[Fe2(m-OH)2(m-O2CAr4-FPh)(O2CAr4-FPh)3(OH2)(2-Ph2P(O)py)] (8) data_052704sad _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H68 Cl6 F8 Fe2 N O12 P' _chemical_formula_weight 1934.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9063(17) _cell_length_b 14.1811(18) _cell_length_c 24.990(3) _cell_angle_alpha 78.235(3) _cell_angle_beta 86.110(2) _cell_angle_gamma 86.837(3) _cell_volume 4463.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 823 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 18.60 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 0.602 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.752148 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39033 _diffrn_reflns_av_R_equivalents 0.0881 _diffrn_reflns_av_sigmaI/netI 0.1713 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.10 _reflns_number_total 19334 _reflns_number_gt 9193 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0814P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19334 _refine_ls_number_parameters 1151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1883 _refine_ls_R_factor_gt 0.0854 _refine_ls_wR_factor_ref 0.2037 _refine_ls_wR_factor_gt 0.1613 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.41005(6) 0.08334(5) 0.24404(3) 0.0235(2) Uani 1 1 d . . . Fe2 Fe 0.22181(6) 0.20166(5) 0.26793(3) 0.0237(2) Uani 1 1 d . . . N1 N 0.3582(3) -0.0651(3) 0.27409(17) 0.0272(10) Uani 1 1 d . . . O1 O 0.5370(3) 0.0242(3) 0.28359(14) 0.0287(9) Uani 1 1 d . . . O2 O 0.3277(3) 0.1128(3) 0.30762(17) 0.0289(10) Uani 1 1 d . . . O3 O 0.2750(3) 0.1273(3) 0.21225(17) 0.0275(10) Uani 1 1 d . . . O4 O 0.1099(3) 0.0979(3) 0.2950(2) 0.0331(10) Uani 1 1 d . . . O5 O 0.4678(3) 0.2150(2) 0.22481(13) 0.0239(8) Uani 1 1 d . . . O6 O 0.3262(3) 0.3046(2) 0.24310(13) 0.0239(8) Uani 1 1 d . . . O7 O 0.4725(3) 0.0515(2) 0.17644(14) 0.0275(9) Uani 1 1 d . . . O8 O 0.3789(3) 0.1373(3) 0.10917(14) 0.0340(9) Uani 1 1 d . . . O9 O 0.1785(3) 0.2540(3) 0.33376(13) 0.0278(9) Uani 1 1 d . . . O10 O 0.3180(3) 0.2234(3) 0.38443(14) 0.0336(9) Uani 1 1 d . . . O11 O 0.1162(3) 0.2820(2) 0.22357(13) 0.0266(8) Uani 1 1 d . . . O12 O -0.0323(3) 0.2048(3) 0.24548(16) 0.0373(10) Uani 1 1 d . . . P1 P 0.54961(11) -0.08228(11) 0.30554(6) 0.0282(3) Uani 1 1 d . . . F1 F 0.6971(3) 0.0977(3) 0.41010(17) 0.0802(14) Uani 1 1 d . . . F2 F 0.1151(3) 0.4367(3) 0.04020(15) 0.0654(12) Uani 1 1 d . . . F3 F 0.2246(3) -0.2954(3) 0.20899(18) 0.0734(13) Uani 1 1 d . . . F4 F 0.6300(3) 0.4924(3) 0.04437(15) 0.0578(10) Uani 1 1 d . . . F5 F -0.0031(4) -0.1197(3) 0.40723(19) 0.0902(15) Uani 1 1 d . . . F6 F 0.5182(3) 0.5883(3) 0.31522(19) 0.0779(13) Uani 1 1 d . . . F7 F 0.0835(3) -0.0165(3) 0.05862(15) 0.0589(11) Uani 1 1 d . . . F8 F 0.0410(3) 0.5801(3) 0.37006(15) 0.0682(12) Uani 1 1 d . . . H1 H 0.346(4) 0.132(4) 0.326(2) 0.02(2) Uiso 1 1 d . . . H2 H 0.292(4) 0.144(4) 0.186(2) 0.021(19) Uiso 1 1 d . . . H3 H 0.046(7) 0.138(6) 0.278(4) 0.12(3) Uiso 1 1 d . . . H4 H 0.111(6) 0.082(5) 0.323(3) 0.06(3) Uiso 1 1 d . . . C1 C 0.4215(4) -0.1297(4) 0.3050(2) 0.0284(13) Uani 1 1 d . . . C2 C 0.3885(5) -0.2161(4) 0.3344(2) 0.0373(15) Uani 1 1 d . . . H2A H 0.4354 -0.2597 0.3558 0.045 Uiso 1 1 calc R . . C3 C 0.2866(5) -0.2394(4) 0.3327(3) 0.0431(16) Uani 1 1 d . . . H3A H 0.2621 -0.2992 0.3527 0.052 Uiso 1 1 calc R . . C4 C 0.2214(5) -0.1738(4) 0.3014(3) 0.0408(15) Uani 1 1 d . . . H4A H 0.1506 -0.1876 0.2997 0.049 Uiso 1 1 calc R . . C5 C 0.2588(4) -0.0885(4) 0.2727(2) 0.0345(14) Uani 1 1 d . . . H5A H 0.2130 -0.0442 0.2510 0.041 Uiso 1 1 calc R . . C6 C 0.6395(4) -0.1396(4) 0.2636(2) 0.0305(13) Uani 1 1 d . . . C7 C 0.6706(5) -0.2369(4) 0.2789(3) 0.0416(16) Uani 1 1 d . . . H7A H 0.6447 -0.2739 0.3127 0.050 Uiso 1 1 calc R . . C8 C 0.7381(5) -0.2789(5) 0.2452(3) 0.0461(17) Uani 1 1 d . . . H8A H 0.7601 -0.3448 0.2560 0.055 Uiso 1 1 calc R . . C9 C 0.7740(5) -0.2261(5) 0.1961(3) 0.0503(18) Uani 1 1 d . . . H9A H 0.8217 -0.2552 0.1731 0.060 Uiso 1 1 calc R . . C10 C 0.7415(5) -0.1313(5) 0.1798(2) 0.0464(17) Uani 1 1 d . . . H10A H 0.7653 -0.0954 0.1452 0.056 Uiso 1 1 calc R . . C11 C 0.6747(4) -0.0888(4) 0.2136(2) 0.0357(14) Uani 1 1 d . . . H11A H 0.6525 -0.0231 0.2024 0.043 Uiso 1 1 calc R . . C12 C 0.5832(5) -0.1120(4) 0.3751(2) 0.0338(14) Uani 1 1 d . . . C13 C 0.5101(6) -0.0921(5) 0.4146(3) 0.0538(19) Uani 1 1 d . . . H13A H 0.4447 -0.0627 0.4040 0.065 Uiso 1 1 calc R . . C14 C 0.5306(6) -0.1144(6) 0.4695(3) 0.070(2) Uani 1 1 d . . . H14A H 0.4799 -0.1000 0.4963 0.085 Uiso 1 1 calc R . . C15 C 0.6241(6) -0.1569(6) 0.4847(3) 0.069(2) Uani 1 1 d . . . H15A H 0.6371 -0.1748 0.5225 0.083 Uiso 1 1 calc R . . C16 C 0.7002(6) -0.1743(5) 0.4459(3) 0.061(2) Uani 1 1 d . . . H16A H 0.7662 -0.2015 0.4570 0.073 Uiso 1 1 calc R . . C17 C 0.6802(5) -0.1521(5) 0.3908(3) 0.0441(16) Uani 1 1 d . . . H17A H 0.7323 -0.1641 0.3640 0.053 Uiso 1 1 calc R . . C18 C 0.4209(4) 0.2941(4) 0.2275(2) 0.0254(12) Uani 1 1 d . . . C19 C 0.4826(4) 0.3831(4) 0.2115(2) 0.0264(12) Uani 1 1 d . . . C20 C 0.5734(4) 0.3904(4) 0.2377(2) 0.0268(12) Uani 1 1 d . . . C21 C 0.6302(5) 0.4721(4) 0.2203(2) 0.0384(15) Uani 1 1 d . . . H21A H 0.6924 0.4779 0.2374 0.046 Uiso 1 1 calc R . . C22 C 0.5981(5) 0.5455(4) 0.1784(2) 0.0405(15) Uani 1 1 d . . . H22A H 0.6384 0.6008 0.1666 0.049 Uiso 1 1 calc R . . C23 C 0.5075(5) 0.5378(4) 0.1540(2) 0.0344(14) Uani 1 1 d . . . H23A H 0.4850 0.5888 0.1258 0.041 Uiso 1 1 calc R . . C24 C 0.4485(4) 0.4571(4) 0.1697(2) 0.0301(13) Uani 1 1 d . . . C25 C 0.6082(4) 0.3143(4) 0.2834(2) 0.0296(13) Uani 1 1 d . . . C26 C 0.5399(4) 0.2824(4) 0.3284(2) 0.0355(14) Uani 1 1 d . . . H26A H 0.4718 0.3112 0.3297 0.043 Uiso 1 1 calc R . . C27 C 0.5693(5) 0.2098(5) 0.3712(2) 0.0446(17) Uani 1 1 d . . . H27A H 0.5228 0.1881 0.4018 0.053 Uiso 1 1 calc R . . C28 C 0.6687(6) 0.1703(5) 0.3677(3) 0.0552(19) Uani 1 1 d . . . C29 C 0.7377(5) 0.1993(5) 0.3244(3) 0.0478(17) Uani 1 1 d . . . H29A H 0.8055 0.1700 0.3231 0.057 Uiso 1 1 calc R . . C30 C 0.7065(5) 0.2721(4) 0.2827(2) 0.0386(15) Uani 1 1 d . . . H30A H 0.7541 0.2938 0.2525 0.046 Uiso 1 1 calc R . . C31 C 0.3557(4) 0.4475(4) 0.1376(2) 0.0284(13) Uani 1 1 d . . . C32 C 0.3548(4) 0.3769(4) 0.1075(2) 0.0339(14) Uani 1 1 d . . . H32A H 0.4114 0.3308 0.1088 0.041 Uiso 1 1 calc R . . C33 C 0.2733(5) 0.3714(5) 0.0753(2) 0.0400(15) Uani 1 1 d . . . H33A H 0.2725 0.3217 0.0549 0.048 Uiso 1 1 calc R . . C34 C 0.1944(5) 0.4393(5) 0.0737(2) 0.0440(17) Uani 1 1 d . . . C35 C 0.1904(5) 0.5097(5) 0.1030(2) 0.0445(17) Uani 1 1 d . . . H35A H 0.1332 0.5551 0.1014 0.053 Uiso 1 1 calc R . . C36 C 0.2730(5) 0.5139(4) 0.1356(2) 0.0407(15) Uani 1 1 d . . . H36A H 0.2723 0.5627 0.1566 0.049 Uiso 1 1 calc R . . C37 C 0.4516(4) 0.0817(4) 0.1255(2) 0.0254(12) Uani 1 1 d . . . C38 C 0.5277(4) 0.0399(4) 0.0872(2) 0.0279(13) Uani 1 1 d . . . C39 C 0.6021(4) 0.0975(4) 0.0545(2) 0.0313(13) Uani 1 1 d . . . C40 C 0.6758(4) 0.0525(5) 0.0230(2) 0.0375(15) Uani 1 1 d . . . H40A H 0.7281 0.0900 0.0014 0.045 Uiso 1 1 calc R . . C41 C 0.6746(5) -0.0436(5) 0.0227(2) 0.0425(16) Uani 1 1 d . . . H41A H 0.7249 -0.0720 0.0006 0.051 Uiso 1 1 calc R . . C42 C 0.6001(5) -0.0993(4) 0.0546(2) 0.0372(15) Uani 1 1 d . . . H42A H 0.5991 -0.1661 0.0540 0.045 Uiso 1 1 calc R . . C43 C 0.5261(4) -0.0588(4) 0.0876(2) 0.0285(13) Uani 1 1 d . . . C44 C 0.6067(4) 0.2027(4) 0.0530(2) 0.0315(14) Uani 1 1 d . . . C45 C 0.6185(4) 0.2380(4) 0.0993(2) 0.0337(14) Uani 1 1 d . . . H45A H 0.6202 0.1946 0.1337 0.040 Uiso 1 1 calc R . . C46 C 0.6280(4) 0.3358(4) 0.0970(2) 0.0345(14) Uani 1 1 d . . . H46A H 0.6374 0.3597 0.1291 0.041 Uiso 1 1 calc R . . C47 C 0.6234(5) 0.3961(4) 0.0475(3) 0.0381(15) Uani 1 1 d . . . C48 C 0.6113(5) 0.3637(5) 0.0004(3) 0.0480(17) Uani 1 1 d . . . H48A H 0.6073 0.4078 -0.0337 0.058 Uiso 1 1 calc R . . C49 C 0.6051(5) 0.2669(5) 0.0031(2) 0.0426(16) Uani 1 1 d . . . H49A H 0.5997 0.2434 -0.0295 0.051 Uiso 1 1 calc R . . C50 C 0.4467(5) -0.1203(4) 0.1210(2) 0.0337(14) Uani 1 1 d . . . C51 C 0.3402(5) -0.0984(4) 0.1151(2) 0.0381(15) Uani 1 1 d . . . H51A H 0.3186 -0.0414 0.0906 0.046 Uiso 1 1 calc R . . C52 C 0.2666(5) -0.1580(5) 0.1442(3) 0.0435(16) Uani 1 1 d . . . H52A H 0.1947 -0.1438 0.1392 0.052 Uiso 1 1 calc R . . C53 C 0.2983(6) -0.2366(5) 0.1800(3) 0.0471(17) Uani 1 1 d . . . C54 C 0.4001(6) -0.2610(5) 0.1895(3) 0.0518(18) Uani 1 1 d . . . H54A H 0.4192 -0.3160 0.2162 0.062 Uiso 1 1 calc R . . C55 C 0.4750(5) -0.2026(4) 0.1588(2) 0.0402(15) Uani 1 1 d . . . H55A H 0.5465 -0.2191 0.1637 0.048 Uiso 1 1 calc R . . C56 C 0.2282(4) 0.2532(4) 0.3769(2) 0.0289(13) Uani 1 1 d . . . C57 C 0.1664(4) 0.2938(5) 0.4211(2) 0.0342(14) Uani 1 1 d . . . C58 C 0.0839(5) 0.2403(5) 0.4491(2) 0.0384(15) Uani 1 1 d . . . C59 C 0.0246(5) 0.2794(6) 0.4889(3) 0.0536(19) Uani 1 1 d . . . H59A H -0.0338 0.2463 0.5072 0.064 Uiso 1 1 calc R . . C60 C 0.0490(6) 0.3643(6) 0.5019(3) 0.063(2) Uani 1 1 d . . . H60A H 0.0098 0.3880 0.5303 0.076 Uiso 1 1 calc R . . C61 C 0.1308(6) 0.4157(5) 0.4737(2) 0.0506(18) Uani 1 1 d . . . H61A H 0.1465 0.4751 0.4826 0.061 Uiso 1 1 calc R . . C62 C 0.1904(5) 0.3815(5) 0.4324(2) 0.0383(15) Uani 1 1 d . . . C63 C 0.0606(5) 0.1448(5) 0.4385(2) 0.0411(16) Uani 1 1 d . . . C64 C 0.1384(5) 0.0737(5) 0.4386(2) 0.0474(17) Uani 1 1 d . . . H64A H 0.2071 0.0861 0.4460 0.057 Uiso 1 1 calc R . . C65 C 0.1171(6) -0.0158(5) 0.4281(3) 0.059(2) Uani 1 1 d . . . H65A H 0.1707 -0.0644 0.4281 0.070 Uiso 1 1 calc R . . C66 C 0.0183(7) -0.0324(6) 0.4179(3) 0.063(2) Uani 1 1 d . . . C67 C -0.0607(6) 0.0349(7) 0.4180(3) 0.067(2) Uani 1 1 d . . . H67A H -0.1291 0.0210 0.4110 0.080 Uiso 1 1 calc R . . C68 C -0.0404(5) 0.1243(6) 0.4284(3) 0.056(2) Uani 1 1 d . . . H68A H -0.0952 0.1718 0.4288 0.068 Uiso 1 1 calc R . . C69 C 0.2749(5) 0.4372(4) 0.4014(3) 0.0428(16) Uani 1 1 d . . . C70 C 0.2833(5) 0.4575(4) 0.3440(3) 0.0431(16) Uani 1 1 d . . . H70A H 0.2315 0.4358 0.3246 0.052 Uiso 1 1 calc R . . C71 C 0.3643(6) 0.5079(4) 0.3147(3) 0.0485(18) Uani 1 1 d . . . H71A H 0.3695 0.5208 0.2758 0.058 Uiso 1 1 calc R . . C72 C 0.4366(6) 0.5385(5) 0.3440(3) 0.057(2) Uani 1 1 d . . . C73 C 0.4328(6) 0.5223(5) 0.3992(3) 0.062(2) Uani 1 1 d . . . H73A H 0.4849 0.5454 0.4177 0.074 Uiso 1 1 calc R . . C74 C 0.3516(6) 0.4715(5) 0.4282(3) 0.0565(19) Uani 1 1 d . . . H74A H 0.3480 0.4598 0.4670 0.068 Uiso 1 1 calc R . . C75 C 0.0197(4) 0.2713(4) 0.2186(2) 0.0249(12) Uani 1 1 d . . . C76 C -0.0352(4) 0.3466(4) 0.1772(2) 0.0285(13) Uani 1 1 d . . . C77 C -0.0616(4) 0.3201(4) 0.1286(2) 0.0310(13) Uani 1 1 d . . . C78 C -0.1182(4) 0.3862(4) 0.0918(2) 0.0370(15) Uani 1 1 d . . . H78A H -0.1373 0.3690 0.0591 0.044 Uiso 1 1 calc R . . C79 C -0.1472(4) 0.4763(5) 0.1015(2) 0.0401(16) Uani 1 1 d . . . H79A H -0.1866 0.5204 0.0760 0.048 Uiso 1 1 calc R . . C80 C -0.1188(4) 0.5023(4) 0.1486(2) 0.0343(14) Uani 1 1 d . . . H80A H -0.1383 0.5649 0.1550 0.041 Uiso 1 1 calc R . . C81 C -0.0621(4) 0.4384(4) 0.1869(2) 0.0301(13) Uani 1 1 d . . . C82 C -0.0259(4) 0.2270(4) 0.1141(2) 0.0285(13) Uani 1 1 d . . . C83 C 0.0786(4) 0.1963(4) 0.1166(2) 0.0333(14) Uani 1 1 d . . . H83A H 0.1253 0.2324 0.1313 0.040 Uiso 1 1 calc R . . C84 C 0.1159(5) 0.1140(4) 0.0980(2) 0.0397(15) Uani 1 1 d . . . H84A H 0.1872 0.0936 0.0998 0.048 Uiso 1 1 calc R . . C85 C 0.0471(5) 0.0637(4) 0.0771(2) 0.0389(15) Uani 1 1 d . . . C86 C -0.0568(5) 0.0894(5) 0.0743(2) 0.0452(17) Uani 1 1 d . . . H86A H -0.1027 0.0518 0.0601 0.054 Uiso 1 1 calc R . . C87 C -0.0930(5) 0.1717(4) 0.0927(2) 0.0406(15) Uani 1 1 d . . . H87A H -0.1646 0.1909 0.0908 0.049 Uiso 1 1 calc R . . C88 C -0.0317(4) 0.4728(4) 0.2368(2) 0.0303(13) Uani 1 1 d . . . C89 C -0.0430(5) 0.4179(5) 0.2897(2) 0.0401(15) Uani 1 1 d . . . H89A H -0.0693 0.3553 0.2949 0.048 Uiso 1 1 calc R . . C90 C -0.0169(5) 0.4521(5) 0.3347(3) 0.0455(17) Uani 1 1 d . . . H90A H -0.0223 0.4131 0.3705 0.055 Uiso 1 1 calc R . . C91 C 0.0167(5) 0.5435(5) 0.3263(3) 0.0460(17) Uani 1 1 d . . . C92 C 0.0288(5) 0.6016(5) 0.2754(3) 0.0475(17) Uani 1 1 d . . . H92A H 0.0532 0.6650 0.2708 0.057 Uiso 1 1 calc R . . C93 C 0.0039(5) 0.5644(4) 0.2307(3) 0.0409(15) Uani 1 1 d . . . H93A H 0.0117 0.6032 0.1950 0.049 Uiso 1 1 calc R . . C94 C 0.9410(6) 0.9869(5) 0.2223(3) 0.065(2) Uani 1 1 d . . . H94A H 0.8823 1.0059 0.1982 0.078 Uiso 1 1 calc R . . H94B H 0.9867 1.0423 0.2169 0.078 Uiso 1 1 calc R . . Cl1 Cl 1.01028(16) 0.89003(16) 0.20322(10) 0.0806(6) Uani 1 1 d . . . Cl2 Cl 0.89258(19) 0.96178(19) 0.28999(9) 0.0949(8) Uani 1 1 d . . . C95 C 0.0454(6) 0.2925(5) 0.9657(3) 0.065(2) Uani 1 1 d . . . H95A H 0.0278 0.2631 1.0044 0.078 Uiso 1 1 calc R . . H95B H 0.0341 0.3632 0.9612 0.078 Uiso 1 1 calc R . . Cl3 Cl 0.1771(2) 0.26528(17) 0.94953(9) 0.1005(9) Uani 1 1 d . . . Cl4 Cl -0.0358(3) 0.25048(18) 0.92435(12) 0.1272(12) Uani 1 1 d . . . C96 C 0.7083(10) 0.4234(12) 0.3965(7) 0.188(8) Uani 1 1 d . . . H96A H 0.7591 0.4005 0.3699 0.225 Uiso 1 1 calc R . . H96B H 0.6378 0.4221 0.3833 0.225 Uiso 1 1 calc R . . Cl5 Cl 0.7338(3) 0.5384(3) 0.40081(16) 0.1742(16) Uani 1 1 d . . . Cl6 Cl 0.7164(5) 0.3444(4) 0.4634(3) 0.293(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0224(4) 0.0276(4) 0.0218(4) -0.0078(3) -0.0038(3) 0.0012(3) Fe2 0.0203(4) 0.0304(5) 0.0212(4) -0.0073(3) -0.0024(3) -0.0001(3) N1 0.027(3) 0.029(3) 0.026(3) -0.006(2) -0.002(2) -0.001(2) O1 0.023(2) 0.039(2) 0.025(2) -0.0085(17) -0.0059(16) 0.0006(17) O2 0.033(3) 0.034(3) 0.022(2) -0.011(2) -0.0071(19) 0.0047(19) O3 0.024(2) 0.037(3) 0.023(2) -0.009(2) -0.0019(19) -0.0017(18) O4 0.034(3) 0.031(2) 0.032(3) -0.002(2) -0.004(2) -0.0023(19) O5 0.021(2) 0.025(2) 0.027(2) -0.0060(16) -0.0019(15) -0.0016(16) O6 0.018(2) 0.027(2) 0.027(2) -0.0079(16) -0.0018(15) 0.0005(16) O7 0.027(2) 0.033(2) 0.023(2) -0.0073(17) -0.0048(16) 0.0031(17) O8 0.030(2) 0.043(2) 0.030(2) -0.0101(19) -0.0066(17) 0.0095(19) O9 0.026(2) 0.041(2) 0.018(2) -0.0114(17) -0.0002(16) 0.0035(17) O10 0.029(2) 0.048(3) 0.026(2) -0.0115(19) -0.0049(17) 0.0041(19) O11 0.022(2) 0.034(2) 0.024(2) -0.0064(17) -0.0041(16) -0.0011(17) O12 0.026(2) 0.042(3) 0.042(2) 0.000(2) -0.0068(19) -0.0059(19) P1 0.0273(8) 0.0343(9) 0.0233(8) -0.0064(7) -0.0055(6) 0.0023(7) F1 0.051(3) 0.098(3) 0.070(3) 0.032(3) -0.013(2) 0.008(2) F2 0.042(2) 0.101(3) 0.054(3) -0.008(2) -0.0233(19) -0.007(2) F3 0.081(3) 0.057(3) 0.085(3) -0.025(2) 0.027(2) -0.032(2) F4 0.065(3) 0.048(2) 0.061(3) -0.0098(19) -0.004(2) -0.015(2) F5 0.112(4) 0.060(3) 0.091(4) 0.019(3) -0.030(3) -0.032(3) F6 0.070(3) 0.061(3) 0.105(4) -0.024(3) 0.015(3) -0.022(2) F7 0.065(3) 0.056(2) 0.066(3) -0.035(2) -0.012(2) 0.009(2) F8 0.085(3) 0.078(3) 0.053(3) -0.038(2) -0.014(2) 0.002(2) C1 0.032(3) 0.029(3) 0.027(3) -0.011(3) -0.003(2) 0.001(3) C2 0.041(4) 0.029(3) 0.040(4) -0.002(3) -0.004(3) 0.000(3) C3 0.040(4) 0.038(4) 0.050(4) -0.005(3) 0.007(3) -0.014(3) C4 0.031(4) 0.038(4) 0.057(4) -0.016(3) 0.001(3) -0.013(3) C5 0.031(3) 0.033(3) 0.042(4) -0.013(3) -0.006(3) 0.004(3) C6 0.026(3) 0.036(3) 0.034(3) -0.015(3) -0.003(2) -0.005(3) C7 0.036(4) 0.039(4) 0.051(4) -0.011(3) -0.003(3) 0.001(3) C8 0.038(4) 0.036(4) 0.069(5) -0.023(4) -0.004(3) 0.004(3) C9 0.035(4) 0.064(5) 0.064(5) -0.041(4) -0.007(3) 0.004(4) C10 0.033(4) 0.080(5) 0.031(4) -0.023(4) -0.002(3) -0.002(4) C11 0.033(3) 0.045(4) 0.032(3) -0.011(3) -0.006(3) -0.002(3) C12 0.037(4) 0.038(4) 0.027(3) -0.006(3) -0.009(3) 0.000(3) C13 0.057(5) 0.074(5) 0.030(4) -0.013(3) -0.009(3) 0.016(4) C14 0.064(5) 0.119(7) 0.028(4) -0.015(4) -0.002(4) 0.004(5) C15 0.069(6) 0.109(7) 0.026(4) -0.003(4) -0.023(4) -0.004(5) C16 0.052(5) 0.083(6) 0.043(4) 0.002(4) -0.022(4) 0.000(4) C17 0.032(4) 0.060(4) 0.039(4) -0.004(3) -0.013(3) 0.001(3) C18 0.025(3) 0.037(3) 0.015(3) -0.006(2) -0.004(2) -0.003(3) C19 0.026(3) 0.027(3) 0.027(3) -0.006(2) -0.002(2) 0.001(2) C20 0.022(3) 0.036(3) 0.024(3) -0.010(3) 0.002(2) -0.004(3) C21 0.032(4) 0.049(4) 0.037(4) -0.015(3) 0.000(3) -0.002(3) C22 0.041(4) 0.038(4) 0.046(4) -0.014(3) 0.000(3) -0.015(3) C23 0.044(4) 0.027(3) 0.031(3) -0.002(3) -0.006(3) -0.003(3) C24 0.030(3) 0.029(3) 0.034(3) -0.012(3) -0.003(3) 0.003(3) C25 0.025(3) 0.038(3) 0.029(3) -0.012(3) -0.004(2) -0.006(3) C26 0.029(3) 0.048(4) 0.032(3) -0.012(3) -0.009(3) -0.004(3) C27 0.032(4) 0.065(5) 0.033(4) -0.001(3) -0.004(3) -0.010(3) C28 0.048(5) 0.066(5) 0.045(4) 0.009(4) -0.015(3) 0.005(4) C29 0.029(4) 0.063(5) 0.050(4) -0.006(4) -0.012(3) 0.009(3) C30 0.035(4) 0.048(4) 0.033(3) -0.010(3) -0.004(3) -0.001(3) C31 0.026(3) 0.027(3) 0.030(3) 0.002(3) -0.001(2) -0.002(2) C32 0.030(3) 0.032(3) 0.041(4) -0.008(3) -0.002(3) -0.006(3) C33 0.038(4) 0.048(4) 0.036(4) -0.010(3) -0.002(3) -0.015(3) C34 0.032(4) 0.067(5) 0.031(4) 0.000(3) -0.010(3) -0.009(3) C35 0.032(4) 0.056(4) 0.041(4) -0.002(3) -0.007(3) 0.011(3) C36 0.046(4) 0.038(4) 0.038(4) -0.008(3) -0.010(3) 0.006(3) C37 0.029(3) 0.028(3) 0.022(3) -0.009(2) 0.001(2) -0.008(3) C38 0.029(3) 0.038(3) 0.017(3) -0.008(2) -0.012(2) 0.010(3) C39 0.028(3) 0.041(4) 0.025(3) -0.003(3) -0.010(2) 0.001(3) C40 0.028(3) 0.055(4) 0.029(3) -0.010(3) 0.000(3) 0.002(3) C41 0.038(4) 0.056(4) 0.032(4) -0.014(3) 0.001(3) 0.022(3) C42 0.047(4) 0.037(4) 0.031(3) -0.014(3) -0.007(3) 0.010(3) C43 0.028(3) 0.036(3) 0.023(3) -0.009(3) -0.008(2) 0.006(3) C44 0.028(3) 0.042(4) 0.023(3) -0.004(3) 0.003(2) -0.004(3) C45 0.024(3) 0.047(4) 0.027(3) 0.001(3) -0.001(2) -0.002(3) C46 0.032(3) 0.042(4) 0.031(3) -0.010(3) -0.001(3) -0.004(3) C47 0.035(4) 0.034(4) 0.042(4) -0.001(3) 0.001(3) -0.008(3) C48 0.061(5) 0.049(4) 0.033(4) -0.001(3) -0.007(3) -0.011(3) C49 0.052(4) 0.050(4) 0.028(3) -0.007(3) -0.004(3) -0.018(3) C50 0.044(4) 0.033(3) 0.027(3) -0.012(3) -0.004(3) 0.002(3) C51 0.044(4) 0.040(4) 0.036(4) -0.020(3) -0.011(3) 0.004(3) C52 0.032(4) 0.057(4) 0.048(4) -0.029(4) 0.005(3) -0.008(3) C53 0.061(5) 0.034(4) 0.048(4) -0.015(3) 0.017(4) -0.014(4) C54 0.059(5) 0.036(4) 0.061(5) -0.013(3) 0.001(4) 0.001(4) C55 0.040(4) 0.037(4) 0.046(4) -0.015(3) -0.002(3) -0.001(3) C56 0.026(3) 0.037(3) 0.021(3) -0.003(3) -0.001(2) 0.005(3) C57 0.028(3) 0.054(4) 0.020(3) -0.011(3) -0.003(2) 0.011(3) C58 0.036(4) 0.048(4) 0.028(3) -0.004(3) -0.004(3) 0.014(3) C59 0.047(4) 0.079(6) 0.031(4) -0.009(4) 0.005(3) 0.012(4) C60 0.060(5) 0.096(6) 0.032(4) -0.022(4) 0.004(4) 0.030(5) C61 0.068(5) 0.052(4) 0.033(4) -0.016(3) -0.002(3) 0.018(4) C62 0.043(4) 0.050(4) 0.024(3) -0.015(3) -0.009(3) 0.010(3) C63 0.037(4) 0.060(4) 0.020(3) 0.004(3) 0.007(3) 0.001(3) C64 0.044(4) 0.055(5) 0.037(4) 0.005(3) -0.001(3) -0.001(4) C65 0.065(5) 0.048(5) 0.056(5) 0.004(4) -0.007(4) 0.000(4) C66 0.085(7) 0.054(5) 0.043(4) 0.016(4) -0.011(4) -0.031(5) C67 0.049(5) 0.089(7) 0.053(5) 0.013(5) -0.008(4) -0.014(5) C68 0.039(4) 0.080(6) 0.042(4) 0.003(4) 0.001(3) 0.009(4) C69 0.047(4) 0.043(4) 0.041(4) -0.020(3) 0.001(3) 0.010(3) C70 0.055(4) 0.033(4) 0.045(4) -0.017(3) -0.003(3) 0.004(3) C71 0.072(5) 0.027(4) 0.047(4) -0.013(3) 0.005(4) 0.004(3) C72 0.063(5) 0.037(4) 0.075(6) -0.021(4) 0.008(4) -0.005(4) C73 0.060(5) 0.061(5) 0.071(6) -0.025(4) -0.020(4) -0.003(4) C74 0.065(5) 0.061(5) 0.052(5) -0.030(4) -0.010(4) 0.003(4) C75 0.026(3) 0.030(3) 0.021(3) -0.013(2) -0.003(2) 0.000(3) C76 0.020(3) 0.038(3) 0.028(3) -0.007(3) -0.003(2) -0.004(3) C77 0.017(3) 0.042(4) 0.034(3) -0.006(3) -0.003(2) -0.002(3) C78 0.032(4) 0.041(4) 0.038(4) -0.006(3) -0.008(3) 0.006(3) C79 0.031(4) 0.054(4) 0.034(4) -0.003(3) -0.013(3) 0.005(3) C80 0.027(3) 0.034(3) 0.040(4) -0.005(3) -0.004(3) 0.006(3) C81 0.026(3) 0.033(3) 0.029(3) -0.003(3) 0.000(2) -0.001(3) C82 0.025(3) 0.035(3) 0.025(3) -0.004(3) -0.007(2) 0.000(3) C83 0.029(3) 0.044(4) 0.029(3) -0.012(3) -0.002(3) -0.002(3) C84 0.034(4) 0.054(4) 0.035(4) -0.018(3) -0.010(3) 0.007(3) C85 0.047(4) 0.040(4) 0.034(4) -0.019(3) -0.004(3) 0.007(3) C86 0.041(4) 0.061(5) 0.042(4) -0.027(3) -0.009(3) -0.004(3) C87 0.027(3) 0.052(4) 0.045(4) -0.013(3) -0.006(3) -0.005(3) C88 0.023(3) 0.035(3) 0.032(3) -0.007(3) 0.003(2) 0.006(3) C89 0.039(4) 0.043(4) 0.038(4) -0.009(3) -0.004(3) 0.003(3) C90 0.054(4) 0.046(4) 0.036(4) -0.010(3) -0.001(3) 0.007(3) C91 0.047(4) 0.057(5) 0.040(4) -0.027(4) -0.004(3) 0.012(3) C92 0.051(4) 0.044(4) 0.052(4) -0.022(4) 0.001(3) -0.005(3) C93 0.046(4) 0.039(4) 0.037(4) -0.008(3) 0.001(3) 0.002(3) C94 0.077(6) 0.066(5) 0.056(5) -0.016(4) -0.006(4) -0.019(4) Cl1 0.0521(13) 0.0859(16) 0.1031(18) -0.0181(13) -0.0029(11) -0.0021(11) Cl2 0.1037(19) 0.128(2) 0.0621(14) -0.0297(14) 0.0136(13) -0.0631(16) C95 0.079(6) 0.063(5) 0.057(5) -0.020(4) -0.014(4) 0.005(4) Cl3 0.124(2) 0.0963(18) 0.0699(15) -0.0099(13) 0.0035(14) 0.0581(16) Cl4 0.200(3) 0.0720(16) 0.123(2) -0.0211(15) -0.084(2) -0.0216(18) C96 0.126(11) 0.263(18) 0.246(18) -0.210(16) -0.038(11) -0.015(11) Cl5 0.128(3) 0.256(5) 0.158(3) -0.080(3) -0.023(2) -0.012(3) Cl6 0.386(9) 0.257(6) 0.292(7) -0.156(6) -0.171(7) 0.056(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O7 1.947(3) . ? Fe1 O2 1.955(4) . ? Fe1 O3 1.981(4) . ? Fe1 O5 2.003(3) . ? Fe1 O1 2.023(3) . ? Fe1 N1 2.210(4) . ? Fe1 Fe2 2.9725(11) . ? Fe2 O9 1.974(3) . ? Fe2 O11 1.976(3) . ? Fe2 O3 1.977(4) . ? Fe2 O2 1.981(4) . ? Fe2 O6 2.017(3) . ? Fe2 O4 2.099(4) . ? N1 C5 1.347(7) . ? N1 C1 1.349(6) . ? O1 P1 1.502(4) . ? O5 C18 1.257(6) . ? O6 C18 1.267(6) . ? O7 C37 1.299(6) . ? O8 C37 1.227(6) . ? O9 C56 1.289(6) . ? O10 C56 1.224(6) . ? O11 C75 1.280(6) . ? O12 C75 1.242(6) . ? P1 C12 1.780(6) . ? P1 C6 1.785(6) . ? P1 C1 1.821(6) . ? F1 C28 1.371(7) . ? F2 C34 1.371(6) . ? F3 C53 1.368(7) . ? F4 C47 1.358(6) . ? F5 C66 1.364(8) . ? F6 C72 1.377(8) . ? F7 C85 1.361(6) . ? F8 C91 1.364(7) . ? C1 C2 1.367(7) . ? C2 C3 1.379(8) . ? C3 C4 1.376(8) . ? C4 C5 1.369(8) . ? C6 C11 1.370(8) . ? C6 C7 1.398(8) . ? C7 C8 1.367(8) . ? C8 C9 1.367(9) . ? C9 C10 1.373(9) . ? C10 C11 1.370(8) . ? C12 C13 1.380(8) . ? C12 C17 1.394(8) . ? C13 C14 1.383(8) . ? C14 C15 1.361(10) . ? C15 C16 1.381(10) . ? C16 C17 1.387(8) . ? C18 C19 1.500(7) . ? C19 C24 1.397(7) . ? C19 C20 1.399(7) . ? C20 C21 1.383(8) . ? C20 C25 1.477(7) . ? C21 C22 1.385(8) . ? C22 C23 1.373(8) . ? C23 C24 1.384(7) . ? C24 C31 1.513(7) . ? C25 C30 1.373(7) . ? C25 C26 1.396(7) . ? C26 C27 1.382(8) . ? C27 C28 1.375(9) . ? C28 C29 1.365(9) . ? C29 C30 1.374(8) . ? C31 C32 1.371(7) . ? C31 C36 1.380(7) . ? C32 C33 1.382(8) . ? C33 C34 1.360(8) . ? C34 C35 1.350(9) . ? C35 C36 1.397(8) . ? C37 C38 1.508(7) . ? C38 C43 1.399(7) . ? C38 C39 1.402(8) . ? C39 C40 1.402(7) . ? C39 C44 1.490(8) . ? C40 C41 1.366(8) . ? C41 C42 1.381(8) . ? C42 C43 1.397(7) . ? C43 C50 1.481(8) . ? C44 C45 1.372(8) . ? C44 C49 1.387(7) . ? C45 C46 1.388(8) . ? C46 C47 1.355(8) . ? C47 C48 1.371(8) . ? C48 C49 1.367(8) . ? C50 C55 1.392(8) . ? C50 C51 1.403(8) . ? C51 C52 1.375(8) . ? C52 C53 1.342(9) . ? C53 C54 1.365(9) . ? C54 C55 1.392(9) . ? C56 C57 1.508(7) . ? C57 C62 1.387(8) . ? C57 C58 1.404(8) . ? C58 C59 1.398(8) . ? C58 C63 1.483(9) . ? C59 C60 1.367(10) . ? C60 C61 1.384(10) . ? C61 C62 1.394(8) . ? C62 C69 1.465(9) . ? C63 C64 1.383(8) . ? C63 C68 1.401(9) . ? C64 C65 1.392(9) . ? C65 C66 1.361(10) . ? C66 C67 1.358(10) . ? C67 C68 1.386(10) . ? C69 C74 1.393(9) . ? C69 C70 1.402(8) . ? C70 C71 1.381(9) . ? C71 C72 1.365(10) . ? C72 C73 1.348(10) . ? C73 C74 1.382(10) . ? C75 C76 1.509(7) . ? C76 C81 1.394(7) . ? C76 C77 1.410(7) . ? C77 C78 1.387(7) . ? C77 C82 1.482(8) . ? C78 C79 1.376(8) . ? C79 C80 1.380(8) . ? C80 C81 1.394(7) . ? C81 C88 1.510(8) . ? C82 C83 1.396(7) . ? C82 C87 1.399(8) . ? C83 C84 1.392(8) . ? C84 C85 1.363(8) . ? C85 C86 1.373(8) . ? C86 C87 1.387(8) . ? C88 C93 1.377(8) . ? C88 C89 1.394(8) . ? C89 C90 1.382(8) . ? C90 C91 1.360(9) . ? C91 C92 1.372(9) . ? C92 C93 1.392(8) . ? C94 Cl1 1.729(7) . ? C94 Cl2 1.737(7) . ? C95 Cl4 1.728(7) . ? C95 Cl3 1.760(8) . ? C96 Cl5 1.708(13) . ? C96 Cl6 1.821(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Fe1 O2 171.53(17) . . ? O7 Fe1 O3 93.82(16) . . ? O2 Fe1 O3 78.42(17) . . ? O7 Fe1 O5 91.13(15) . . ? O2 Fe1 O5 92.76(17) . . ? O3 Fe1 O5 93.69(16) . . ? O7 Fe1 O1 89.80(14) . . ? O2 Fe1 O1 97.49(16) . . ? O3 Fe1 O1 172.12(17) . . ? O5 Fe1 O1 93.24(14) . . ? O7 Fe1 N1 92.15(15) . . ? O2 Fe1 N1 84.84(17) . . ? O3 Fe1 N1 92.33(17) . . ? O5 Fe1 N1 172.94(15) . . ? O1 Fe1 N1 80.52(15) . . ? O7 Fe1 Fe2 132.48(10) . . ? O2 Fe1 Fe2 41.28(12) . . ? O3 Fe1 Fe2 41.27(12) . . ? O5 Fe1 Fe2 80.08(10) . . ? O1 Fe1 Fe2 136.92(10) . . ? N1 Fe1 Fe2 102.18(12) . . ? O9 Fe2 O11 92.99(14) . . ? O9 Fe2 O3 168.92(16) . . ? O11 Fe2 O3 97.05(16) . . ? O9 Fe2 O2 91.91(16) . . ? O11 Fe2 O2 174.67(17) . . ? O3 Fe2 O2 77.90(17) . . ? O9 Fe2 O6 91.57(14) . . ? O11 Fe2 O6 90.43(14) . . ? O3 Fe2 O6 93.04(16) . . ? O2 Fe2 O6 91.55(16) . . ? O9 Fe2 O4 86.74(17) . . ? O11 Fe2 O4 88.66(17) . . ? O3 Fe2 O4 88.80(17) . . ? O2 Fe2 O4 89.51(19) . . ? O6 Fe2 O4 178.03(16) . . ? O9 Fe2 Fe1 130.27(10) . . ? O11 Fe2 Fe1 135.23(10) . . ? O3 Fe2 Fe1 41.38(11) . . ? O2 Fe2 Fe1 40.62(12) . . ? O6 Fe2 Fe1 79.00(10) . . ? O4 Fe2 Fe1 102.86(12) . . ? C5 N1 C1 117.4(5) . . ? C5 N1 Fe1 122.4(4) . . ? C1 N1 Fe1 118.8(4) . . ? P1 O1 Fe1 121.9(2) . . ? Fe1 O2 Fe2 98.10(19) . . ? Fe2 O3 Fe1 97.35(18) . . ? C18 O5 Fe1 127.5(3) . . ? C18 O6 Fe2 128.0(3) . . ? C37 O7 Fe1 132.1(3) . . ? C56 O9 Fe2 129.6(3) . . ? C75 O11 Fe2 132.4(3) . . ? O1 P1 C12 113.7(2) . . ? O1 P1 C6 111.9(2) . . ? C12 P1 C6 110.6(3) . . ? O1 P1 C1 105.7(2) . . ? C12 P1 C1 105.5(3) . . ? C6 P1 C1 109.1(2) . . ? N1 C1 C2 122.7(5) . . ? N1 C1 P1 111.1(4) . . ? C2 C1 P1 126.1(4) . . ? C1 C2 C3 119.5(6) . . ? C4 C3 C2 118.2(6) . . ? C5 C4 C3 119.8(6) . . ? N1 C5 C4 122.4(5) . . ? C11 C6 C7 118.8(5) . . ? C11 C6 P1 119.3(4) . . ? C7 C6 P1 121.8(5) . . ? C8 C7 C6 120.2(6) . . ? C9 C8 C7 119.9(6) . . ? C8 C9 C10 120.6(6) . . ? C11 C10 C9 119.6(6) . . ? C10 C11 C6 120.9(6) . . ? C13 C12 C17 119.1(6) . . ? C13 C12 P1 118.0(5) . . ? C17 C12 P1 122.9(5) . . ? C12 C13 C14 121.0(6) . . ? C15 C14 C13 119.5(7) . . ? C14 C15 C16 120.8(6) . . ? C15 C16 C17 119.9(6) . . ? C16 C17 C12 119.5(6) . . ? O5 C18 O6 125.4(5) . . ? O5 C18 C19 117.1(5) . . ? O6 C18 C19 117.5(5) . . ? C24 C19 C20 121.2(5) . . ? C24 C19 C18 118.7(5) . . ? C20 C19 C18 120.1(5) . . ? C21 C20 C19 118.2(5) . . ? C21 C20 C25 120.0(5) . . ? C19 C20 C25 121.7(5) . . ? C22 C21 C20 121.2(6) . . ? C23 C22 C21 119.6(6) . . ? C22 C23 C24 121.3(5) . . ? C23 C24 C19 118.4(5) . . ? C23 C24 C31 119.2(5) . . ? C19 C24 C31 122.1(5) . . ? C30 C25 C26 118.3(5) . . ? C30 C25 C20 121.7(5) . . ? C26 C25 C20 120.0(5) . . ? C27 C26 C25 121.4(6) . . ? C28 C27 C26 117.3(6) . . ? C29 C28 F1 119.9(6) . . ? C29 C28 C27 123.1(6) . . ? F1 C28 C27 117.0(6) . . ? C28 C29 C30 118.3(6) . . ? C29 C30 C25 121.7(6) . . ? C32 C31 C36 118.9(5) . . ? C32 C31 C24 120.9(5) . . ? C36 C31 C24 120.0(5) . . ? C31 C32 C33 121.3(6) . . ? C34 C33 C32 117.9(6) . . ? C35 C34 C33 123.4(6) . . ? C35 C34 F2 118.3(6) . . ? C33 C34 F2 118.3(6) . . ? C34 C35 C36 118.0(6) . . ? C31 C36 C35 120.5(6) . . ? O8 C37 O7 125.5(5) . . ? O8 C37 C38 122.5(5) . . ? O7 C37 C38 112.0(4) . . ? C43 C38 C39 121.0(5) . . ? C43 C38 C37 118.2(5) . . ? C39 C38 C37 120.7(5) . . ? C38 C39 C40 117.8(5) . . ? C38 C39 C44 122.6(5) . . ? C40 C39 C44 119.5(5) . . ? C41 C40 C39 121.8(6) . . ? C40 C41 C42 119.9(5) . . ? C41 C42 C43 120.8(6) . . ? C42 C43 C38 118.7(5) . . ? C42 C43 C50 119.5(5) . . ? C38 C43 C50 121.7(5) . . ? C45 C44 C49 118.6(6) . . ? C45 C44 C39 121.9(5) . . ? C49 C44 C39 119.3(5) . . ? C44 C45 C46 121.3(5) . . ? C47 C46 C45 118.1(5) . . ? C46 C47 F4 119.1(6) . . ? C46 C47 C48 122.4(6) . . ? F4 C47 C48 118.5(6) . . ? C49 C48 C47 118.9(6) . . ? C48 C49 C44 120.7(6) . . ? C55 C50 C51 117.7(6) . . ? C55 C50 C43 121.2(5) . . ? C51 C50 C43 121.1(5) . . ? C52 C51 C50 121.1(6) . . ? C53 C52 C51 118.8(6) . . ? C52 C53 F3 118.5(7) . . ? C52 C53 C54 123.7(6) . . ? F3 C53 C54 117.9(6) . . ? C53 C54 C55 117.7(6) . . ? C50 C55 C54 121.0(6) . . ? O10 C56 O9 126.3(5) . . ? O10 C56 C57 119.2(5) . . ? O9 C56 C57 114.5(5) . . ? C62 C57 C58 122.0(5) . . ? C62 C57 C56 120.5(5) . . ? C58 C57 C56 117.5(6) . . ? C59 C58 C57 117.5(6) . . ? C59 C58 C63 120.4(6) . . ? C57 C58 C63 122.1(5) . . ? C60 C59 C58 121.3(7) . . ? C59 C60 C61 120.0(6) . . ? C60 C61 C62 121.0(7) . . ? C57 C62 C61 118.1(6) . . ? C57 C62 C69 120.8(5) . . ? C61 C62 C69 121.1(6) . . ? C64 C63 C68 118.6(7) . . ? C64 C63 C58 120.4(6) . . ? C68 C63 C58 121.0(6) . . ? C63 C64 C65 120.6(7) . . ? C66 C65 C64 119.0(7) . . ? C67 C66 C65 122.3(8) . . ? C67 C66 F5 118.4(8) . . ? C65 C66 F5 119.3(8) . . ? C66 C67 C68 119.3(7) . . ? C67 C68 C63 120.2(7) . . ? C74 C69 C70 117.1(6) . . ? C74 C69 C62 120.8(6) . . ? C70 C69 C62 122.1(6) . . ? C71 C70 C69 122.1(6) . . ? C72 C71 C70 117.2(7) . . ? C73 C72 C71 123.8(7) . . ? C73 C72 F6 118.6(7) . . ? C71 C72 F6 117.6(7) . . ? C72 C73 C74 118.7(7) . . ? C73 C74 C69 121.2(7) . . ? O12 C75 O11 125.3(5) . . ? O12 C75 C76 117.6(5) . . ? O11 C75 C76 117.1(5) . . ? C81 C76 C77 120.6(5) . . ? C81 C76 C75 121.7(5) . . ? C77 C76 C75 117.7(5) . . ? C78 C77 C76 118.5(5) . . ? C78 C77 C82 119.0(5) . . ? C76 C77 C82 122.4(5) . . ? C79 C78 C77 121.4(6) . . ? C78 C79 C80 119.7(6) . . ? C79 C80 C81 121.1(6) . . ? C80 C81 C76 118.8(5) . . ? C80 C81 C88 118.0(5) . . ? C76 C81 C88 123.2(5) . . ? C83 C82 C87 117.9(5) . . ? C83 C82 C77 120.5(5) . . ? C87 C82 C77 121.4(5) . . ? C84 C83 C82 121.5(5) . . ? C85 C84 C83 118.0(6) . . ? F7 C85 C84 118.1(6) . . ? F7 C85 C86 118.7(6) . . ? C84 C85 C86 123.2(6) . . ? C85 C86 C87 118.3(6) . . ? C86 C87 C82 121.1(6) . . ? C93 C88 C89 117.7(5) . . ? C93 C88 C81 119.2(5) . . ? C89 C88 C81 123.0(5) . . ? C90 C89 C88 121.8(6) . . ? C91 C90 C89 117.8(6) . . ? C90 C91 F8 119.3(6) . . ? C90 C91 C92 123.3(6) . . ? F8 C91 C92 117.4(6) . . ? C91 C92 C93 117.5(6) . . ? C88 C93 C92 121.8(6) . . ? Cl1 C94 Cl2 112.7(4) . . ? Cl4 C95 Cl3 111.8(4) . . ? Cl5 C96 Cl6 109.8(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H1 O10 0.63(5) 2.15(5) 2.708(6) 148(7) . O3 H2 O8 0.68(5) 2.17(5) 2.803(6) 155(6) . O4 H3 O12 1.04(10) 1.51(10) 2.537(6) 169(8) . _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.787 _refine_diff_density_min -0.736 _refine_diff_density_rms 0.090