Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Soumen Mukherjee' 'Thomas Weyhermuller' 'Phalguni Chaudhuri' 'Karl Wieghardt' _publ_contact_author_name 'Professor Karl Wieghardt' _publ_contact_author_address ; Max-Planck-Institut fur Bioinorganic Chemistry Stiftstrasse 34-36 Mulheim an der Ruhr D-45470 GERMANY ; _publ_contact_author_email WIEGHARDT@MPI-MUELHEIM.MPG.DE _publ_section_title ; The Molecular and Electronic Structure of [Fe1112(t-buLISQ)2(u-O)] - a Dinuclear Ferric Complex Containing Four, O,N-Coordinated o- lminobenzo-semiquinonate(1-) n Radical Anions ; data_1 _database_code_CSD 211465 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[C96 H132 Fe2 N4 O5], 2.75 CH2Cl2' _chemical_formula_sum 'C98.75 H137.50 Cl5.50 Fe2 N4 O5' _chemical_formula_weight 1767.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9826(6) _cell_length_b 15.9612(9) _cell_length_c 27.5321(15) _cell_angle_alpha 84.48(1) _cell_angle_beta 82.47(1) _cell_angle_gamma 77.64(1) _cell_volume 5086.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'opaque parallelepiped' _exptl_crystal_colour black _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1887 _exptl_absorpt_coefficient_mu 0.479 _exptl_absorpt_correction_type 'Gaussian, face-indexed' _exptl_absorpt_correction_T_min 0.9270 _exptl_absorpt_correction_T_max 0.9527 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '395 images at 1.0 deg. in \w, 150 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38197 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0829 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 27.50 _reflns_number_total 21829 _reflns_number_gt 15345 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO, Nonius Collect Software' _computing_cell_refinement 'DENZO, Nonius Collect Software' _computing_data_reduction 'DENZO, Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+8.7536P] 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 21829 _refine_ls_number_parameters 1065 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.1066 _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.1799 _refine_ls_wR_factor_gt 0.1562 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.29745(4) 0.25405(3) 0.250723(15) 0.01552(11) Uani 1 d . . . O1 O 0.24913(19) 0.15002(14) 0.28311(8) 0.0204(5) Uani 1 d . . . C1 C 0.2000(3) 0.1551(2) 0.32786(11) 0.0193(6) Uani 1 d . . . C2 C 0.1696(3) 0.0823(2) 0.35715(12) 0.0200(6) Uani 1 d . . . C3 C 0.1128(3) 0.0975(2) 0.40316(12) 0.0239(7) Uani 1 d . . . H3 H 0.0909 0.0502 0.4229 0.029 Uiso 1 calc R . . C4 C 0.0843(3) 0.1795(2) 0.42332(12) 0.0262(7) Uani 1 d . . . C5 C 0.1193(3) 0.2483(2) 0.39649(12) 0.0245(7) Uani 1 d . . . H5 H 0.1053 0.3025 0.4102 0.029 Uiso 1 calc R . . C6 C 0.1766(3) 0.2382(2) 0.34816(11) 0.0194(6) Uani 1 d . . . N7 N 0.2173(2) 0.29796(16) 0.31691(9) 0.0179(5) Uani 1 d . . . C8 C 0.2050(3) 0.3848(2) 0.32688(11) 0.0193(6) Uani 1 d . . . C9 C 0.1038(3) 0.4358(2) 0.34728(12) 0.0222(7) Uani 1 d . . . H9 H 0.0382 0.4113 0.3577 0.027 Uiso 1 calc R . . C10 C 0.0982(3) 0.5224(2) 0.35254(12) 0.0237(7) Uani 1 d . . . H10 H 0.0285 0.5560 0.3668 0.028 Uiso 1 calc R . . C11 C 0.1917(3) 0.5612(2) 0.33746(12) 0.0215(7) Uani 1 d . . . C12 C 0.2928(3) 0.5091(2) 0.31666(12) 0.0225(7) Uani 1 d . . . H12 H 0.3584 0.5335 0.3061 0.027 Uiso 1 calc R . . C13 C 0.2993(3) 0.4230(2) 0.31123(12) 0.0205(7) Uani 1 d . . . H13 H 0.3686 0.3893 0.2967 0.025 Uiso 1 calc R . . C14 C 0.2036(3) -0.0069(2) 0.33729(12) 0.0224(7) Uani 1 d . . . C15 C 0.1641(3) -0.0747(2) 0.37533(13) 0.0301(8) Uani 1 d . . . H15A H 0.1867 -0.1314 0.3620 0.045 Uiso 1 calc R . . H15B H 0.0803 -0.0602 0.3828 0.045 Uiso 1 calc R . . H15C H 0.2001 -0.0756 0.4054 0.045 Uiso 1 calc R . . C16 C 0.1478(3) -0.0087(2) 0.29006(13) 0.0300(8) Uani 1 d . . . H16A H 0.1707 -0.0664 0.2780 0.045 Uiso 1 calc R . . H16B H 0.1733 0.0331 0.2649 0.045 Uiso 1 calc R . . H16C H 0.0639 0.0060 0.2973 0.045 Uiso 1 calc R . . C17 C 0.3351(3) -0.0316(2) 0.32683(14) 0.0306(8) Uani 1 d . . . H17A H 0.3570 -0.0889 0.3142 0.046 Uiso 1 calc R . . H17B H 0.3696 -0.0322 0.3573 0.046 Uiso 1 calc R . . H17C H 0.3626 0.0104 0.3024 0.046 Uiso 1 calc R . . C18 C 0.0164(4) 0.1872(3) 0.47468(13) 0.0345(9) Uani 1 d . . . C19 C -0.0819(4) 0.1390(3) 0.47935(15) 0.0419(10) Uani 1 d . . . H19A H -0.1346 0.1642 0.4550 0.063 Uiso 1 calc R . . H19B H -0.1235 0.1434 0.5124 0.063 Uiso 1 calc R . . H19C H -0.0507 0.0783 0.4736 0.063 Uiso 1 calc R . . C20 C 0.0961(4) 0.1465(5) 0.51298(16) 0.079(2) Uani 1 d . . . H20A H 0.1601 0.1764 0.5107 0.119 Uiso 1 calc R . . H20B H 0.1261 0.0857 0.5071 0.119 Uiso 1 calc R . . H20C H 0.0534 0.1509 0.5458 0.119 Uiso 1 calc R . . C21 C -0.0421(5) 0.2817(3) 0.48332(19) 0.0653(16) Uani 1 d . . . H21A H -0.0924 0.3045 0.4577 0.098 Uiso 1 calc R . . H21B H 0.0168 0.3162 0.4822 0.098 Uiso 1 calc R . . H21C H -0.0879 0.2843 0.5156 0.098 Uiso 1 calc R . . C22 C 0.1873(3) 0.6561(2) 0.34292(13) 0.0261(7) Uani 1 d . . . C23 C 0.2286(5) 0.6987(3) 0.29395(17) 0.0574(14) Uani 1 d . . . H23A H 0.3059 0.6680 0.2823 0.086 Uiso 1 calc R . . H23B H 0.2304 0.7586 0.2981 0.086 Uiso 1 calc R . . H23C H 0.1759 0.6969 0.2698 0.086 Uiso 1 calc R . . C24 C 0.2663(4) 0.6625(3) 0.38142(17) 0.0428(10) Uani 1 d . . . H24A H 0.2395 0.6350 0.4129 0.064 Uiso 1 calc R . . H24B H 0.2647 0.7231 0.3854 0.064 Uiso 1 calc R . . H24C H 0.3451 0.6334 0.3706 0.064 Uiso 1 calc R . . C25 C 0.0667(4) 0.7040(3) 0.3608(2) 0.0635(16) Uani 1 d . . . H25A H 0.0399 0.6768 0.3923 0.095 Uiso 1 calc R . . H25B H 0.0143 0.7021 0.3366 0.095 Uiso 1 calc R . . H25C H 0.0685 0.7640 0.3649 0.095 Uiso 1 calc R . . O31 O 0.22412(19) 0.36179(14) 0.21658(8) 0.0201(5) Uani 1 d . . . C31 C 0.2020(3) 0.3575(2) 0.17199(11) 0.0192(6) Uani 1 d . . . C32 C 0.1496(3) 0.4308(2) 0.14276(11) 0.0187(6) Uani 1 d . . . C33 C 0.1289(3) 0.4156(2) 0.09646(12) 0.0219(7) Uani 1 d . . . H33 H 0.0911 0.4629 0.0769 0.026 Uiso 1 calc R . . C34 C 0.1604(3) 0.3342(2) 0.07609(12) 0.0249(7) Uani 1 d . . . C35 C 0.2138(3) 0.2648(2) 0.10326(12) 0.0255(7) Uani 1 d . . . H35 H 0.2378 0.2106 0.0895 0.031 Uiso 1 calc R . . C36 C 0.2336(3) 0.2736(2) 0.15236(12) 0.0204(7) Uani 1 d . . . N37 N 0.2827(2) 0.21225(17) 0.18415(9) 0.0183(5) Uani 1 d . . . C38 C 0.3157(3) 0.1242(2) 0.17463(11) 0.0193(6) Uani 1 d . . . C39 C 0.2441(3) 0.0794(2) 0.15667(12) 0.0239(7) Uani 1 d . . . H39 H 0.1715 0.1088 0.1474 0.029 Uiso 1 calc R . . C40 C 0.2794(3) -0.0088(2) 0.15232(13) 0.0251(7) Uani 1 d . . . H40 H 0.2298 -0.0388 0.1401 0.030 Uiso 1 calc R . . C41 C 0.3851(3) -0.0544(2) 0.16534(12) 0.0229(7) Uani 1 d . . . C42 C 0.4553(3) -0.0076(2) 0.18323(13) 0.0256(7) Uani 1 d . . . H42 H 0.5285 -0.0367 0.1921 0.031 Uiso 1 calc R . . C43 C 0.4214(3) 0.0793(2) 0.18837(12) 0.0224(7) Uani 1 d . . . H43 H 0.4704 0.1090 0.2014 0.027 Uiso 1 calc R . . C44 C 0.1219(3) 0.5202(2) 0.16238(12) 0.0229(7) Uani 1 d . . . C45 C 0.0647(3) 0.5881(2) 0.12502(13) 0.0266(7) Uani 1 d . . . H45A H 0.0478 0.6447 0.1385 0.040 Uiso 1 calc R . . H45B H -0.0070 0.5737 0.1182 0.040 Uiso 1 calc R . . H45C H 0.1168 0.5894 0.0945 0.040 Uiso 1 calc R . . C46 C 0.2339(3) 0.5444(2) 0.17170(13) 0.0282(8) Uani 1 d . . . H46A H 0.2167 0.6018 0.1842 0.042 Uiso 1 calc R . . H46B H 0.2852 0.5446 0.1409 0.042 Uiso 1 calc R . . H46C H 0.2714 0.5024 0.1959 0.042 Uiso 1 calc R . . C47 C 0.0394(3) 0.5224(2) 0.21055(12) 0.0286(8) Uani 1 d . . . H47A H 0.0227 0.5802 0.2223 0.043 Uiso 1 calc R . . H47B H 0.0754 0.4810 0.2354 0.043 Uiso 1 calc R . . H47C H -0.0324 0.5073 0.2044 0.043 Uiso 1 calc R . . C48 C 0.1304(4) 0.3277(2) 0.02428(13) 0.0324(8) Uani 1 d . . . C49 C 0.1747(4) 0.3951(4) -0.01184(14) 0.0504(12) Uani 1 d . . . H49A H 0.1422 0.4525 -0.0004 0.076 Uiso 1 calc R . . H49B H 0.1515 0.3916 -0.0443 0.076 Uiso 1 calc R . . H49C H 0.2587 0.3845 -0.0140 0.076 Uiso 1 calc R . . C50 C -0.0006(4) 0.3469(4) 0.02591(16) 0.0614(16) Uani 1 d . . . H50A H -0.0322 0.4034 0.0387 0.092 Uiso 1 calc R . . H50B H -0.0317 0.3028 0.0474 0.092 Uiso 1 calc R . . H50C H -0.0217 0.3468 -0.0073 0.092 Uiso 1 calc R . . C51 C 0.1836(7) 0.2405(4) 0.0046(2) 0.103(3) Uani 1 d . . . H51A H 0.1572 0.1953 0.0269 0.155 Uiso 1 calc R . . H51B H 0.2676 0.2315 0.0023 0.155 Uiso 1 calc R . . H51C H 0.1604 0.2387 -0.0280 0.155 Uiso 1 calc R . . C52 C 0.4260(3) -0.1511(2) 0.16063(13) 0.0292(8) Uani 1 d . . . C53 C 0.5238(4) -0.1646(3) 0.11808(14) 0.0434(11) Uani 1 d . . . H53A H 0.5514 -0.2263 0.1144 0.065 Uiso 1 calc R . . H53B H 0.5871 -0.1394 0.1252 0.065 Uiso 1 calc R . . H53C H 0.4950 -0.1366 0.0876 0.065 Uiso 1 calc R . . C54 C 0.3288(4) -0.1937(3) 0.1511(2) 0.0526(13) Uani 1 d . . . H54A H 0.3584 -0.2555 0.1484 0.079 Uiso 1 calc R . . H54B H 0.2986 -0.1680 0.1205 0.079 Uiso 1 calc R . . H54C H 0.2671 -0.1850 0.1784 0.079 Uiso 1 calc R . . C55 C 0.4709(3) -0.1948(2) 0.20861(13) 0.0306(8) Uani 1 d . . . H55A H 0.4968 -0.2567 0.2053 0.046 Uiso 1 calc R . . H55B H 0.4090 -0.1849 0.2358 0.046 Uiso 1 calc R . . H55C H 0.5354 -0.1705 0.2153 0.046 Uiso 1 calc R . . Fe2 Fe 0.59374(4) 0.25059(3) 0.253102(16) 0.01611(11) Uani 1 d . . . O101 O 0.6741(2) 0.14850(14) 0.28933(8) 0.0212(5) Uani 1 d . . . C101 C 0.7219(3) 0.0828(2) 0.26417(12) 0.0194(6) Uani 1 d . . . C102 C 0.7687(3) 0.0007(2) 0.28661(12) 0.0217(7) Uani 1 d . . . C103 C 0.8201(3) -0.0623(2) 0.25558(13) 0.0250(7) Uani 1 d . . . H103 H 0.8540 -0.1169 0.2699 0.030 Uiso 1 calc R . . C104 C 0.8262(3) -0.0518(2) 0.20334(13) 0.0258(7) Uani 1 d . . . C105 C 0.7779(3) 0.0259(2) 0.18169(13) 0.0244(7) Uani 1 d . . . H105 H 0.7784 0.0332 0.1470 0.029 Uiso 1 calc R . . C106 C 0.7267(3) 0.0958(2) 0.21114(12) 0.0208(7) Uani 1 d . . . N107 N 0.6736(2) 0.17572(17) 0.19628(9) 0.0188(5) Uani 1 d . . . C108 C 0.6714(3) 0.2064(2) 0.14645(12) 0.0201(7) Uani 1 d . . . C109 C 0.7662(3) 0.1922(2) 0.11094(12) 0.0248(7) Uani 1 d . . . H109 H 0.8372 0.1581 0.1194 0.030 Uiso 1 calc R . . C110 C 0.7571(3) 0.2279(2) 0.06309(12) 0.0273(8) Uani 1 d . . . H110 H 0.8221 0.2166 0.0391 0.033 Uiso 1 calc R . . C111 C 0.6557(3) 0.2795(2) 0.04938(12) 0.0253(7) Uani 1 d . . . C112 C 0.5626(3) 0.2949(2) 0.08571(12) 0.0263(7) Uani 1 d . . . H112 H 0.4925 0.3308 0.0775 0.032 Uiso 1 calc R . . C113 C 0.5694(3) 0.2592(2) 0.13345(12) 0.0236(7) Uani 1 d . . . H113 H 0.5044 0.2707 0.1574 0.028 Uiso 1 calc R . . C114 C 0.7542(3) -0.0151(2) 0.34291(12) 0.0236(7) Uani 1 d . . . C115 C 0.8064(3) 0.0477(2) 0.36755(13) 0.0290(8) Uani 1 d . . . H11A H 0.7706 0.1069 0.3576 0.043 Uiso 1 calc R . . H11B H 0.8894 0.0381 0.3574 0.043 Uiso 1 calc R . . H11C H 0.7925 0.0379 0.4033 0.043 Uiso 1 calc R . . C116 C 0.6250(3) -0.0031(2) 0.36047(13) 0.0298(8) Uani 1 d . . . H11D H 0.5862 0.0553 0.3504 0.045 Uiso 1 calc R . . H11E H 0.6139 -0.0121 0.3963 0.045 Uiso 1 calc R . . H11F H 0.5926 -0.0449 0.3459 0.045 Uiso 1 calc R . . C117 C 0.8119(3) -0.1071(2) 0.35921(14) 0.0322(8) Uani 1 d . . . H11G H 0.8945 -0.1163 0.3484 0.048 Uiso 1 calc R . . H11H H 0.7783 -0.1482 0.3446 0.048 Uiso 1 calc R . . H11I H 0.7995 -0.1155 0.3951 0.048 Uiso 1 calc R . . C118 C 0.8873(3) -0.1294(2) 0.17415(15) 0.0334(9) Uani 1 d . . . C119 C 0.8824(5) -0.1093(3) 0.11841(17) 0.0625(15) Uani 1 d . . . H11J H 0.8019 -0.0935 0.1117 0.094 Uiso 1 calc R . . H11K H 0.9212 -0.1602 0.1010 0.094 Uiso 1 calc R . . H11L H 0.9209 -0.0614 0.1071 0.094 Uiso 1 calc R . . C120 C 1.0118(3) -0.1538(3) 0.1844(2) 0.0502(12) Uani 1 d . . . H12A H 1.0493 -0.1050 0.1744 0.075 Uiso 1 calc R . . H12B H 1.0515 -0.2031 0.1658 0.075 Uiso 1 calc R . . H12C H 1.0152 -0.1692 0.2196 0.075 Uiso 1 calc R . . C121 C 0.8282(4) -0.2057(3) 0.18962(18) 0.0451(11) Uani 1 d . . . H12D H 0.7477 -0.1897 0.1829 0.068 Uiso 1 calc R . . H12E H 0.8313 -0.2211 0.2248 0.068 Uiso 1 calc R . . H12F H 0.8677 -0.2550 0.1710 0.068 Uiso 1 calc R . . C122 C 0.6474(3) 0.3226(2) -0.00303(12) 0.0299(8) Uani 1 d . . . C123 C 0.5310(4) 0.3201(4) -0.01991(15) 0.0519(13) Uani 1 d . . . H12G H 0.5238 0.2601 -0.0203 0.078 Uiso 1 calc R . . H12H H 0.5263 0.3483 -0.0530 0.078 Uiso 1 calc R . . H12I H 0.4687 0.3501 0.0028 0.078 Uiso 1 calc R . . C124 C 0.7430(4) 0.2774(3) -0.03991(14) 0.0443(11) Uani 1 d . . . H12J H 0.7363 0.2175 -0.0407 0.066 Uiso 1 calc R . . H12K H 0.8180 0.2792 -0.0300 0.066 Uiso 1 calc R . . H12L H 0.7358 0.3067 -0.0726 0.066 Uiso 1 calc R . . C125 C 0.6593(4) 0.4162(3) -0.00240(15) 0.0450(11) Uani 1 d . . . H12M H 0.5985 0.4459 0.0211 0.068 Uiso 1 calc R . . H12N H 0.6523 0.4450 -0.0353 0.068 Uiso 1 calc R . . H12O H 0.7346 0.4176 0.0074 0.068 Uiso 1 calc R . . O131 O 0.6341(2) 0.35407(14) 0.21733(8) 0.0203(5) Uani 1 d . . . C131 C 0.6412(3) 0.4160(2) 0.24298(11) 0.0183(6) Uani 1 d . . . C132 C 0.6661(3) 0.4959(2) 0.22135(12) 0.0195(6) Uani 1 d . . . C133 C 0.6749(3) 0.5555(2) 0.25282(12) 0.0211(7) Uani 1 d . . . H133 H 0.6947 0.6079 0.2389 0.025 Uiso 1 calc R . . C134 C 0.6559(3) 0.5434(2) 0.30528(12) 0.0204(7) Uani 1 d . . . C135 C 0.6273(3) 0.4685(2) 0.32611(12) 0.0208(7) Uani 1 d . . . H135 H 0.6105 0.4608 0.3607 0.025 Uiso 1 calc R . . C136 C 0.6228(3) 0.4021(2) 0.29611(11) 0.0178(6) Uani 1 d . . . N137 N 0.6000(2) 0.32392(17) 0.31032(9) 0.0190(5) Uani 1 d . . . C138 C 0.5850(3) 0.2932(2) 0.36019(11) 0.0181(6) Uani 1 d . . . C139 C 0.4996(3) 0.2451(2) 0.37445(12) 0.0208(7) Uani 1 d . . . H139 H 0.4522 0.2362 0.3511 0.025 Uiso 1 calc R . . C140 C 0.4837(3) 0.2104(2) 0.42242(12) 0.0227(7) Uani 1 d . . . H140 H 0.4250 0.1783 0.4314 0.027 Uiso 1 calc R . . C141 C 0.5520(3) 0.2216(2) 0.45789(11) 0.0192(6) Uani 1 d . . . C142 C 0.6378(3) 0.2677(2) 0.44280(12) 0.0232(7) Uani 1 d . . . H142 H 0.6860 0.2759 0.4660 0.028 Uiso 1 calc R . . C143 C 0.6555(3) 0.3023(2) 0.39488(12) 0.0217(7) Uani 1 d . . . H143 H 0.7162 0.3325 0.3857 0.026 Uiso 1 calc R . . C144 C 0.6782(3) 0.5132(2) 0.16532(12) 0.0224(7) Uani 1 d . . . C145 C 0.5636(3) 0.5122(2) 0.14642(13) 0.0319(8) Uani 1 d . . . H14A H 0.5709 0.5232 0.1106 0.048 Uiso 1 calc R . . H14B H 0.5031 0.5570 0.1614 0.048 Uiso 1 calc R . . H14C H 0.5435 0.4559 0.1552 0.048 Uiso 1 calc R . . C146 C 0.7748(3) 0.4447(2) 0.14039(13) 0.0279(8) Uani 1 d . . . H14D H 0.8479 0.4455 0.1525 0.042 Uiso 1 calc R . . H14E H 0.7814 0.4577 0.1047 0.042 Uiso 1 calc R . . H14F H 0.7563 0.3877 0.1482 0.042 Uiso 1 calc R . . C147 C 0.7084(3) 0.6017(2) 0.15020(13) 0.0293(8) Uani 1 d . . . H14G H 0.7816 0.6036 0.1619 0.044 Uiso 1 calc R . . H14H H 0.6476 0.6466 0.1647 0.044 Uiso 1 calc R . . H14I H 0.7153 0.6113 0.1143 0.044 Uiso 1 calc R . . C148 C 0.6727(3) 0.6143(2) 0.33598(13) 0.0253(7) Uani 1 d . . . C149 C 0.5950(3) 0.7004(2) 0.32234(14) 0.0326(8) Uani 1 d . . . H14J H 0.6103 0.7153 0.2871 0.049 Uiso 1 calc R . . H14K H 0.6105 0.7452 0.3409 0.049 Uiso 1 calc R . . H14L H 0.5143 0.6958 0.3303 0.049 Uiso 1 calc R . . C150 C 0.7992(3) 0.6236(3) 0.32511(17) 0.0422(10) Uani 1 d . . . H15D H 0.8498 0.5688 0.3337 0.063 Uiso 1 calc R . . H15E H 0.8121 0.6682 0.3446 0.063 Uiso 1 calc R . . H15F H 0.8161 0.6398 0.2901 0.063 Uiso 1 calc R . . C151 C 0.6473(4) 0.5921(2) 0.39133(14) 0.0377(10) Uani 1 d . . . H15G H 0.6966 0.5371 0.4006 0.057 Uiso 1 calc R . . H15H H 0.5664 0.5878 0.3990 0.057 Uiso 1 calc R . . H15I H 0.6626 0.6374 0.4097 0.057 Uiso 1 calc R . . C152 C 0.5359(3) 0.1799(2) 0.51032(12) 0.0227(7) Uani 1 d . . . C153 C 0.5862(3) 0.2243(2) 0.54684(12) 0.0294(8) Uani 1 d . . . H15J H 0.6681 0.2220 0.5363 0.044 Uiso 1 calc R . . H15K H 0.5770 0.1949 0.5796 0.044 Uiso 1 calc R . . H15L H 0.5457 0.2845 0.5479 0.044 Uiso 1 calc R . . C154 C 0.4082(3) 0.1846(3) 0.52780(13) 0.0361(9) Uani 1 d . . . H15M H 0.3743 0.1566 0.5049 0.054 Uiso 1 calc R . . H15N H 0.3686 0.2449 0.5291 0.054 Uiso 1 calc R . . H15O H 0.3999 0.1552 0.5606 0.054 Uiso 1 calc R . . C155 C 0.5980(4) 0.0850(2) 0.51003(13) 0.0322(8) Uani 1 d . . . H15P H 0.6798 0.0815 0.4989 0.048 Uiso 1 calc R . . H15Q H 0.5644 0.0556 0.4877 0.048 Uiso 1 calc R . . H15R H 0.5892 0.0573 0.5433 0.048 Uiso 1 calc R . . O40 O 0.44623(19) 0.24814(15) 0.25340(8) 0.0219(5) Uani 1 d . . . C60 C 0.5796(5) 0.0638(4) 0.0590(2) 0.050(3) Uani 0.50 d PD . . H60A H 0.5739 0.0233 0.0884 0.060 Uiso 0.50 calc PR . . H60B H 0.5935 0.1176 0.0700 0.060 Uiso 0.50 calc PR . . Cl61 Cl 0.6961(3) 0.0202(3) 0.01921(17) 0.1086(13) Uani 0.50 d PD . . Cl62 Cl 0.4537(3) 0.0856(3) 0.03551(14) 0.0925(11) Uani 0.50 d PD . . C70 C 0.2996(4) 0.4268(3) 0.44847(18) 0.0697(17) Uani 1 d D . . H70A H 0.3297 0.3643 0.4462 0.084 Uiso 1 calc R . . H70B H 0.2828 0.4521 0.4153 0.084 Uiso 1 calc R . . Cl71 Cl 0.40308(15) 0.47247(14) 0.46746(7) 0.0970(6) Uani 1 d D . . Cl72 Cl 0.1737(2) 0.44264(19) 0.48832(7) 0.1267(9) Uani 1 d D . . C80 C 0.9356(6) 0.2254(4) 0.2674(2) 0.112(5) Uani 0.80 d PD A 1 H80A H 0.8663 0.2025 0.2806 0.134 Uiso 0.80 calc PR A 1 H80B H 1.0033 0.1869 0.2801 0.134 Uiso 0.80 calc PR A 1 Cl81 Cl 0.92205(14) 0.32993(12) 0.28594(7) 0.0663(5) Uani 0.80 d PD A 1 Cl82 Cl 0.95219(17) 0.22946(18) 0.20163(10) 0.0913(7) Uani 0.80 d PD A 1 C85 C 0.950(4) 0.2809(9) 0.2444(5) 0.118(14) Uiso 0.20 d PD B 2 H85A H 1.0208 0.3042 0.2380 0.142 Uiso 0.20 calc PR B 2 H85B H 0.8881 0.3212 0.2284 0.142 Uiso 0.20 calc PR B 2 Cl86 Cl 0.9097(8) 0.2685(6) 0.3070(3) 0.078(2) Uiso 0.20 d PD B 2 Cl87 Cl 0.9725(7) 0.1803(5) 0.2216(3) 0.067(2) Uiso 0.20 d PD B 2 Cl91 Cl 1.0487(8) 0.0539(6) 0.0632(3) 0.120(3) Uiso 0.25 d PD . 2 Cl92 Cl 1.0036(11) -0.0522(8) -0.0074(4) 0.159(4) Uiso 0.25 d PD . 2 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 0.0189(2) 0.0138(2) 0.0143(2) 0.00132(16) -0.00434(17) -0.00382(17) O1 0.0272(12) 0.0162(11) 0.0178(11) -0.0004(9) 0.0003(9) -0.0064(9) C1 0.0208(16) 0.0183(16) 0.0194(15) 0.0008(12) -0.0034(13) -0.0057(12) C2 0.0202(16) 0.0189(16) 0.0212(15) 0.0028(12) -0.0045(13) -0.0054(12) C3 0.0275(18) 0.0221(17) 0.0233(16) 0.0041(13) -0.0029(14) -0.0101(14) C4 0.0308(19) 0.0284(19) 0.0191(16) -0.0008(14) 0.0006(14) -0.0082(15) C5 0.0325(19) 0.0230(17) 0.0178(15) -0.0025(13) -0.0011(14) -0.0061(14) C6 0.0187(16) 0.0192(16) 0.0199(15) 0.0021(12) -0.0050(13) -0.0029(12) N7 0.0202(13) 0.0139(13) 0.0197(13) -0.0004(10) -0.0027(11) -0.0037(10) C8 0.0246(16) 0.0190(16) 0.0150(14) 0.0010(12) -0.0040(13) -0.0058(13) C9 0.0196(16) 0.0210(17) 0.0265(17) 0.0005(13) -0.0048(14) -0.0046(13) C10 0.0224(17) 0.0211(17) 0.0271(17) -0.0028(13) -0.0053(14) -0.0009(13) C11 0.0227(16) 0.0181(16) 0.0249(16) -0.0005(13) -0.0110(14) -0.0025(13) C12 0.0243(17) 0.0198(17) 0.0243(16) -0.0006(13) -0.0030(14) -0.0068(13) C13 0.0219(16) 0.0151(15) 0.0240(16) -0.0016(12) -0.0045(13) -0.0014(12) C14 0.0272(18) 0.0158(16) 0.0247(16) 0.0017(13) -0.0011(14) -0.0082(13) C15 0.041(2) 0.0182(17) 0.0314(19) 0.0039(14) -0.0026(16) -0.0106(15) C16 0.042(2) 0.0230(18) 0.0276(18) -0.0025(14) -0.0025(16) -0.0139(16) C17 0.033(2) 0.0197(18) 0.0348(19) 0.0001(15) 0.0017(16) -0.0005(15) C18 0.044(2) 0.039(2) 0.0207(17) -0.0023(16) 0.0073(16) -0.0156(18) C19 0.032(2) 0.052(3) 0.036(2) -0.0014(19) 0.0090(18) -0.0033(19) C20 0.036(3) 0.179(7) 0.022(2) 0.004(3) -0.004(2) -0.027(3) C21 0.091(4) 0.052(3) 0.050(3) -0.021(2) 0.039(3) -0.029(3) C22 0.0270(18) 0.0162(16) 0.0358(19) -0.0027(14) -0.0089(15) -0.0026(13) C23 0.107(4) 0.022(2) 0.042(3) 0.0008(18) -0.007(3) -0.012(2) C24 0.051(3) 0.025(2) 0.057(3) -0.0086(19) -0.022(2) -0.0064(18) C25 0.037(2) 0.023(2) 0.132(5) -0.028(3) -0.008(3) -0.0003(18) O31 0.0278(12) 0.0164(11) 0.0162(10) 0.0003(8) -0.0068(9) -0.0030(9) C31 0.0203(16) 0.0182(16) 0.0190(15) 0.0016(12) -0.0036(13) -0.0041(12) C32 0.0195(16) 0.0184(16) 0.0175(14) 0.0016(12) -0.0033(12) -0.0030(12) C33 0.0215(16) 0.0229(17) 0.0206(15) 0.0040(13) -0.0058(13) -0.0033(13) C34 0.0294(18) 0.0259(18) 0.0191(16) 0.0009(13) -0.0087(14) -0.0027(14) C35 0.0348(19) 0.0225(17) 0.0192(16) -0.0005(13) -0.0097(15) -0.0025(14) C36 0.0230(16) 0.0184(16) 0.0205(15) 0.0006(12) -0.0054(13) -0.0050(13) N37 0.0213(14) 0.0167(13) 0.0172(12) 0.0010(10) -0.0061(11) -0.0032(11) C38 0.0235(16) 0.0190(16) 0.0152(14) -0.0012(12) -0.0034(13) -0.0028(13) C39 0.0238(17) 0.0207(17) 0.0275(17) -0.0017(13) -0.0110(14) -0.0005(13) C40 0.0261(18) 0.0244(18) 0.0282(17) -0.0058(14) -0.0079(15) -0.0078(14) C41 0.0273(18) 0.0191(17) 0.0220(16) -0.0022(13) -0.0036(14) -0.0030(13) C42 0.0231(17) 0.0245(18) 0.0282(18) -0.0001(14) -0.0075(14) -0.0003(14) C43 0.0254(17) 0.0210(17) 0.0222(16) -0.0028(13) -0.0056(14) -0.0058(13) C44 0.0301(18) 0.0173(16) 0.0195(15) 0.0024(13) -0.0060(14) -0.0010(13) C45 0.0333(19) 0.0169(16) 0.0264(17) 0.0040(13) -0.0046(15) 0.0003(14) C46 0.037(2) 0.0203(17) 0.0302(18) 0.0015(14) -0.0109(16) -0.0084(15) C47 0.036(2) 0.0239(18) 0.0223(17) 0.0002(14) -0.0030(15) 0.0008(15) C48 0.046(2) 0.032(2) 0.0209(17) -0.0007(15) -0.0168(16) -0.0047(17) C49 0.051(3) 0.086(4) 0.0181(18) 0.002(2) -0.0056(18) -0.023(3) C50 0.049(3) 0.124(5) 0.027(2) -0.004(3) -0.010(2) -0.048(3) C51 0.205(8) 0.051(3) 0.050(3) -0.026(3) -0.080(4) 0.035(4) C52 0.032(2) 0.0224(18) 0.0318(19) -0.0057(15) -0.0093(16) 0.0021(15) C53 0.065(3) 0.026(2) 0.029(2) -0.0039(16) 0.001(2) 0.0114(19) C54 0.053(3) 0.019(2) 0.093(4) -0.017(2) -0.034(3) -0.0035(19) C55 0.037(2) 0.0203(18) 0.0314(19) 0.0002(14) -0.0003(16) -0.0014(15) Fe2 0.0185(2) 0.0138(2) 0.0162(2) 0.00068(16) -0.00419(17) -0.00306(17) O101 0.0274(12) 0.0151(11) 0.0192(11) 0.0010(9) -0.0044(10) 0.0000(9) C101 0.0169(15) 0.0184(16) 0.0234(16) 0.0000(13) -0.0036(13) -0.0042(12) C102 0.0190(16) 0.0200(16) 0.0262(17) 0.0006(13) -0.0059(13) -0.0030(13) C103 0.0235(17) 0.0188(17) 0.0318(18) 0.0003(14) -0.0076(15) -0.0005(13) C104 0.0235(17) 0.0239(18) 0.0292(18) -0.0040(14) -0.0016(14) -0.0031(14) C105 0.0254(17) 0.0242(18) 0.0235(16) -0.0024(14) -0.0022(14) -0.0049(14) C106 0.0206(16) 0.0204(16) 0.0219(16) 0.0007(13) -0.0041(13) -0.0050(13) N107 0.0186(13) 0.0192(14) 0.0185(13) 0.0016(10) -0.0026(11) -0.0047(11) C108 0.0227(16) 0.0192(16) 0.0204(15) -0.0009(12) -0.0038(13) -0.0081(13) C109 0.0224(17) 0.0277(18) 0.0234(16) 0.0007(14) -0.0005(14) -0.0055(14) C110 0.0290(19) 0.033(2) 0.0207(16) -0.0007(14) 0.0002(14) -0.0117(15) C111 0.0351(19) 0.0277(18) 0.0177(15) 0.0019(13) -0.0058(14) -0.0161(15) C112 0.0305(19) 0.0234(18) 0.0256(17) 0.0003(14) -0.0098(15) -0.0035(14) C113 0.0257(17) 0.0242(17) 0.0214(16) 0.0001(13) -0.0032(14) -0.0068(14) C114 0.0257(17) 0.0182(16) 0.0254(17) 0.0055(13) -0.0092(14) -0.0004(13) C115 0.034(2) 0.0272(19) 0.0264(17) 0.0039(14) -0.0124(16) -0.0043(15) C116 0.0285(19) 0.030(2) 0.0277(18) 0.0091(15) -0.0043(15) -0.0038(15) C117 0.038(2) 0.0248(19) 0.0299(19) 0.0068(15) -0.0113(17) 0.0016(16) C118 0.034(2) 0.0234(19) 0.040(2) -0.0089(16) -0.0002(17) 0.0019(15) C119 0.091(4) 0.040(3) 0.044(3) -0.016(2) 0.009(3) 0.009(3) C120 0.029(2) 0.040(3) 0.081(3) -0.030(2) 0.003(2) -0.0014(18) C121 0.041(2) 0.028(2) 0.068(3) -0.021(2) -0.001(2) -0.0071(18) C122 0.043(2) 0.034(2) 0.0175(16) 0.0059(14) -0.0092(15) -0.0177(17) C123 0.055(3) 0.080(4) 0.028(2) 0.017(2) -0.020(2) -0.029(3) C124 0.063(3) 0.051(3) 0.0209(18) 0.0030(18) -0.0042(19) -0.018(2) C125 0.076(3) 0.035(2) 0.027(2) 0.0105(17) -0.011(2) -0.020(2) O131 0.0293(12) 0.0175(11) 0.0152(10) 0.0011(9) -0.0039(9) -0.0076(9) C131 0.0164(15) 0.0178(16) 0.0205(15) 0.0002(12) -0.0040(12) -0.0023(12) C132 0.0165(15) 0.0188(16) 0.0218(16) 0.0016(12) -0.0017(13) -0.0020(12) C133 0.0215(16) 0.0162(16) 0.0262(17) 0.0011(13) -0.0041(14) -0.0056(12) C134 0.0192(16) 0.0179(16) 0.0237(16) -0.0012(13) -0.0050(13) -0.0016(12) C135 0.0231(16) 0.0206(16) 0.0188(15) 0.0001(13) -0.0049(13) -0.0036(13) C136 0.0165(15) 0.0170(15) 0.0203(15) 0.0004(12) -0.0045(12) -0.0031(12) N137 0.0194(13) 0.0189(14) 0.0187(13) 0.0021(10) -0.0051(11) -0.0041(11) C138 0.0227(16) 0.0150(15) 0.0163(14) -0.0001(12) -0.0028(12) -0.0036(12) C139 0.0250(17) 0.0202(16) 0.0198(15) -0.0004(12) -0.0071(13) -0.0082(13) C140 0.0228(17) 0.0221(17) 0.0251(17) 0.0001(13) -0.0037(14) -0.0093(13) C141 0.0221(16) 0.0183(16) 0.0166(15) 0.0003(12) -0.0035(13) -0.0023(12) C142 0.0244(17) 0.0277(18) 0.0204(16) 0.0008(13) -0.0099(14) -0.0087(14) C143 0.0216(16) 0.0235(17) 0.0216(16) 0.0018(13) -0.0043(13) -0.0087(13) C144 0.0287(18) 0.0165(16) 0.0203(16) 0.0018(12) -0.0007(14) -0.0036(13) C145 0.037(2) 0.033(2) 0.0245(18) 0.0055(15) -0.0075(16) -0.0069(16) C146 0.034(2) 0.0213(17) 0.0263(17) -0.0017(14) 0.0042(15) -0.0056(15) C147 0.041(2) 0.0171(17) 0.0255(17) 0.0027(14) 0.0083(16) -0.0046(15) C148 0.0312(19) 0.0187(17) 0.0283(17) -0.0068(14) -0.0088(15) -0.0047(14) C149 0.041(2) 0.0209(18) 0.035(2) -0.0056(15) -0.0067(17) -0.0015(16) C150 0.032(2) 0.043(2) 0.058(3) -0.019(2) -0.007(2) -0.0126(18) C151 0.064(3) 0.0239(19) 0.0302(19) -0.0063(15) -0.0149(19) -0.0129(19) C152 0.0244(17) 0.0254(18) 0.0179(15) 0.0031(13) -0.0023(13) -0.0065(14) C153 0.035(2) 0.035(2) 0.0188(16) 0.0005(14) -0.0062(15) -0.0061(16) C154 0.032(2) 0.054(3) 0.0229(18) 0.0076(17) -0.0005(16) -0.0154(18) C155 0.045(2) 0.0248(19) 0.0255(18) 0.0076(14) -0.0051(17) -0.0069(16) O40 0.0157(11) 0.0257(12) 0.0251(11) -0.0048(9) -0.0049(9) -0.0028(9) C60 0.123(9) 0.033(4) 0.014(3) 0.005(3) -0.010(4) -0.061(5) Cl61 0.078(2) 0.115(3) 0.130(3) -0.047(3) -0.013(2) 0.005(2) Cl62 0.069(2) 0.112(3) 0.087(2) -0.020(2) 0.0091(18) -0.0035(19) C70 0.108(5) 0.042(3) 0.053(3) -0.010(2) -0.030(3) 0.013(3) Cl71 0.0723(11) 0.1373(17) 0.0800(11) 0.0223(11) -0.0199(9) -0.0246(11) Cl72 0.1183(17) 0.221(3) 0.0693(11) -0.0085(14) -0.0123(11) -0.0961(18) C80 0.072(5) 0.059(5) 0.226(12) 0.073(6) -0.104(7) -0.045(4) Cl81 0.0463(9) 0.0710(11) 0.0855(12) -0.0074(10) -0.0230(9) -0.0104(8) Cl82 0.0540(11) 0.1002(18) 0.125(2) -0.0488(16) -0.0014(12) -0.0140(11) _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 O40 1.776(2) . ? Fe1 O31 1.968(2) . ? Fe1 O1 1.970(2) . ? Fe1 N37 2.051(3) . ? Fe1 N7 2.057(3) . ? O1 C1 1.296(4) . ? C1 C2 1.434(4) . ? C1 C6 1.447(5) . ? C2 C3 1.375(5) . ? C2 C14 1.527(5) . ? C3 C4 1.426(5) . ? C4 C5 1.374(5) . ? C4 C18 1.538(5) . ? C5 C6 1.422(4) . ? C6 N7 1.348(4) . ? N7 C8 1.412(4) . ? C8 C9 1.391(5) . ? C8 C13 1.397(4) . ? C9 C10 1.390(5) . ? C10 C11 1.392(5) . ? C11 C12 1.403(5) . ? C11 C22 1.526(5) . ? C12 C13 1.381(5) . ? C14 C17 1.535(5) . ? C14 C15 1.537(4) . ? C14 C16 1.544(5) . ? C18 C20 1.521(6) . ? C18 C19 1.525(6) . ? C18 C21 1.547(6) . ? C22 C23 1.522(6) . ? C22 C25 1.526(5) . ? C22 C24 1.534(5) . ? O31 C31 1.300(4) . ? C31 C32 1.431(4) . ? C31 C36 1.448(5) . ? C32 C33 1.383(4) . ? C32 C44 1.529(5) . ? C33 C34 1.421(5) . ? C34 C35 1.364(5) . ? C34 C48 1.534(4) . ? C35 C36 1.428(4) . ? C36 N37 1.340(4) . ? N37 C38 1.417(4) . ? C38 C39 1.391(5) . ? C38 C43 1.395(5) . ? C39 C40 1.392(5) . ? C40 C41 1.391(5) . ? C41 C42 1.399(5) . ? C41 C52 1.529(5) . ? C42 C43 1.376(5) . ? C44 C46 1.532(5) . ? C44 C45 1.535(4) . ? C44 C47 1.546(5) . ? C48 C51 1.519(6) . ? C48 C49 1.525(6) . ? C48 C50 1.529(6) . ? C52 C54 1.530(5) . ? C52 C55 1.539(5) . ? C52 C53 1.540(5) . ? Fe2 O40 1.775(2) . ? Fe2 O131 1.958(2) . ? Fe2 O101 1.961(2) . ? Fe2 N107 2.066(3) . ? Fe2 N137 2.069(3) . ? O101 C101 1.299(4) . ? C101 C102 1.425(4) . ? C101 C106 1.450(4) . ? C102 C103 1.373(5) . ? C102 C114 1.539(5) . ? C103 C104 1.426(5) . ? C104 C105 1.367(5) . ? C104 C118 1.538(5) . ? C105 C106 1.425(5) . ? C106 N107 1.349(4) . ? N107 C108 1.413(4) . ? C108 C109 1.392(5) . ? C108 C113 1.396(5) . ? C109 C110 1.392(5) . ? C110 C111 1.390(5) . ? C111 C112 1.394(5) . ? C111 C122 1.543(4) . ? C112 C113 1.387(5) . ? C114 C117 1.535(4) . ? C114 C116 1.536(5) . ? C114 C115 1.538(5) . ? C118 C120 1.516(6) . ? C118 C121 1.535(6) . ? C118 C119 1.543(6) . ? C122 C124 1.531(6) . ? C122 C125 1.532(5) . ? C122 C123 1.537(5) . ? O131 C131 1.292(4) . ? C131 C132 1.428(4) . ? C131 C136 1.453(4) . ? C132 C133 1.376(5) . ? C132 C144 1.534(4) . ? C133 C134 1.433(4) . ? C134 C135 1.367(4) . ? C134 C148 1.536(5) . ? C135 C136 1.418(4) . ? C136 N137 1.345(4) . ? N137 C138 1.415(4) . ? C138 C143 1.392(4) . ? C138 C139 1.401(4) . ? C139 C140 1.388(4) . ? C140 C141 1.401(4) . ? C141 C142 1.387(5) . ? C141 C152 1.537(4) . ? C142 C143 1.388(4) . ? C144 C145 1.535(5) . ? C144 C147 1.538(4) . ? C144 C146 1.549(5) . ? C148 C149 1.530(5) . ? C148 C151 1.537(5) . ? C148 C150 1.542(5) . ? C152 C154 1.531(5) . ? C152 C153 1.536(5) . ? C152 C155 1.538(5) . ? C60 Cl62 1.675(6) . ? C60 Cl61 1.722(6) . ? C70 Cl71 1.724(5) . ? C70 Cl72 1.732(5) . ? C80 Cl81 1.760(5) . ? C80 Cl82 1.791(6) . ? C85 Cl86 1.731(8) . ? C85 Cl87 1.735(8) . ? Cl91 Cl92 1.736(15) 2_755 ? Cl92 Cl91 1.736(15) 2_755 ? Cl92 Cl92 1.74(2) 2_755 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O40 Fe1 O31 112.40(10) . . ? O40 Fe1 O1 110.92(10) . . ? O31 Fe1 O1 136.68(10) . . ? O40 Fe1 N37 106.84(11) . . ? O31 Fe1 N37 78.84(10) . . ? O1 Fe1 N37 88.94(10) . . ? O40 Fe1 N7 105.10(10) . . ? O31 Fe1 N7 90.04(10) . . ? O1 Fe1 N7 78.76(10) . . ? N37 Fe1 N7 148.04(11) . . ? C1 O1 Fe1 116.9(2) . . ? O1 C1 C2 122.6(3) . . ? O1 C1 C6 117.3(3) . . ? C2 C1 C6 120.1(3) . . ? C3 C2 C1 116.6(3) . . ? C3 C2 C14 123.4(3) . . ? C1 C2 C14 120.0(3) . . ? C2 C3 C4 124.5(3) . . ? C5 C4 C3 119.0(3) . . ? C5 C4 C18 122.4(3) . . ? C3 C4 C18 118.6(3) . . ? C4 C5 C6 119.9(3) . . ? N7 C6 C5 127.9(3) . . ? N7 C6 C1 112.2(3) . . ? C5 C6 C1 119.8(3) . . ? C6 N7 C8 124.3(3) . . ? C6 N7 Fe1 114.6(2) . . ? C8 N7 Fe1 121.1(2) . . ? C9 C8 C13 118.5(3) . . ? C9 C8 N7 124.7(3) . . ? C13 C8 N7 116.6(3) . . ? C10 C9 C8 120.3(3) . . ? C9 C10 C11 121.9(3) . . ? C10 C11 C12 117.2(3) . . ? C10 C11 C22 122.7(3) . . ? C12 C11 C22 120.1(3) . . ? C13 C12 C11 121.4(3) . . ? C12 C13 C8 120.8(3) . . ? C2 C14 C17 109.4(3) . . ? C2 C14 C15 110.6(3) . . ? C17 C14 C15 107.8(3) . . ? C2 C14 C16 110.9(3) . . ? C17 C14 C16 110.1(3) . . ? C15 C14 C16 108.0(3) . . ? C20 C18 C19 107.9(4) . . ? C20 C18 C4 109.0(3) . . ? C19 C18 C4 110.3(3) . . ? C20 C18 C21 113.1(4) . . ? C19 C18 C21 105.2(4) . . ? C4 C18 C21 111.3(3) . . ? C23 C22 C25 109.3(4) . . ? C23 C22 C11 109.8(3) . . ? C25 C22 C11 112.3(3) . . ? C23 C22 C24 109.7(4) . . ? C25 C22 C24 107.5(4) . . ? C11 C22 C24 108.4(3) . . ? C31 O31 Fe1 117.0(2) . . ? O31 C31 C32 123.0(3) . . ? O31 C31 C36 116.6(3) . . ? C32 C31 C36 120.3(3) . . ? C33 C32 C31 116.3(3) . . ? C33 C32 C44 123.2(3) . . ? C31 C32 C44 120.5(3) . . ? C32 C33 C34 124.5(3) . . ? C35 C34 C33 119.4(3) . . ? C35 C34 C48 122.4(3) . . ? C33 C34 C48 118.2(3) . . ? C34 C35 C36 119.9(3) . . ? N37 C36 C35 127.6(3) . . ? N37 C36 C31 112.8(3) . . ? C35 C36 C31 119.5(3) . . ? C36 N37 C38 123.7(3) . . ? C36 N37 Fe1 114.7(2) . . ? C38 N37 Fe1 121.56(19) . . ? C39 C38 C43 119.0(3) . . ? C39 C38 N37 123.3(3) . . ? C43 C38 N37 117.4(3) . . ? C38 C39 C40 119.6(3) . . ? C41 C40 C39 122.1(3) . . ? C40 C41 C42 116.9(3) . . ? C40 C41 C52 123.1(3) . . ? C42 C41 C52 120.0(3) . . ? C43 C42 C41 121.8(3) . . ? C42 C43 C38 120.4(3) . . ? C32 C44 C46 109.1(3) . . ? C32 C44 C45 111.1(3) . . ? C46 C44 C45 107.9(3) . . ? C32 C44 C47 111.0(3) . . ? C46 C44 C47 109.6(3) . . ? C45 C44 C47 108.0(3) . . ? C51 C48 C49 106.9(4) . . ? C51 C48 C50 111.4(5) . . ? C49 C48 C50 107.2(4) . . ? C51 C48 C34 112.3(3) . . ? C49 C48 C34 110.8(3) . . ? C50 C48 C34 108.1(3) . . ? C41 C52 C54 112.0(3) . . ? C41 C52 C55 110.0(3) . . ? C54 C52 C55 107.1(3) . . ? C41 C52 C53 108.1(3) . . ? C54 C52 C53 110.1(4) . . ? C55 C52 C53 109.6(3) . . ? O40 Fe2 O131 112.34(10) . . ? O40 Fe2 O101 111.18(10) . . ? O131 Fe2 O101 136.47(10) . . ? O40 Fe2 N107 103.33(10) . . ? O131 Fe2 N107 91.61(10) . . ? O101 Fe2 N107 78.80(10) . . ? O40 Fe2 N137 105.46(11) . . ? O131 Fe2 N137 78.68(10) . . ? O101 Fe2 N137 89.64(10) . . ? N107 Fe2 N137 151.19(11) . . ? C101 O101 Fe2 116.84(19) . . ? O101 C101 C102 122.7(3) . . ? O101 C101 C106 117.1(3) . . ? C102 C101 C106 120.2(3) . . ? C103 C102 C101 116.6(3) . . ? C103 C102 C114 123.2(3) . . ? C101 C102 C114 120.1(3) . . ? C102 C103 C104 124.6(3) . . ? C105 C104 C103 119.0(3) . . ? C105 C104 C118 123.3(3) . . ? C103 C104 C118 117.7(3) . . ? C104 C105 C106 120.0(3) . . ? N107 C106 C105 128.0(3) . . ? N107 C106 C101 112.4(3) . . ? C105 C106 C101 119.5(3) . . ? C106 N107 C108 123.7(3) . . ? C106 N107 Fe2 114.0(2) . . ? C108 N107 Fe2 122.3(2) . . ? C109 C108 C113 118.7(3) . . ? C109 C108 N107 124.1(3) . . ? C113 C108 N107 117.0(3) . . ? C108 C109 C110 120.1(3) . . ? C111 C110 C109 121.9(3) . . ? C110 C111 C112 117.2(3) . . ? C110 C111 C122 121.8(3) . . ? C112 C111 C122 120.9(3) . . ? C113 C112 C111 121.8(3) . . ? C112 C113 C108 120.2(3) . . ? C117 C114 C116 107.9(3) . . ? C117 C114 C115 108.2(3) . . ? C116 C114 C115 109.6(3) . . ? C117 C114 C102 111.5(3) . . ? C116 C114 C102 108.2(3) . . ? C115 C114 C102 111.3(3) . . ? C120 C118 C121 109.7(3) . . ? C120 C118 C104 109.0(3) . . ? C121 C118 C104 109.9(3) . . ? C120 C118 C119 109.3(4) . . ? C121 C118 C119 107.3(4) . . ? C104 C118 C119 111.6(3) . . ? C124 C122 C125 108.7(3) . . ? C124 C122 C123 108.3(3) . . ? C125 C122 C123 109.7(4) . . ? C124 C122 C111 111.6(3) . . ? C125 C122 C111 108.3(3) . . ? C123 C122 C111 110.3(3) . . ? C131 O131 Fe2 117.38(19) . . ? O131 C131 C132 122.9(3) . . ? O131 C131 C136 117.4(3) . . ? C132 C131 C136 119.7(3) . . ? C133 C132 C131 117.1(3) . . ? C133 C132 C144 122.9(3) . . ? C131 C132 C144 120.0(3) . . ? C132 C133 C134 124.0(3) . . ? C135 C134 C133 119.0(3) . . ? C135 C134 C148 122.5(3) . . ? C133 C134 C148 118.4(3) . . ? C134 C135 C136 120.1(3) . . ? N137 C136 C135 128.0(3) . . ? N137 C136 C131 112.0(3) . . ? C135 C136 C131 119.9(3) . . ? C136 N137 C138 122.9(3) . . ? C136 N137 Fe2 114.4(2) . . ? C138 N137 Fe2 122.6(2) . . ? C143 C138 C139 118.2(3) . . ? C143 C138 N137 123.9(3) . . ? C139 C138 N137 117.7(3) . . ? C140 C139 C138 120.4(3) . . ? C139 C140 C141 121.6(3) . . ? C142 C141 C140 117.1(3) . . ? C142 C141 C152 122.1(3) . . ? C140 C141 C152 120.7(3) . . ? C141 C142 C143 122.1(3) . . ? C142 C143 C138 120.5(3) . . ? C132 C144 C145 109.2(3) . . ? C132 C144 C147 111.1(3) . . ? C145 C144 C147 108.2(3) . . ? C132 C144 C146 111.1(3) . . ? C145 C144 C146 109.6(3) . . ? C147 C144 C146 107.5(3) . . ? C149 C148 C134 111.0(3) . . ? C149 C148 C151 108.6(3) . . ? C134 C148 C151 111.9(3) . . ? C149 C148 C150 108.8(3) . . ? C134 C148 C150 108.0(3) . . ? C151 C148 C150 108.4(3) . . ? C154 C152 C153 108.1(3) . . ? C154 C152 C141 110.7(3) . . ? C153 C152 C141 111.6(3) . . ? C154 C152 C155 109.1(3) . . ? C153 C152 C155 108.9(3) . . ? C141 C152 C155 108.3(3) . . ? Fe2 O40 Fe1 175.21(15) . . ? Cl62 C60 Cl61 114.7(4) . . ? Cl71 C70 Cl72 111.9(3) . . ? Cl81 C80 Cl82 108.8(3) . . ? Cl86 C85 Cl87 107.3(7) . . ? Cl91 Cl92 Cl92 111.5(11) 2_755 2_755 ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 1.083 _refine_diff_density_min -1.032 _refine_diff_density_rms 0.078 #===END