# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Prof. Dr. Sascha Ott' _publ_contact_author_address ; Institute for Chemistry, University of Kassel, Heinrich-Plett-Str. 40, 34132 Kassel Germany ; _publ_contact_author_phone '+46-18-471 7340' _publ_contact_author_fax +46-18-471-6844 _publ_contact_author_email sascha.ott@fotomol.uu.se _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission as a pre publication in "Chem. Comm.". Clemens Bruhn ; #===================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_paper_category ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _iucr_compatibility_tag ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #===================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Gating the Protonation of the Iron-Iron Bond in [FeFe] Hydrogenase Active Site Models by Modifications to the Second Coordination Sphere ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Ezzaher, Salah' ? ; Department of Photochemistry and Molecular Science, \\%Angstr\"om Laboratories, Uppsala University, Box 523, 75120 Uppsala Sweden ; 'Gogoll, Adolf' ? ; Department of Biochemistry and Organic Chemistry, Uppsala University, Box 576, 75123 Uppsala Sweden ; 'Bruhn, Clemens' ? ; Institute for Chemistry, University of Kassel, Heinrich-Plett-Str. 40, 34132 Kassel Germany ; 'Ott, Sascha' ? ; Department of Photochemistry and Molecular Science, \\%Angstr\"om Laboratories, Uppsala University, Box 523, 75120 Uppsala Sweden ; #====================================================================== data_i0602a _database_code_depnum_ccdc_archive 'CCDC 762982' #TrackingRef 'i0602a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H29 Cl2 Fe2 N O4 P2 S2' _chemical_formula_sum 'C37 H29 Cl2 Fe2 N O4 P2 S2' _chemical_formula_weight 860.27 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.8131(9) _cell_length_b 25.2997(13) _cell_length_c 18.4815(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.763(4) _cell_angle_gamma 90.00 _cell_volume 7385.2(7) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16634 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 25.53 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 1.171 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6917 _exptl_absorpt_correction_T_max 0.9485 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 47501 _diffrn_reflns_av_R_equivalents 0.1052 _diffrn_reflns_av_sigmaI/netI 0.1289 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12999 _reflns_number_gt 6663 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12999 _refine_ls_number_parameters 903 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1291 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1133 _refine_ls_wR_factor_gt 0.0943 _refine_ls_goodness_of_fit_ref 0.851 _refine_ls_restrained_S_all 0.851 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1090(4) 0.6220(2) 0.2209(3) 0.0320(14) Uani 1 1 d . . . H1A H -0.0912 0.6534 0.2497 0.038 Uiso 1 1 calc R . . H1B H -0.0586 0.5992 0.2160 0.038 Uiso 1 1 calc R . . C2 C -0.1470(4) 0.5951(2) 0.0961(3) 0.0342(14) Uani 1 1 d . . . H2A H -0.0906 0.5782 0.0954 0.041 Uiso 1 1 calc R . . H2B H -0.1595 0.6102 0.0473 0.041 Uiso 1 1 calc R . . C3 C -0.0838(4) 0.6798(3) 0.1206(4) 0.0418(16) Uani 1 1 d . . . H3C H -0.1029 0.6897 0.0712 0.050 Uiso 1 1 calc R . . H3B H -0.0261 0.6657 0.1204 0.050 Uiso 1 1 calc R . . H3A H -0.0846 0.7110 0.1520 0.050 Uiso 1 1 calc R . . C4 C -0.1399(4) 0.5828(2) 0.3613(3) 0.0320(14) Uani 1 1 d . . . C5 C -0.0590(4) 0.5598(3) 0.3706(4) 0.0432(17) Uani 1 1 d . . . H5A H -0.0309 0.5470 0.3298 0.052 Uiso 1 1 calc R . . C6 C -0.0201(5) 0.5560(3) 0.4407(4) 0.0487(19) Uani 1 1 d . . . H6A H 0.0348 0.5409 0.4467 0.058 Uiso 1 1 calc R . . C7 C -0.0592(5) 0.5733(3) 0.4995(4) 0.0516(19) Uani 1 1 d . . . H7A H -0.0319 0.5705 0.5463 0.062 Uiso 1 1 calc R . . C8 C -0.1388(5) 0.5950(3) 0.4914(4) 0.057(2) Uani 1 1 d . . . H8A H -0.1670 0.6064 0.5329 0.069 Uiso 1 1 calc R . . C9 C -0.1788(5) 0.6005(3) 0.4221(4) 0.0484(18) Uani 1 1 d . . . H9A H -0.2331 0.6164 0.4171 0.058 Uiso 1 1 calc R . . C10 C -0.2722(4) 0.6358(2) 0.2774(3) 0.0317(14) Uani 1 1 d . . . C11 C -0.3577(4) 0.6239(3) 0.2653(4) 0.0404(16) Uani 1 1 d . . . H11A H -0.3743 0.5889 0.2526 0.048 Uiso 1 1 calc R . . C12 C -0.4196(4) 0.6629(3) 0.2714(4) 0.0449(17) Uani 1 1 d . . . H12A H -0.4777 0.6543 0.2629 0.054 Uiso 1 1 calc R . . C13 C -0.3964(5) 0.7140(3) 0.2897(4) 0.053(2) Uani 1 1 d . . . H13A H -0.4386 0.7404 0.2942 0.064 Uiso 1 1 calc R . . C14 C -0.3117(6) 0.7268(3) 0.3016(4) 0.056(2) Uani 1 1 d . . . H14A H -0.2954 0.7619 0.3142 0.068 Uiso 1 1 calc R . . C15 C -0.2505(5) 0.6876(3) 0.2950(4) 0.0515(19) Uani 1 1 d . . . H15A H -0.1925 0.6966 0.3026 0.062 Uiso 1 1 calc R . . C16 C -0.2045(4) 0.5043(2) 0.0288(3) 0.0329(14) Uani 1 1 d . . . C17 C -0.2406(5) 0.5188(3) -0.0383(4) 0.0465(17) Uani 1 1 d . . . H17A H -0.2827 0.5456 -0.0412 0.056 Uiso 1 1 calc R . . C18 C -0.2156(5) 0.4948(3) -0.1010(4) 0.058(2) Uani 1 1 d . . . H18A H -0.2415 0.5051 -0.1463 0.069 Uiso 1 1 calc R . . C19 C -0.1547(5) 0.4565(3) -0.0992(4) 0.0541(19) Uani 1 1 d . . . H19A H -0.1372 0.4409 -0.1428 0.065 Uiso 1 1 calc R . . C20 C -0.1183(5) 0.4407(3) -0.0323(4) 0.059(2) Uani 1 1 d . . . H20A H -0.0761 0.4139 -0.0300 0.071 Uiso 1 1 calc R . . C21 C -0.1441(5) 0.4643(3) 0.0305(4) 0.0491(18) Uani 1 1 d . . . H21A H -0.1198 0.4529 0.0759 0.059 Uiso 1 1 calc R . . C22 C -0.3295(4) 0.5738(3) 0.0881(3) 0.0336(15) Uani 1 1 d . . . C23 C -0.3404(4) 0.6279(3) 0.0907(3) 0.0382(15) Uani 1 1 d . . . H23A H -0.2930 0.6502 0.1016 0.046 Uiso 1 1 calc R . . C24 C -0.4205(4) 0.6502(3) 0.0773(4) 0.0432(17) Uani 1 1 d . . . H24A H -0.4273 0.6875 0.0791 0.052 Uiso 1 1 calc R . . C25 C -0.4904(4) 0.6179(3) 0.0613(4) 0.0469(18) Uani 1 1 d . . . H25A H -0.5447 0.6331 0.0518 0.056 Uiso 1 1 calc R . . C26 C -0.4802(4) 0.5640(3) 0.0592(4) 0.0438(17) Uani 1 1 d . . . H26A H -0.5280 0.5420 0.0492 0.053 Uiso 1 1 calc R . . C27 C -0.4006(4) 0.5410(3) 0.0717(3) 0.0403(16) Uani 1 1 d . . . H27A H -0.3941 0.5037 0.0693 0.048 Uiso 1 1 calc R . . C28 C -0.3237(4) 0.3583(3) 0.2607(4) 0.0447(17) Uani 1 1 d . . . C29 C -0.1698(5) 0.3794(3) 0.2092(4) 0.0432(17) Uani 1 1 d . . . C30 C -0.3043(4) 0.4031(3) 0.1297(4) 0.0468(18) Uani 1 1 d . . . C31 C -0.1047(4) 0.4949(2) 0.2068(3) 0.0337(14) Uani 1 1 d . . . C32 C -0.3638(4) 0.4906(2) 0.3235(3) 0.0343(14) Uani 1 1 d . . . C33 C -0.2928(4) 0.4748(3) 0.3679(3) 0.0375(15) Uani 1 1 d . . . C34 C -0.2944(4) 0.4803(3) 0.4423(4) 0.0445(17) Uani 1 1 d . . . C35 C -0.3637(5) 0.5033(3) 0.4732(4) 0.056(2) Uani 1 1 d . . . H35A H -0.3633 0.5079 0.5243 0.067 Uiso 1 1 calc R . . C36 C -0.4332(5) 0.5197(3) 0.4310(4) 0.057(2) Uani 1 1 d . . . H36A H -0.4802 0.5361 0.4522 0.069 Uiso 1 1 calc R . . C37 C -0.4324(4) 0.5115(3) 0.3558(4) 0.0426(16) Uani 1 1 d . . . C38 C -0.4182(4) 0.6346(3) -0.2406(3) 0.0352(15) Uani 1 1 d . . . H38A H -0.4675 0.6581 -0.2342 0.042 Uiso 1 1 calc R . . H38B H -0.4388 0.6026 -0.2667 0.042 Uiso 1 1 calc R . . C39 C -0.3710(4) 0.6643(2) -0.1182(3) 0.0329(14) Uani 1 1 d . . . H39A H -0.3556 0.6501 -0.0694 0.039 Uiso 1 1 calc R . . H39B H -0.4267 0.6818 -0.1155 0.039 Uiso 1 1 calc R . . C40 C -0.4363(4) 0.5791(3) -0.1372(4) 0.0418(16) Uani 1 1 d . . . H40C H -0.4129 0.5687 -0.0892 0.050 Uiso 1 1 calc R . . H40B H -0.4395 0.5481 -0.1690 0.050 Uiso 1 1 calc R . . H40A H -0.4932 0.5938 -0.1327 0.050 Uiso 1 1 calc R . . C41 C -0.3956(4) 0.6686(2) -0.3858(3) 0.0330(14) Uani 1 1 d . . . C42 C -0.4835(5) 0.6726(4) -0.3942(4) 0.076(3) Uani 1 1 d . . . H42A H -0.5163 0.6760 -0.3527 0.091 Uiso 1 1 calc R . . C43 C -0.5231(5) 0.6718(5) -0.4625(4) 0.088(4) Uani 1 1 d . . . H43A H -0.5831 0.6740 -0.4676 0.106 Uiso 1 1 calc R . . C44 C -0.4767(5) 0.6678(4) -0.5228(4) 0.060(2) Uani 1 1 d . . . H44A H -0.5044 0.6662 -0.5695 0.072 Uiso 1 1 calc R . . C45 C -0.3900(5) 0.6660(3) -0.5157(4) 0.0518(19) Uani 1 1 d . . . H45A H -0.3574 0.6643 -0.5575 0.062 Uiso 1 1 calc R . . C46 C -0.3497(4) 0.6666(3) -0.4469(4) 0.0441(17) Uani 1 1 d . . . H46A H -0.2897 0.6657 -0.4423 0.053 Uiso 1 1 calc R . . C47 C -0.2630(4) 0.6155(3) -0.3051(3) 0.0342(14) Uani 1 1 d . . . C48 C -0.2894(4) 0.5643(2) -0.3239(3) 0.0398(16) Uani 1 1 d . . . H48A H -0.3478 0.5577 -0.3346 0.048 Uiso 1 1 calc R . . C49 C -0.2325(5) 0.5233(3) -0.3272(4) 0.0488(18) Uani 1 1 d . . . H49A H -0.2519 0.4886 -0.3385 0.059 Uiso 1 1 calc R . . C50 C -0.1463(5) 0.5329(3) -0.3138(4) 0.0471(18) Uani 1 1 d . . . H50A H -0.1069 0.5047 -0.3165 0.056 Uiso 1 1 calc R . . C51 C -0.1184(4) 0.5828(3) -0.2969(4) 0.0424(16) Uani 1 1 d . . . H51A H -0.0596 0.5891 -0.2883 0.051 Uiso 1 1 calc R . . C52 C -0.1757(4) 0.6245(3) -0.2923(3) 0.0366(15) Uani 1 1 d . . . H52A H -0.1558 0.6590 -0.2805 0.044 Uiso 1 1 calc R . . C53 C -0.3071(4) 0.7577(3) -0.0595(3) 0.0350(15) Uani 1 1 d . . . C54 C -0.3589(4) 0.8028(3) -0.0630(4) 0.0469(17) Uani 1 1 d . . . H54A H -0.3864 0.8128 -0.1078 0.056 Uiso 1 1 calc R . . C55 C -0.3701(5) 0.8327(3) -0.0016(5) 0.059(2) Uani 1 1 d . . . H55A H -0.4051 0.8633 -0.0049 0.070 Uiso 1 1 calc R . . C56 C -0.3313(5) 0.8191(3) 0.0647(4) 0.057(2) Uani 1 1 d . . . H56A H -0.3385 0.8405 0.1062 0.068 Uiso 1 1 calc R . . C57 C -0.2815(5) 0.7736(3) 0.0694(4) 0.0540(19) Uani 1 1 d . . . H57A H -0.2552 0.7633 0.1145 0.065 Uiso 1 1 calc R . . C58 C -0.2707(4) 0.7435(3) 0.0080(4) 0.0445(17) Uani 1 1 d . . . H58A H -0.2375 0.7122 0.0120 0.053 Uiso 1 1 calc R . . C59 C -0.1894(4) 0.6858(2) -0.1159(3) 0.0345(14) Uani 1 1 d . . . C60 C -0.1197(4) 0.7193(3) -0.0965(3) 0.0401(16) Uani 1 1 d . . . H60A H -0.1278 0.7564 -0.0936 0.048 Uiso 1 1 calc R . . C61 C -0.0399(4) 0.6981(3) -0.0818(4) 0.0498(19) Uani 1 1 d . . . H61A H 0.0063 0.7208 -0.0690 0.060 Uiso 1 1 calc R . . C62 C -0.0274(4) 0.6452(3) -0.0855(4) 0.052(2) Uani 1 1 d . . . H62A H 0.0276 0.6312 -0.0753 0.063 Uiso 1 1 calc R . . C63 C -0.0936(4) 0.6111(3) -0.1042(4) 0.0482(18) Uani 1 1 d . . . H63A H -0.0842 0.5740 -0.1062 0.058 Uiso 1 1 calc R . . C64 C -0.1750(4) 0.6321(3) -0.1200(3) 0.0381(16) Uani 1 1 d . . . H64A H -0.2204 0.6090 -0.1336 0.046 Uiso 1 1 calc R . . C65 C -0.1788(4) 0.8872(3) -0.2996(4) 0.0413(16) Uani 1 1 d . . . C66 C -0.3342(4) 0.8754(2) -0.2307(4) 0.0349(15) Uani 1 1 d . . . C67 C -0.1970(4) 0.8522(3) -0.1639(4) 0.0417(17) Uani 1 1 d . . . C68 C -0.4144(4) 0.7610(2) -0.2330(3) 0.0332(14) Uani 1 1 d . . . C69 C -0.1609(4) 0.7605(2) -0.3593(3) 0.0325(14) Uani 1 1 d . . . C70 C -0.2303(4) 0.7805(2) -0.4000(3) 0.0339(14) Uani 1 1 d . . . C71 C -0.2278(4) 0.7800(3) -0.4753(4) 0.0428(16) Uani 1 1 d . . . C72 C -0.1583(5) 0.7603(3) -0.5104(4) 0.0520(19) Uani 1 1 d . . . H72A H -0.1573 0.7611 -0.5618 0.062 Uiso 1 1 calc R . . C73 C -0.0914(5) 0.7400(3) -0.4696(4) 0.055(2) Uani 1 1 d . . . H73A H -0.0442 0.7260 -0.4932 0.066 Uiso 1 1 calc R . . C74 C -0.0910(4) 0.7392(3) -0.3945(4) 0.0451(17) Uani 1 1 d . . . N1 N -0.1407(3) 0.63927(19) 0.1479(3) 0.0312(11) Uani 1 1 d . . . N2 N -0.3814(3) 0.6192(2) -0.1682(3) 0.0347(12) Uani 1 1 d . . . O1 O -0.3543(3) 0.3207(2) 0.2826(3) 0.0635(15) Uani 1 1 d . . . O2 O -0.1057(3) 0.3575(2) 0.2041(3) 0.0577(14) Uani 1 1 d . . . O3 O -0.3313(3) 0.3980(2) 0.0701(3) 0.0573(14) Uani 1 1 d . . . O4 O -0.0331(3) 0.48756(19) 0.1990(3) 0.0473(12) Uani 1 1 d . . . O5 O -0.1390(3) 0.9173(2) -0.3288(3) 0.0641(15) Uani 1 1 d . . . O6 O -0.3940(3) 0.89918(19) -0.2162(3) 0.0530(13) Uani 1 1 d . . . O7 O -0.1668(3) 0.8622(2) -0.1073(3) 0.0584(14) Uani 1 1 d . . . O8 O -0.4858(3) 0.77041(18) -0.2212(3) 0.0443(11) Uani 1 1 d . . . P1 P -0.18977(9) 0.58510(6) 0.26955(8) 0.0294(3) Uani 1 1 d . . . P2 P -0.22617(9) 0.54236(6) 0.11096(8) 0.0278(3) Uani 1 1 d . . . P3 P -0.34094(10) 0.66896(6) -0.29542(9) 0.0303(4) Uani 1 1 d . . . P4 P -0.29240(9) 0.71555(6) -0.13904(8) 0.0292(3) Uani 1 1 d . . . S1 S -0.35343(9) 0.48482(6) 0.22811(9) 0.0327(4) Uani 1 1 d . . . S2 S -0.20368(10) 0.45302(6) 0.32059(9) 0.0336(4) Uani 1 1 d . . . S3 S -0.16788(9) 0.76242(6) -0.26270(8) 0.0318(3) Uani 1 1 d . . . S4 S -0.31691(9) 0.80213(6) -0.34956(9) 0.0330(4) Uani 1 1 d . . . Cl1 Cl -0.52360(10) 0.53054(8) 0.30281(11) 0.0531(5) Uani 1 1 d . . . Cl2 Cl -0.20929(13) 0.45965(9) 0.49790(10) 0.0620(5) Uani 1 1 d . . . Cl3 Cl -0.00886(12) 0.71113(9) -0.34664(13) 0.0688(6) Uani 1 1 d . . . Cl4 Cl -0.31426(12) 0.80542(8) -0.52739(10) 0.0537(5) Uani 1 1 d . . . Fe1 Fe -0.26740(5) 0.41223(4) 0.22149(5) 0.0339(2) Uani 1 1 d . . . Fe2 Fe -0.21242(5) 0.50617(3) 0.22006(5) 0.0272(2) Uani 1 1 d . . . Fe3 Fe -0.30931(5) 0.74828(3) -0.24990(5) 0.0281(2) Uani 1 1 d . . . Fe4 Fe -0.24237(5) 0.83929(4) -0.25241(5) 0.0326(2) 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 C1 0.036(3) 0.034(3) 0.024(3) 0.001(3) -0.005(3) 0.000(3) C2 0.032(3) 0.041(4) 0.029(3) 0.000(3) -0.002(3) 0.004(3) C3 0.049(4) 0.043(4) 0.032(4) 0.010(3) -0.007(3) -0.015(3) C4 0.032(3) 0.035(3) 0.028(3) 0.003(3) -0.001(3) -0.002(3) C5 0.035(3) 0.060(4) 0.035(4) -0.002(3) -0.002(3) -0.001(3) C6 0.044(4) 0.060(5) 0.041(4) 0.004(4) -0.009(4) -0.002(4) C7 0.062(5) 0.054(4) 0.038(4) -0.002(4) -0.011(4) -0.007(4) C8 0.082(6) 0.059(5) 0.030(4) -0.008(3) 0.001(4) 0.018(4) C9 0.055(4) 0.057(5) 0.032(4) 0.003(3) -0.001(3) 0.018(4) C10 0.037(3) 0.030(3) 0.028(3) -0.001(3) 0.000(3) 0.005(3) C11 0.040(4) 0.045(4) 0.036(4) -0.002(3) 0.000(3) 0.006(3) C12 0.039(4) 0.056(5) 0.040(4) 0.004(3) 0.001(3) 0.017(3) C13 0.068(5) 0.060(5) 0.032(4) 0.002(4) 0.004(4) 0.032(4) C14 0.083(6) 0.034(4) 0.051(5) -0.009(3) 0.000(4) 0.012(4) C15 0.057(4) 0.041(4) 0.056(5) -0.002(4) -0.002(4) -0.001(3) C16 0.028(3) 0.036(3) 0.034(4) 0.003(3) -0.001(3) -0.008(3) C17 0.053(4) 0.048(4) 0.038(4) -0.008(3) -0.005(3) 0.004(3) C18 0.083(5) 0.059(5) 0.030(4) -0.018(4) -0.006(4) 0.010(4) C19 0.067(5) 0.049(4) 0.047(4) -0.020(4) 0.007(4) 0.005(4) C20 0.077(5) 0.058(5) 0.041(4) -0.011(4) 0.002(4) 0.024(4) C21 0.063(5) 0.050(4) 0.034(4) 0.004(3) 0.003(4) 0.013(4) C22 0.031(3) 0.047(4) 0.022(3) -0.001(3) -0.003(3) 0.004(3) C23 0.035(3) 0.048(4) 0.031(4) 0.011(3) 0.000(3) 0.003(3) C24 0.041(4) 0.047(4) 0.041(4) 0.003(3) -0.001(3) 0.011(3) C25 0.036(4) 0.063(5) 0.042(4) 0.009(4) 0.000(3) 0.012(3) C26 0.026(3) 0.068(5) 0.037(4) 0.005(3) -0.001(3) 0.006(3) C27 0.038(4) 0.047(4) 0.034(4) 0.008(3) -0.007(3) 0.001(3) C28 0.039(4) 0.035(4) 0.060(5) -0.002(3) -0.001(4) 0.006(3) C29 0.048(4) 0.040(4) 0.041(4) -0.003(3) -0.004(3) -0.004(3) C30 0.045(4) 0.046(4) 0.050(5) -0.008(4) 0.005(4) -0.001(3) C31 0.045(4) 0.031(3) 0.025(3) 0.003(3) -0.001(3) -0.005(3) C32 0.036(3) 0.038(3) 0.030(3) 0.002(3) 0.004(3) -0.006(3) C33 0.039(3) 0.045(4) 0.029(3) 0.004(3) 0.010(3) -0.003(3) C34 0.044(4) 0.050(4) 0.040(4) 0.005(3) 0.002(3) 0.001(3) C35 0.064(5) 0.075(5) 0.028(4) 0.000(4) 0.008(4) 0.007(4) C36 0.050(4) 0.071(5) 0.052(5) -0.005(4) 0.018(4) 0.006(4) C37 0.040(4) 0.044(4) 0.044(4) 0.002(3) 0.007(3) 0.007(3) C38 0.027(3) 0.041(4) 0.037(4) 0.000(3) -0.003(3) 0.001(3) C39 0.034(3) 0.039(3) 0.025(3) 0.001(3) 0.000(3) -0.002(3) C40 0.039(3) 0.047(4) 0.039(4) 0.012(3) -0.002(3) -0.014(3) C41 0.031(3) 0.035(3) 0.032(3) -0.002(3) -0.003(3) -0.001(3) C42 0.040(4) 0.153(9) 0.035(4) 0.000(5) 0.002(3) 0.017(5) C43 0.039(4) 0.191(11) 0.032(4) 0.012(6) -0.010(4) 0.020(6) C44 0.046(4) 0.097(6) 0.036(4) -0.003(4) -0.015(4) 0.006(4) C45 0.049(4) 0.079(5) 0.027(4) -0.001(4) 0.004(3) 0.018(4) C46 0.034(3) 0.061(5) 0.037(4) 0.001(3) -0.004(3) 0.009(3) C47 0.032(3) 0.044(4) 0.026(3) 0.004(3) 0.000(3) 0.007(3) C48 0.047(4) 0.036(4) 0.036(4) -0.007(3) -0.004(3) 0.004(3) C49 0.058(4) 0.041(4) 0.047(4) -0.002(3) -0.001(4) 0.002(3) C50 0.054(4) 0.046(4) 0.042(4) 0.007(3) 0.003(3) 0.015(3) C51 0.036(3) 0.047(4) 0.044(4) -0.002(3) -0.002(3) 0.012(3) C52 0.041(4) 0.035(3) 0.033(4) 0.003(3) -0.002(3) -0.001(3) C53 0.032(3) 0.041(4) 0.032(4) -0.001(3) 0.000(3) -0.009(3) C54 0.041(4) 0.047(4) 0.053(5) 0.002(4) 0.004(3) 0.011(3) C55 0.059(5) 0.041(4) 0.077(6) -0.007(4) 0.017(4) 0.005(4) C56 0.071(5) 0.053(5) 0.048(5) -0.017(4) 0.013(4) -0.009(4) C57 0.067(5) 0.057(5) 0.037(4) -0.009(4) -0.002(4) 0.001(4) C58 0.054(4) 0.041(4) 0.039(4) -0.002(3) -0.001(3) 0.004(3) C59 0.037(3) 0.038(4) 0.029(3) 0.007(3) 0.002(3) 0.002(3) C60 0.034(3) 0.050(4) 0.036(4) 0.009(3) -0.004(3) 0.003(3) C61 0.028(3) 0.075(5) 0.046(4) 0.017(4) -0.006(3) -0.003(3) C62 0.038(4) 0.070(5) 0.048(5) 0.022(4) -0.002(3) 0.014(4) C63 0.042(4) 0.056(4) 0.047(4) 0.006(4) 0.002(3) 0.020(3) C64 0.035(3) 0.049(4) 0.030(3) -0.002(3) -0.006(3) 0.012(3) C65 0.039(4) 0.044(4) 0.041(4) -0.005(3) 0.000(3) 0.004(3) C66 0.033(3) 0.034(3) 0.037(4) 0.002(3) 0.000(3) -0.001(3) C67 0.029(3) 0.044(4) 0.051(5) -0.005(3) -0.004(3) 0.003(3) C68 0.032(3) 0.034(3) 0.033(4) 0.009(3) -0.005(3) 0.000(3) C69 0.035(3) 0.029(3) 0.034(3) 0.005(3) 0.007(3) 0.004(3) C70 0.041(3) 0.026(3) 0.034(4) 0.002(3) -0.001(3) -0.004(3) C71 0.048(4) 0.049(4) 0.032(4) 0.005(3) 0.003(3) 0.001(3) C72 0.069(5) 0.048(4) 0.039(4) 0.001(3) 0.011(4) 0.009(4) C73 0.058(5) 0.059(5) 0.051(5) 0.009(4) 0.027(4) 0.012(4) C74 0.040(4) 0.048(4) 0.048(4) 0.006(3) 0.011(3) 0.007(3) N1 0.033(3) 0.033(3) 0.027(3) 0.001(2) -0.005(2) -0.004(2) N2 0.038(3) 0.040(3) 0.026(3) 0.003(2) -0.003(2) -0.002(2) O1 0.060(3) 0.051(3) 0.080(4) 0.014(3) 0.016(3) -0.010(3) O2 0.039(3) 0.051(3) 0.083(4) -0.005(3) 0.009(3) 0.010(2) O3 0.062(3) 0.065(3) 0.044(3) -0.011(3) -0.006(3) 0.003(3) O4 0.025(2) 0.057(3) 0.061(3) 0.001(2) 0.001(2) 0.005(2) O5 0.048(3) 0.065(4) 0.081(4) 0.013(3) 0.017(3) -0.010(3) O6 0.043(3) 0.051(3) 0.065(3) -0.002(3) 0.008(3) 0.012(2) O7 0.054(3) 0.068(3) 0.051(3) -0.011(3) -0.017(3) 0.005(3) O8 0.028(2) 0.054(3) 0.051(3) 0.003(2) 0.003(2) 0.011(2) P1 0.0276(7) 0.0326(8) 0.0277(8) -0.0016(7) -0.0018(7) 0.0014(7) P2 0.0272(8) 0.0314(8) 0.0245(8) 0.0002(7) -0.0024(7) 0.0021(6) P3 0.0288(8) 0.0347(9) 0.0273(8) 0.0006(7) -0.0007(7) 0.0027(7) P4 0.0276(8) 0.0327(8) 0.0270(8) 0.0008(7) -0.0018(7) 0.0023(7) S1 0.0265(7) 0.0379(9) 0.0335(9) 0.0000(7) -0.0003(7) 0.0000(6) S2 0.0326(8) 0.0366(8) 0.0314(8) 0.0036(7) -0.0011(7) 0.0012(7) S3 0.0269(7) 0.0361(8) 0.0322(8) 0.0020(7) 0.0002(7) 0.0037(6) S4 0.0316(8) 0.0349(8) 0.0319(8) 0.0046(7) -0.0041(7) 0.0029(7) Cl1 0.0321(8) 0.0648(12) 0.0625(12) 0.0043(9) 0.0044(8) 0.0084(8) Cl2 0.0641(12) 0.0799(14) 0.0409(10) 0.0040(10) -0.0073(9) 0.0087(10) Cl3 0.0458(10) 0.0867(16) 0.0739(14) 0.0008(12) 0.0028(10) 0.0080(10) Cl4 0.0599(11) 0.0631(11) 0.0371(10) 0.0069(9) -0.0075(8) 0.0029(9) Fe1 0.0327(5) 0.0328(5) 0.0359(6) -0.0011(4) 0.0011(4) -0.0009(4) Fe2 0.0245(4) 0.0303(5) 0.0267(5) 0.0014(4) -0.0008(4) 0.0021(4) Fe3 0.0246(4) 0.0325(5) 0.0270(5) 0.0034(4) -0.0008(4) 0.0028(4) Fe4 0.0295(5) 0.0332(5) 0.0348(5) 0.0004(4) -0.0009(4) 0.0018(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.482(7) . ? C1 P1 1.850(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N1 1.471(8) . ? C2 P2 1.860(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N1 1.468(8) . ? C3 H3C 0.9800 . ? C3 H3B 0.9800 . ? C3 H3A 0.9800 . ? C4 C9 1.380(9) . ? C4 C5 1.407(9) . ? C4 P1 1.837(6) . ? C5 C6 1.412(9) . ? C5 H5A 0.9500 . ? C6 C7 1.349(10) . ? C6 H6A 0.9500 . ? C7 C8 1.375(11) . ? C7 H7A 0.9500 . ? C8 C9 1.407(9) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C10 C15 1.389(9) . ? C10 C11 1.394(9) . ? C10 P1 1.839(6) . ? C11 C12 1.398(9) . ? C11 H11A 0.9500 . ? C12 C13 1.380(10) . ? C12 H12A 0.9500 . ? C13 C14 1.386(11) . ? C13 H13A 0.9500 . ? C14 C15 1.394(10) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C21 1.391(9) . ? C16 C17 1.390(9) . ? C16 P2 1.844(7) . ? C17 C18 1.383(10) . ? C17 H17A 0.9500 . ? C18 C19 1.365(10) . ? C18 H18A 0.9500 . ? C19 C20 1.397(10) . ? C19 H19A 0.9500 . ? C20 C21 1.385(10) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.383(9) . ? C22 C27 1.416(9) . ? C22 P2 1.848(6) . ? C23 C24 1.398(9) . ? C23 H23A 0.9500 . ? C24 C25 1.394(10) . ? C24 H24A 0.9500 . ? C25 C26 1.376(10) . ? C25 H25A 0.9500 . ? C26 C27 1.395(9) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 O1 1.149(8) . ? C28 Fe1 1.801(8) . ? C29 O2 1.163(8) . ? C29 Fe1 1.777(8) . ? C30 O3 1.168(8) . ? C30 Fe1 1.783(8) . ? C31 O4 1.163(7) . ? C31 Fe2 1.755(7) . ? C32 C37 1.370(9) . ? C32 C33 1.415(8) . ? C32 S1 1.785(6) . ? C33 C34 1.383(9) . ? C33 S2 1.782(7) . ? C34 C35 1.389(10) . ? C34 Cl2 1.734(7) . ? C35 C36 1.381(10) . ? C35 H35A 0.9500 . ? C36 C37 1.407(10) . ? C36 H36A 0.9500 . ? C37 Cl1 1.770(7) . ? C38 N2 1.485(7) . ? C38 P3 1.843(6) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 N2 1.473(8) . ? C39 P4 1.849(6) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 N2 1.470(8) . ? C40 H40C 0.9800 . ? C40 H40B 0.9800 . ? C40 H40A 0.9800 . ? C41 C46 1.373(9) . ? C41 C42 1.395(9) . ? C41 P3 1.843(6) . ? C42 C43 1.382(10) . ? C42 H42A 0.9500 . ? C43 C44 1.368(11) . ? C43 H43A 0.9500 . ? C44 C45 1.372(10) . ? C44 H44A 0.9500 . ? C45 C46 1.393(9) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 C48 1.400(9) . ? C47 C52 1.408(8) . ? C47 P3 1.844(6) . ? C48 C49 1.376(9) . ? C48 H48A 0.9500 . ? C49 C50 1.395(10) . ? C49 H49A 0.9500 . ? C50 C51 1.368(10) . ? C50 H50A 0.9500 . ? C51 C52 1.397(9) . ? C51 H51A 0.9500 . ? C52 H52A 0.9500 . ? C53 C58 1.397(9) . ? C53 C54 1.406(9) . ? C53 P4 1.839(7) . ? C54 C55 1.383(10) . ? C54 H54A 0.9500 . ? C55 C56 1.388(11) . ? C55 H55A 0.9500 . ? C56 C57 1.397(11) . ? C56 H56A 0.9500 . ? C57 C58 1.384(10) . ? C57 H57A 0.9500 . ? C58 H58A 0.9500 . ? C59 C64 1.381(9) . ? C59 C60 1.424(9) . ? C59 P4 1.826(6) . ? C60 C61 1.385(9) . ? C60 H60A 0.9500 . ? C61 C62 1.356(11) . ? C61 H61A 0.9500 . ? C62 C63 1.387(10) . ? C62 H62A 0.9500 . ? C63 C64 1.411(9) . ? C63 H63A 0.9500 . ? C64 H64A 0.9500 . ? C65 O5 1.141(8) . ? C65 Fe4 1.823(8) . ? C66 O6 1.163(7) . ? C66 Fe4 1.777(7) . ? C67 O7 1.157(8) . ? C67 Fe4 1.785(7) . ? C68 O8 1.183(7) . ? C68 Fe3 1.737(6) . ? C69 C70 1.397(8) . ? C69 C74 1.415(9) . ? C69 S3 1.794(6) . ? C70 C71 1.395(9) . ? C70 S4 1.779(7) . ? C71 C72 1.395(10) . ? C71 Cl4 1.755(7) . ? C72 C73 1.371(10) . ? C72 H72A 0.9500 . ? C73 C74 1.388(10) . ? C73 H73A 0.9500 . ? C74 Cl3 1.692(7) . ? P1 Fe2 2.2185(18) . ? P2 Fe2 2.2157(17) . ? P3 Fe3 2.2234(18) . ? P4 Fe3 2.2141(18) . ? S1 Fe1 2.2921(18) . ? S1 Fe2 2.3060(17) . ? S2 Fe2 2.2921(18) . ? S2 Fe1 2.2928(18) . ? S3 Fe4 2.2865(18) . ? S3 Fe3 2.2885(17) . ? S4 Fe3 2.2895(18) . ? S4 Fe4 2.3006(17) . ? Fe1 Fe2 2.5311(13) . ? Fe3 Fe4 2.5357(13) . ? 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 N1 C1 P1 112.3(4) . . ? N1 C1 H1A 109.1 . . ? P1 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? P1 C1 H1B 109.1 . . ? H1A C1 H1B 107.9 . . ? N1 C2 P2 118.3(4) . . ? N1 C2 H2A 107.7 . . ? P2 C2 H2A 107.7 . . ? N1 C2 H2B 107.7 . . ? P2 C2 H2B 107.7 . . ? H2A C2 H2B 107.1 . . ? N1 C3 H3C 109.5 . . ? N1 C3 H3B 109.5 . . ? H3C C3 H3B 109.5 . . ? N1 C3 H3A 109.5 . . ? H3C C3 H3A 109.5 . . ? H3B C3 H3A 109.5 . . ? C9 C4 C5 118.2(6) . . ? C9 C4 P1 123.5(5) . . ? C5 C4 P1 118.2(5) . . ? C4 C5 C6 119.5(7) . . ? C4 C5 H5A 120.2 . . ? C6 C5 H5A 120.2 . . ? C7 C6 C5 121.4(7) . . ? C7 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? C6 C7 C8 119.7(7) . . ? C6 C7 H7A 120.2 . . ? C8 C7 H7A 120.2 . . ? C7 C8 C9 120.4(7) . . ? C7 C8 H8A 119.8 . . ? C9 C8 H8A 119.8 . . ? C4 C9 C8 120.7(6) . . ? C4 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C15 C10 C11 117.8(6) . . ? C15 C10 P1 120.6(5) . . ? C11 C10 P1 121.6(5) . . ? C10 C11 C12 120.9(6) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C13 C12 C11 120.1(7) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C12 C13 C14 120.1(7) . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C13 C14 C15 119.3(7) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? C10 C15 C14 121.8(7) . . ? C10 C15 H15A 119.1 . . ? C14 C15 H15A 119.1 . . ? C21 C16 C17 117.7(6) . . ? C21 C16 P2 121.1(5) . . ? C17 C16 P2 120.8(5) . . ? C18 C17 C16 120.6(7) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C19 C18 C17 121.5(7) . . ? C19 C18 H18A 119.3 . . ? C17 C18 H18A 119.3 . . ? C18 C19 C20 119.0(7) . . ? C18 C19 H19A 120.5 . . ? C20 C19 H19A 120.5 . . ? C21 C20 C19 119.5(7) . . ? C21 C20 H20A 120.2 . . ? C19 C20 H20A 120.2 . . ? C20 C21 C16 121.6(6) . . ? C20 C21 H21A 119.2 . . ? C16 C21 H21A 119.2 . . ? C23 C22 C27 119.3(6) . . ? C23 C22 P2 121.9(5) . . ? C27 C22 P2 118.8(5) . . ? C22 C23 C24 120.4(6) . . ? C22 C23 H23A 119.8 . . ? C24 C23 H23A 119.8 . . ? C25 C24 C23 120.3(7) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C26 C25 C24 119.6(6) . . ? C26 C25 H25A 120.2 . . ? C24 C25 H25A 120.2 . . ? C25 C26 C27 120.9(7) . . ? C25 C26 H26A 119.5 . . ? C27 C26 H26A 119.5 . . ? C26 C27 C22 119.5(6) . . ? C26 C27 H27A 120.3 . . ? C22 C27 H27A 120.3 . . ? O1 C28 Fe1 173.4(6) . . ? O2 C29 Fe1 177.3(7) . . ? O3 C30 Fe1 177.4(7) . . ? O4 C31 Fe2 179.0(6) . . ? C37 C32 C33 118.7(6) . . ? C37 C32 S1 125.0(5) . . ? C33 C32 S1 116.2(5) . . ? C34 C33 C32 119.7(6) . . ? C34 C33 S2 124.8(5) . . ? C32 C33 S2 115.3(5) . . ? C33 C34 C35 120.3(6) . . ? C33 C34 Cl2 120.5(6) . . ? C35 C34 Cl2 119.2(6) . . ? C36 C35 C34 121.1(7) . . ? C36 C35 H35A 119.5 . . ? C34 C35 H35A 119.5 . . ? C35 C36 C37 118.0(7) . . ? C35 C36 H36A 121.0 . . ? C37 C36 H36A 121.0 . . ? C32 C37 C36 122.2(6) . . ? C32 C37 Cl1 120.4(5) . . ? C36 C37 Cl1 117.4(5) . . ? N2 C38 P3 112.2(4) . . ? N2 C38 H38A 109.2 . . ? P3 C38 H38A 109.2 . . ? N2 C38 H38B 109.2 . . ? P3 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? N2 C39 P4 117.9(4) . . ? N2 C39 H39A 107.8 . . ? P4 C39 H39A 107.8 . . ? N2 C39 H39B 107.8 . . ? P4 C39 H39B 107.8 . . ? H39A C39 H39B 107.2 . . ? N2 C40 H40C 109.5 . . ? N2 C40 H40B 109.5 . . ? H40C C40 H40B 109.5 . . ? N2 C40 H40A 109.5 . . ? H40C C40 H40A 109.5 . . ? H40B C40 H40A 109.5 . . ? C46 C41 C42 118.2(6) . . ? C46 C41 P3 120.2(5) . . ? C42 C41 P3 121.5(5) . . ? C43 C42 C41 120.5(7) . . ? C43 C42 H42A 119.8 . . ? C41 C42 H42A 119.8 . . ? C44 C43 C42 120.5(7) . . ? C44 C43 H43A 119.8 . . ? C42 C43 H43A 119.8 . . ? C43 C44 C45 119.8(7) . . ? C43 C44 H44A 120.1 . . ? C45 C44 H44A 120.1 . . ? C44 C45 C46 119.8(7) . . ? C44 C45 H45A 120.1 . . ? C46 C45 H45A 120.1 . . ? C41 C46 C45 121.0(6) . . ? C41 C46 H46A 119.5 . . ? C45 C46 H46A 119.5 . . ? C48 C47 C52 118.0(6) . . ? C48 C47 P3 120.7(5) . . ? C52 C47 P3 121.3(5) . . ? C49 C48 C47 121.4(6) . . ? C49 C48 H48A 119.3 . . ? C47 C48 H48A 119.3 . . ? C48 C49 C50 119.8(7) . . ? C48 C49 H49A 120.1 . . ? C50 C49 H49A 120.1 . . ? C51 C50 C49 120.2(7) . . ? C51 C50 H50A 119.9 . . ? C49 C50 H50A 119.9 . . ? C50 C51 C52 120.5(6) . . ? C50 C51 H51A 119.7 . . ? C52 C51 H51A 119.7 . . ? C51 C52 C47 120.1(6) . . ? C51 C52 H52A 119.9 . . ? C47 C52 H52A 119.9 . . ? C58 C53 C54 117.7(6) . . ? C58 C53 P4 120.2(5) . . ? C54 C53 P4 122.0(5) . . ? C55 C54 C53 120.4(7) . . ? C55 C54 H54A 119.8 . . ? C53 C54 H54A 119.8 . . ? C54 C55 C56 121.3(7) . . ? C54 C55 H55A 119.3 . . ? C56 C55 H55A 119.3 . . ? C55 C56 C57 119.0(7) . . ? C55 C56 H56A 120.5 . . ? C57 C56 H56A 120.5 . . ? C58 C57 C56 119.6(7) . . ? C58 C57 H57A 120.2 . . ? C56 C57 H57A 120.2 . . ? C57 C58 C53 122.0(6) . . ? C57 C58 H58A 119.0 . . ? C53 C58 H58A 119.0 . . ? C64 C59 C60 118.2(6) . . ? C64 C59 P4 122.7(5) . . ? C60 C59 P4 119.0(5) . . ? C61 C60 C59 120.4(7) . . ? C61 C60 H60A 119.8 . . ? C59 C60 H60A 119.8 . . ? C62 C61 C60 120.4(7) . . ? C62 C61 H61A 119.8 . . ? C60 C61 H61A 119.8 . . ? C61 C62 C63 121.1(6) . . ? C61 C62 H62A 119.4 . . ? C63 C62 H62A 119.4 . . ? C62 C63 C64 119.1(7) . . ? C62 C63 H63A 120.4 . . ? C64 C63 H63A 120.4 . . ? C59 C64 C63 120.7(6) . . ? C59 C64 H64A 119.6 . . ? C63 C64 H64A 119.6 . . ? O5 C65 Fe4 179.7(7) . . ? O6 C66 Fe4 179.5(6) . . ? O7 C67 Fe4 177.7(6) . . ? O8 C68 Fe3 179.1(6) . . ? C70 C69 C74 120.1(6) . . ? C70 C69 S3 116.2(5) . . ? C74 C69 S3 123.7(5) . . ? C71 C70 C69 118.3(6) . . ? C71 C70 S4 125.8(5) . . ? C69 C70 S4 115.8(5) . . ? C72 C71 C70 121.9(6) . . ? C72 C71 Cl4 119.1(5) . . ? C70 C71 Cl4 119.0(5) . . ? C73 C72 C71 118.9(7) . . ? C73 C72 H72A 120.6 . . ? C71 C72 H72A 120.6 . . ? C72 C73 C74 121.5(7) . . ? C72 C73 H73A 119.3 . . ? C74 C73 H73A 119.3 . . ? C73 C74 C69 119.3(6) . . ? C73 C74 Cl3 119.6(6) . . ? C69 C74 Cl3 121.1(5) . . ? C3 N1 C2 109.3(5) . . ? C3 N1 C1 109.4(4) . . ? C2 N1 C1 112.1(5) . . ? C40 N2 C39 109.9(5) . . ? C40 N2 C38 108.6(5) . . ? C39 N2 C38 112.8(5) . . ? C4 P1 C10 102.9(3) . . ? C4 P1 C1 100.9(3) . . ? C10 P1 C1 101.3(3) . . ? C4 P1 Fe2 114.0(2) . . ? C10 P1 Fe2 124.0(2) . . ? C1 P1 Fe2 110.8(2) . . ? C16 P2 C22 103.5(3) . . ? C16 P2 C2 95.8(3) . . ? C22 P2 C2 104.6(3) . . ? C16 P2 Fe2 121.3(2) . . ? C22 P2 Fe2 115.6(2) . . ? C2 P2 Fe2 113.19(19) . . ? C38 P3 C41 101.7(3) . . ? C38 P3 C47 99.9(3) . . ? C41 P3 C47 101.2(3) . . ? C38 P3 Fe3 111.1(2) . . ? C41 P3 Fe3 115.7(2) . . ? C47 P3 Fe3 124.0(2) . . ? C59 P4 C53 101.4(3) . . ? C59 P4 C39 105.2(3) . . ? C53 P4 C39 97.4(3) . . ? C59 P4 Fe3 116.0(2) . . ? C53 P4 Fe3 120.6(2) . . ? C39 P4 Fe3 113.73(19) . . ? C32 S1 Fe1 101.6(2) . . ? C32 S1 Fe2 100.3(2) . . ? Fe1 S1 Fe2 66.80(5) . . ? C33 S2 Fe2 101.4(2) . . ? C33 S2 Fe1 101.7(2) . . ? Fe2 S2 Fe1 67.02(5) . . ? C69 S3 Fe4 99.4(2) . . ? C69 S3 Fe3 101.9(2) . . ? Fe4 S3 Fe3 67.32(5) . . ? C70 S4 Fe3 103.1(2) . . ? C70 S4 Fe4 99.0(2) . . ? Fe3 S4 Fe4 67.07(5) . . ? C29 Fe1 C30 93.7(3) . . ? C29 Fe1 C28 98.4(3) . . ? C30 Fe1 C28 98.0(3) . . ? C29 Fe1 S1 154.6(2) . . ? C30 Fe1 S1 89.3(2) . . ? C28 Fe1 S1 106.2(2) . . ? C29 Fe1 S2 87.8(2) . . ? C30 Fe1 S2 158.4(2) . . ? C28 Fe1 S2 103.1(2) . . ? S1 Fe1 S2 80.55(6) . . ? C29 Fe1 Fe2 97.9(2) . . ? C30 Fe1 Fe2 102.1(2) . . ? C28 Fe1 Fe2 153.2(2) . . ? S1 Fe1 Fe2 56.86(5) . . ? S2 Fe1 Fe2 56.48(5) . . ? C31 Fe2 P2 89.6(2) . . ? C31 Fe2 P1 93.7(2) . . ? P2 Fe2 P1 90.57(6) . . ? C31 Fe2 S2 89.8(2) . . ? P2 Fe2 S2 168.38(7) . . ? P1 Fe2 S2 101.05(7) . . ? C31 Fe2 S1 156.7(2) . . ? P2 Fe2 S1 95.90(6) . . ? P1 Fe2 S1 108.77(7) . . ? S2 Fe2 S1 80.28(6) . . ? C31 Fe2 Fe1 100.7(2) . . ? P2 Fe2 Fe1 112.26(5) . . ? P1 Fe2 Fe1 152.83(6) . . ? S2 Fe2 Fe1 56.51(5) . . ? S1 Fe2 Fe1 56.34(5) . . ? C68 Fe3 P4 88.7(2) . . ? C68 Fe3 P3 92.1(2) . . ? P4 Fe3 P3 91.58(7) . . ? C68 Fe3 S3 159.8(2) . . ? P4 Fe3 S3 94.53(6) . . ? P3 Fe3 S3 107.77(7) . . ? C68 Fe3 S4 91.2(2) . . ? P4 Fe3 S4 165.08(7) . . ? P3 Fe3 S4 103.33(7) . . ? S3 Fe3 S4 80.65(6) . . ? C68 Fe3 Fe4 103.8(2) . . ? P4 Fe3 Fe4 108.94(6) . . ? P3 Fe3 Fe4 154.04(6) . . ? S3 Fe3 Fe4 56.30(5) . . ? S4 Fe3 Fe4 56.68(5) . . ? C66 Fe4 C67 89.8(3) . . ? C66 Fe4 C65 104.0(3) . . ? C67 Fe4 C65 96.3(3) . . ? C66 Fe4 S3 152.3(2) . . ? C67 Fe4 S3 92.6(2) . . ? C65 Fe4 S3 103.2(2) . . ? C66 Fe4 S4 89.6(2) . . ? C67 Fe4 S4 163.4(2) . . ? C65 Fe4 S4 99.9(2) . . ? S3 Fe4 S4 80.45(6) . . ? C66 Fe4 Fe3 96.6(2) . . ? C67 Fe4 Fe3 107.4(2) . . ? C65 Fe4 Fe3 148.5(2) . . ? S3 Fe4 Fe3 56.38(5) . . ? S4 Fe4 Fe3 56.26(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.544 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.085