94.2(3) . . . no Fe1 O36 N35 91.7(3) . . . no Fe2 O38 N39 92.0(3) . . . no Fe2 O40 N39 93.3(3) . . . no Fe2 O42 N43 92.9(3) . . . no Fe2 O44 N43 93.4(3) . . . no Fe1 N4 C5 123.5(4) . . . no Fe1 N4 C9 117.8(4) . . . no C5 N4 C9 118.7(5) . . . no Fe1 N15 C10 113.3(4) . . . no Fe1 N15 C14 127.9(4) . . . no C10 N15 C14 118.7(5) . . . no Fe2 N18 C19 126.6(4) . . . no Fe2 N18 C23 114.3(4) . . . no C19 N18 C23 118.8(5) . . . no Fe2 N29 C24 116.6(4) . . . no Fe2 N29 C28 124.1(4) . . . no C24 N29 C28 119.2(5) . . . no O30 N31 O32 114.5(5) . . . no O30 N31 O33 122.8(5) . . . no O32 N31 O33 122.7(5) . . . no O34 N35 O36 115.2(5) . . . no O34 N35 O37 122.6(5) . . . no O36 N35 O37 122.2(5) . . . no O38 N39 O40 114.9(4) . . . no O38 N39 O41 123.1(5) . . . no O40 N39 O41 122.0(5) . . . no O42 N43 O44 115.3(5) . . . no O42 N43 O45 122.0(5) . . . no O44 N43 O45 122.6(5) . . . no N4 C5 C6 122.8(5) . . . no N4 C5 H1 118.7(6) . . . no C6 C5 H1 118.6(6) . . . no C5 C6 C7 118.2(5) . . . no C5 C6 H2 120.9(6) . . . no C7 C6 H2 120.9(6) . . . no C6 C7 C8 119.8(5) . . . no C6 C7 H3 120.2(6) . . . no C8 C7 H3 120.0(6) . . . no C7 C8 C9 118.8(5) . . . no C7 C8 H4 120.5(5) . . . no C9 C8 H4 120.7(5) . . . no N4 C9 C8 121.7(5) . . . no N4 C9 C10 115.6(5) . . . no C8 C9 C10 122.7(5) . . . no N15 C10 C9 116.5(5) . . . no N15 C10 C11 121.9(5) . . . no C9 C10 C11 121.5(5) . . . no C10 C11 C12 119.1(5) . . . no C10 C11 H5 120.6(6) . . . no C12 C11 H5 120.4(6) . . . no C11 C12 C13 119.1(5) . . . no C11 C12 H6 120.5(6) . . . no C13 C12 H6 120.4(6) . . . no C12 C13 C14 119.7(5) . . . no C12 C13 H7 120.2(6) . . . no C14 C13 H7 120.2(5) . . . no N15 C14 C13 121.5(5) . . . no N15 C14 C16 120.0(5) . . . no C13 C14 C16 118.4(5) . . . no C14 C16 C17 111.8(5) . . . no C14 C16 H8 109.0(5) . . . no C14 C16 H9 108.8(5) . . . no C17 C16 H8 109.0(5) . . . no C17 C16 H9 108.8(5) . . . no H8 C16 H9 109.4(6) . . . no C16 C17 C19 112.8(5) . . . no C16 C17 H10 108.7(5) . . . no C16 C17 H11 108.6(5) . . . no C19 C17 H10 108.6(5) . . . no C19 C17 H11 108.7(5) . . . no H10 C17 H11 109.4(6) . . . no N18 C19 C17 119.5(5) . . . no N18 C19 C20 121.3(5) . . . no C17 C19 C20 119.2(5) . . . no C19 C20 C21 120.4(5) . . . no C19 C20 H12 119.9(6) . . . no C21 C20 H12 119.8(6) . . . no C20 C21 C22 118.2(5) . . . no C20 C21 H13 121.0(6) . . . no C22 C21 H13 120.8(6) . . . no C21 C22 C23 119.5(5) . . . no C21 C22 H14 120.3(6) . . . no C23 C22 H14 120.2(6) . . . no N18 C23 C22 121.8(5) . . . no N18 C23 C24 116.7(5) . . . no C22 C23 C24 121.5(5) . . . no N29 C24 C23 115.8(5) . . . no N29 C24 C25 120.5(5) . . . no C23 C24 C25 123.7(5) . . . no C24 C25 C26 119.9(6) . . . no C24 C25 H15 120.0(6) . . . no C26 C25 H15 120.1(6) . . . no C25 C26 C27 119.0(6) . . . no C25 C26 H16 120.3(6) . . . no C27 C26 H16 120.6(6) . . . no C26 C27 C28 119.1(6) . . . no C26 C27 H17 120.5(6) . . . no C28 C27 H17 120.4(6) . . . no N29 C28 C27 122.1(6) . . . no N29 C28 H18 118.8(6) . . . no C27 C28 H18 119.1(6) . . . no # The following lines may be used to test the character set of files sent by # network email or other means. They are not part of the CIF data archive. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./