Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Sascha Ott' _publ_contact_author_address ; Dept of Photochemistry and Molecular Science Uppsala University Box 579 Uppsala 75123 SWEDEN ; _publ_contact_author_email SASCHA.OTT@FOTOMOL.UU.SE _publ_section_title ; Bio-Inspired, Side-on Attachment of a Ruthenium Photosensitizer to an Iron Hydrogenase Active Site Model ; _publ_section_references ; Bergerhoff, G. (1996). DIAMOND - Visual Crystal Structure Information System Gerhard-Domagk-str. 1, 53121 Bonn, Germany Oxford Diffraction. (2003). Oxford Diffraction Ltd., Xcalibur CCD system, CrysAlis Software system, Version 1.170 Sheldrick, G.M. (1990). Acta Cryst. A46, 467-473 Sheldrick, G.M. (1997). SHELXL-97, University of Gottingen, Germany. Stoe. (1997). X-RED Data reduction program, version 1.09, X-SHAPE Crystal Optimisation for Numerical Absorption Correction, version 1.2, Stoe & CIE GmbH, Hilpertstrase 10, D-64295 Darmstadt, Germany ; loop_ _publ_author_name 'Sascha Ott' 'Maria Abrahamsson' 'Bjorn Akermark' 'Hans-Christian Becker' 'Jonas Bergquist' ; J.Ekstrom ; 'Lars Eriksson' 'Leif Hammarstrom' 'Filiz B. Kaynak' 'Carol Olson' 'Licheng Sun' data_run1 _database_code_depnum_ccdc_archive 'CCDC 607112' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H42 Br2 Fe2 O5 P2 S2' _chemical_formula_weight 1084.39 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' Br Br -0.2901 2.4595 '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' 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' O O 0.0106 0.0060 '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' 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 9.3219(9) _cell_length_b 22.8707(16) _cell_length_c 22.4947(17) _cell_angle_alpha 90.00 _cell_angle_beta 96.750(7) _cell_angle_gamma 90.00 _cell_volume 4762.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 32469 _cell_measurement_theta_min 3.68 _cell_measurement_theta_max 33.38 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 2.485 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.41 _exptl_absorpt_correction_T_max 0.88 _exptl_absorpt_process_details 'X-RED (Stoe, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Xcalibur-3 kappa-diffractometer with Sapphire-III CCD' _diffrn_measurement_method '\w scans at different \f' _diffrn_detector_area_resol_mean 12 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% . _diffrn_reflns_number 32469 _diffrn_reflns_av_R_equivalents 0.1008 _diffrn_reflns_av_sigmaI/netI 0.3943 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 33.38 _reflns_number_total 14784 _reflns_number_gt 3150 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlis CCD(Oxford Diffraction, 2003)' _computing_cell_refinement 'CrysAlis RED(Oxford Diffraction, 2003)' _computing_data_reduction 'CrysAlis RED(Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Bergerhoff, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0792P)^2^] 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 14784 _refine_ls_number_parameters 518 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.3178 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.2224 _refine_ls_wR_factor_gt 0.1624 _refine_ls_goodness_of_fit_ref 0.745 _refine_ls_restrained_S_all 0.746 _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 0.81134(12) 0.13799(5) 0.37537(4) 0.0387(3) Uani 1 1 d . . . Fe2 Fe 0.89556(11) 0.11324(4) 0.27607(4) 0.0367(3) Uani 1 1 d . . . S1 S 0.8282(2) 0.20469(8) 0.30138(8) 0.0427(5) Uani 1 1 d . . . C11 C 0.5347(8) 0.1298(4) 0.2579(3) 0.053(2) Uani 1 1 d . . . H11A H 0.5500 0.1269 0.2161 0.064 Uiso 1 1 calc R . . H11B H 0.4426 0.1115 0.2622 0.064 Uiso 1 1 calc R . . C12 C 0.5244(9) 0.1939(4) 0.2737(3) 0.060(2) Uani 1 1 d . . . H12A H 0.4394 0.2103 0.2506 0.072 Uiso 1 1 calc R . . H12B H 0.5111 0.1971 0.3157 0.072 Uiso 1 1 calc R . . C13 C 0.6532(9) 0.2298(4) 0.2625(3) 0.055(2) Uani 1 1 d . . . H13A H 0.6372 0.2697 0.2746 0.066 Uiso 1 1 calc R . . H13B H 0.6598 0.2301 0.2198 0.066 Uiso 1 1 calc R . . S2 S 0.6750(2) 0.08828(9) 0.30164(9) 0.0452(5) Uani 1 1 d . . . C1 C 0.8574(9) 0.0693(4) 0.4083(4) 0.049(2) Uani 1 1 d . . . O1 O 0.8899(7) 0.0239(3) 0.4264(3) 0.0722(19) Uani 1 1 d . . . C2 C 1.0743(9) 0.1393(3) 0.2838(3) 0.042(2) Uani 1 1 d . . . O2 O 1.1891(7) 0.1599(3) 0.2921(3) 0.0756(19) Uani 1 1 d . . . C3 C 0.9516(9) 0.0430(4) 0.2902(3) 0.048(2) Uani 1 1 d . . . O3 O 0.9922(7) -0.0053(3) 0.3000(3) 0.078(2) Uani 1 1 d . . . C4 C 0.9673(10) 0.1720(4) 0.4115(4) 0.055(2) Uani 1 1 d . . . O4 O 1.0676(8) 0.1948(3) 0.4343(3) 0.081(2) Uani 1 1 d . . . P1 P 0.6668(2) 0.16629(9) 0.44375(8) 0.0414(5) Uani 1 1 d . . . C21 C 0.7616(9) 0.1727(4) 0.5205(3) 0.046(2) Uani 1 1 d . . . C22 C 0.7372(10) 0.2187(4) 0.5583(4) 0.063(3) Uani 1 1 d . . . H22 H 0.6732 0.2483 0.5446 0.075 Uiso 1 1 calc R . . C23 C 0.8057(13) 0.2212(5) 0.6154(5) 0.091(4) Uani 1 1 d . . . H23 H 0.7922 0.2532 0.6396 0.109 Uiso 1 1 calc R . . C24 C 0.8907(12) 0.1782(6) 0.6359(4) 0.076(3) Uani 1 1 d . . . H24 H 0.9306 0.1785 0.6757 0.092 Uiso 1 1 calc R . . C25 C 0.9217(11) 0.1331(5) 0.5999(5) 0.085(3) Uani 1 1 d . . . H25 H 0.9894 0.1050 0.6142 0.103 Uiso 1 1 calc R . . C26 C 0.8535(11) 0.1291(4) 0.5430(4) 0.065(3) Uani 1 1 d . . . H26 H 0.8692 0.0968 0.5194 0.079 Uiso 1 1 calc R . . C31 C 0.5138(9) 0.1185(3) 0.4554(3) 0.044(2) Uani 1 1 d . . . C32 C 0.4190(10) 0.1013(4) 0.4081(4) 0.067(3) Uani 1 1 d . . . H32 H 0.4349 0.1130 0.3699 0.081 Uiso 1 1 calc R . . C33 C 0.2995(10) 0.0668(4) 0.4147(4) 0.070(3) Uani 1 1 d . . . H33 H 0.2350 0.0574 0.3814 0.084 Uiso 1 1 calc R . . C34 C 0.2766(11) 0.0472(4) 0.4685(5) 0.077(3) Uani 1 1 d . . . H34 H 0.1982 0.0232 0.4732 0.092 Uiso 1 1 calc R . . C35 C 0.3743(14) 0.0638(5) 0.5182(5) 0.108(4) Uani 1 1 d . . . H35 H 0.3580 0.0507 0.5560 0.130 Uiso 1 1 calc R . . C36 C 0.4937(11) 0.0988(4) 0.5133(4) 0.080(3) Uani 1 1 d . . . H36 H 0.5576 0.1089 0.5466 0.096 Uiso 1 1 calc R . . C41 C 0.5822(9) 0.2374(3) 0.4336(3) 0.0415(19) Uani 1 1 d . . . C42 C 0.6610(9) 0.2829(4) 0.4131(3) 0.054(2) Uani 1 1 d . . . H42 H 0.7526 0.2755 0.4024 0.065 Uiso 1 1 calc R . . C43 C 0.6061(11) 0.3390(4) 0.4082(4) 0.068(3) Uani 1 1 d . . . H43 H 0.6623 0.3691 0.3957 0.081 Uiso 1 1 calc R . . C44 C 0.4658(10) 0.3507(3) 0.4221(3) 0.053(2) Uani 1 1 d . . . C45 C 0.3891(10) 0.3062(4) 0.4423(4) 0.062(2) Uani 1 1 d . . . H45 H 0.2974 0.3135 0.4530 0.075 Uiso 1 1 calc R . . C46 C 0.4437(10) 0.2508(4) 0.4473(4) 0.058(2) Uani 1 1 d . . . H46 H 0.3868 0.2210 0.4602 0.069 Uiso 1 1 calc R . . Br1 Br 0.39769(13) 0.42799(5) 0.41613(6) 0.1007(4) Uani 1 1 d . . . P2 P 0.8796(2) 0.10742(8) 0.17579(8) 0.0369(5) Uani 1 1 d . . . C51 C 0.8158(9) 0.1734(3) 0.1353(3) 0.0384(19) Uani 1 1 d . . . C52 C 0.6865(10) 0.1757(4) 0.0973(3) 0.050(2) Uani 1 1 d . . . H52 H 0.6284 0.1426 0.0921 0.060 Uiso 1 1 calc R . . C53 C 0.6446(10) 0.2263(4) 0.0677(4) 0.059(2) Uani 1 1 d . . . H53 H 0.5589 0.2279 0.0421 0.071 Uiso 1 1 calc R . . C54 C 0.7322(13) 0.2750(4) 0.0768(4) 0.070(3) Uani 1 1 d . . . H54 H 0.7047 0.3093 0.0564 0.084 Uiso 1 1 calc R . . C55 C 0.8591(11) 0.2743(4) 0.1150(4) 0.055(2) Uani 1 1 d . . . H55 H 0.9173 0.3074 0.1205 0.066 Uiso 1 1 calc R . . C56 C 0.8957(8) 0.2238(3) 0.1444(3) 0.0397(19) Uani 1 1 d . . . H56 H 0.9785 0.2232 0.1718 0.048 Uiso 1 1 calc R . . C61 C 1.0574(8) 0.0956(3) 0.1474(3) 0.0383(19) Uani 1 1 d . . . C62 C 1.0954(9) 0.1220(4) 0.0974(4) 0.062(3) Uani 1 1 d . . . H62 H 1.0316 0.1478 0.0761 0.075 Uiso 1 1 calc R . . C63 C 1.2280(11) 0.1109(4) 0.0782(4) 0.071(3) Uani 1 1 d . . . H63 H 1.2547 0.1301 0.0447 0.085 Uiso 1 1 calc R . . C64 C 1.3203(9) 0.0715(3) 0.1084(4) 0.046(2) Uani 1 1 d . . . H64 H 1.4097 0.0638 0.0955 0.055 Uiso 1 1 calc R . . C65 C 1.2814(9) 0.0443(4) 0.1563(3) 0.054(2) Uani 1 1 d . . . H65 H 1.3438 0.0175 0.1768 0.064 Uiso 1 1 calc R . . C66 C 1.1509(9) 0.0554(4) 0.1753(3) 0.049(2) Uani 1 1 d . . . H66 H 1.1246 0.0352 0.2082 0.058 Uiso 1 1 calc R . . C71 C 0.7742(8) 0.0476(3) 0.1390(3) 0.0352(18) Uani 1 1 d . . . C72 C 0.6937(8) 0.0100(3) 0.1699(3) 0.042(2) Uani 1 1 d . . . H72 H 0.6934 0.0156 0.2109 0.050 Uiso 1 1 calc R . . C73 C 0.6141(9) -0.0352(3) 0.1427(3) 0.048(2) Uani 1 1 d . . . H73 H 0.5587 -0.0592 0.1643 0.058 Uiso 1 1 calc R . . C74 C 0.6188(8) -0.0438(3) 0.0827(4) 0.048(2) Uani 1 1 d . . . C75 C 0.6936(9) -0.0074(4) 0.0490(3) 0.056(2) Uani 1 1 d . . . H75 H 0.6911 -0.0132 0.0080 0.067 Uiso 1 1 calc R . . C76 C 0.7737(9) 0.0387(3) 0.0771(3) 0.053(2) Uani 1 1 d . . . H76 H 0.8265 0.0633 0.0550 0.064 Uiso 1 1 calc R . . Br2 Br 0.51092(10) -0.10808(4) 0.04482(4) 0.0652(3) Uani 1 1 d . . . C81 C 0.6249(18) 0.9001(7) 0.2935(8) 0.189(7) Uiso 1 1 d D . . H81A H 0.6732 0.8822 0.3295 0.227 Uiso 1 1 calc R . . H81B H 0.6925 0.9220 0.2725 0.227 Uiso 1 1 calc R . . C82 C 0.4735(14) 0.9380(6) 0.3045(6) 0.143(5) Uiso 1 1 d D . . H82A H 0.4660 0.9397 0.3471 0.172 Uiso 1 1 calc R . . H82B H 0.4830 0.9777 0.2905 0.172 Uiso 1 1 calc R . . C83 C 0.3222(17) 0.9093(6) 0.2700(7) 0.177(6) Uiso 1 1 d D . . H83A H 0.2745 0.9391 0.2440 0.212 Uiso 1 1 calc R . . H83B H 0.2592 0.9003 0.3001 0.212 Uiso 1 1 calc R . . C84 C 0.3382(18) 0.8453(7) 0.2262(7) 0.186(7) Uiso 1 1 d D . . H84A H 0.2947 0.8105 0.2411 0.224 Uiso 1 1 calc R . . H84B H 0.3109 0.8504 0.1836 0.224 Uiso 1 1 calc R . . O85 O 0.5183(13) 0.8530(5) 0.2489(5) 0.198(5) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0358(7) 0.0493(7) 0.0325(6) -0.0021(5) 0.0099(5) -0.0028(6) Fe2 0.0312(7) 0.0477(7) 0.0324(6) -0.0005(5) 0.0092(5) 0.0013(5) S1 0.0426(13) 0.0462(12) 0.0407(12) 0.0008(9) 0.0109(10) -0.0008(10) C11 0.034(5) 0.090(7) 0.037(5) -0.011(4) 0.007(4) -0.002(5) C12 0.043(6) 0.097(7) 0.040(5) 0.000(5) 0.008(4) 0.017(5) C13 0.056(6) 0.065(6) 0.047(5) -0.003(4) 0.013(4) 0.021(5) S2 0.0395(13) 0.0566(13) 0.0406(12) -0.0062(9) 0.0101(10) -0.0091(10) C1 0.055(6) 0.050(6) 0.047(5) -0.021(4) 0.025(4) -0.010(5) O1 0.101(6) 0.053(4) 0.066(4) 0.009(3) 0.023(4) 0.008(4) C2 0.031(5) 0.059(5) 0.036(5) -0.011(4) 0.007(4) 0.000(4) O2 0.039(4) 0.103(5) 0.085(5) -0.016(4) 0.009(3) -0.016(4) C3 0.037(5) 0.073(6) 0.037(5) 0.005(4) 0.017(4) 0.007(5) O3 0.093(5) 0.079(5) 0.070(4) 0.024(4) 0.036(4) 0.020(4) C4 0.047(6) 0.075(7) 0.045(6) -0.002(5) 0.011(5) -0.004(5) O4 0.069(5) 0.114(6) 0.060(4) -0.011(4) 0.001(4) -0.028(4) P1 0.0393(14) 0.0507(13) 0.0359(12) -0.0027(9) 0.0119(10) -0.0041(11) C21 0.048(6) 0.061(6) 0.031(4) -0.003(4) 0.017(4) -0.002(5) C22 0.058(7) 0.077(7) 0.052(6) -0.009(5) 0.003(5) 0.004(5) C23 0.104(10) 0.105(9) 0.057(7) -0.030(6) -0.020(7) 0.009(8) C24 0.072(8) 0.133(10) 0.022(5) -0.008(6) -0.001(5) -0.010(7) C25 0.085(9) 0.117(9) 0.053(7) 0.035(6) 0.001(6) 0.010(7) C26 0.098(8) 0.071(7) 0.026(5) -0.003(4) 0.004(5) 0.026(6) C31 0.046(6) 0.048(5) 0.037(5) 0.003(4) 0.001(4) -0.009(4) C32 0.057(7) 0.097(8) 0.050(6) 0.001(5) 0.015(5) -0.021(6) C33 0.053(7) 0.097(8) 0.060(7) -0.007(5) 0.007(5) -0.032(6) C34 0.048(7) 0.081(7) 0.104(9) 0.001(7) 0.020(6) -0.018(5) C35 0.143(12) 0.102(9) 0.082(9) 0.037(6) 0.018(8) -0.064(9) C36 0.089(8) 0.099(8) 0.051(6) 0.014(5) 0.005(5) -0.051(7) C41 0.041(5) 0.048(5) 0.036(4) 0.001(4) 0.006(4) -0.002(4) C42 0.059(6) 0.053(6) 0.054(6) -0.002(4) 0.021(4) 0.013(5) C43 0.074(8) 0.064(7) 0.070(6) -0.015(5) 0.028(5) -0.021(6) C44 0.066(7) 0.046(5) 0.049(5) -0.004(4) 0.016(5) 0.009(5) C45 0.050(6) 0.070(7) 0.071(6) 0.012(5) 0.028(5) 0.008(5) C46 0.060(6) 0.047(6) 0.071(6) 0.021(4) 0.027(5) 0.004(5) Br1 0.1003(10) 0.0688(8) 0.1372(11) 0.0151(7) 0.0314(8) 0.0201(7) P2 0.0363(13) 0.0441(12) 0.0320(11) -0.0014(9) 0.0107(9) 0.0003(10) C51 0.033(5) 0.051(5) 0.033(4) -0.011(4) 0.013(4) 0.003(4) C52 0.056(6) 0.048(6) 0.045(5) -0.009(4) 0.005(5) 0.001(5) C53 0.042(6) 0.071(7) 0.064(6) -0.004(5) 0.002(5) 0.023(5) C54 0.109(9) 0.048(6) 0.054(6) 0.016(5) 0.017(6) 0.022(6) C55 0.069(7) 0.049(6) 0.047(5) -0.007(4) 0.007(5) 0.001(5) C56 0.045(5) 0.037(5) 0.035(4) 0.000(4) 0.000(4) 0.005(4) C61 0.027(5) 0.056(5) 0.034(4) 0.006(4) 0.014(4) 0.002(4) C62 0.055(6) 0.076(7) 0.061(6) 0.020(5) 0.029(5) 0.035(5) C63 0.094(8) 0.061(6) 0.067(6) 0.009(5) 0.050(6) 0.004(6) C64 0.034(5) 0.052(5) 0.053(5) -0.014(4) 0.008(4) 0.001(4) C65 0.042(6) 0.080(6) 0.039(5) 0.004(4) 0.010(4) 0.012(5) C66 0.041(5) 0.062(6) 0.046(5) 0.002(4) 0.021(4) -0.003(5) C71 0.035(5) 0.033(4) 0.039(4) -0.001(3) 0.010(4) 0.006(4) C72 0.053(6) 0.044(5) 0.030(4) -0.001(4) 0.015(4) -0.007(4) C73 0.055(6) 0.051(5) 0.041(5) 0.003(4) 0.012(4) -0.015(4) C74 0.039(5) 0.040(5) 0.066(6) -0.004(4) 0.010(4) 0.001(4) C75 0.057(6) 0.075(6) 0.035(5) -0.025(4) 0.007(4) -0.004(5) C76 0.075(7) 0.048(5) 0.041(5) -0.011(4) 0.021(4) -0.006(5) Br2 0.0578(7) 0.0719(7) 0.0658(6) -0.0195(5) 0.0074(5) -0.0156(5) _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 C4 1.761(10) . ? Fe1 C1 1.768(10) . ? Fe1 P1 2.256(2) . ? Fe1 S2 2.273(2) . ? Fe1 S1 2.277(2) . ? Fe1 Fe2 2.5177(14) . ? Fe2 C3 1.708(9) . ? Fe2 C2 1.759(9) . ? Fe2 P2 2.247(2) . ? Fe2 S2 2.272(2) . ? Fe2 S1 2.275(2) . ? S1 C13 1.850(8) . ? C11 C12 1.514(11) . ? C11 S2 1.809(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.499(11) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C1 O1 1.144(9) . ? C2 O2 1.164(8) . ? C3 O3 1.180(8) . ? C4 O4 1.138(9) . ? P1 C41 1.810(8) . ? P1 C31 1.840(8) . ? P1 C21 1.851(8) . ? C21 C26 1.373(11) . ? C21 C22 1.388(10) . ? C22 C23 1.366(11) . ? C22 H22 0.9300 . ? C23 C24 1.313(13) . ? C23 H23 0.9300 . ? C24 C25 1.362(13) . ? C24 H24 0.9300 . ? C25 C26 1.364(11) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C32 1.360(10) . ? C31 C36 1.410(10) . ? C32 C33 1.386(11) . ? C32 H32 0.9300 . ? C33 C34 1.331(12) . ? C33 H33 0.9300 . ? C34 C35 1.408(13) . ? C34 H34 0.9300 . ? C35 C36 1.385(13) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C41 C42 1.383(10) . ? C41 C46 1.395(10) . ? C42 C43 1.381(11) . ? C42 H42 0.9300 . ? C43 C44 1.406(11) . ? C43 H43 0.9300 . ? C44 C45 1.353(11) . ? C44 Br1 1.877(8) . ? C45 C46 1.366(11) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? P2 C71 1.825(7) . ? P2 C51 1.826(8) . ? P2 C61 1.864(7) . ? C51 C56 1.375(9) . ? C51 C52 1.394(10) . ? C52 C53 1.371(10) . ? C52 H52 0.9300 . ? C53 C54 1.381(12) . ? C53 H53 0.9300 . ? C54 C55 1.379(12) . ? C54 H54 0.9300 . ? C55 C56 1.355(10) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C61 C62 1.359(10) . ? C61 C66 1.367(10) . ? C62 C63 1.381(11) . ? C62 H62 0.9300 . ? C63 C64 1.370(11) . ? C63 H63 0.9300 . ? C64 C65 1.330(10) . ? C64 H64 0.9300 . ? C65 C66 1.361(10) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C71 C72 1.380(9) . ? C71 C76 1.407(9) . ? C72 C73 1.375(9) . ? C72 H72 0.9300 . ? C73 C74 1.369(10) . ? C73 H73 0.9300 . ? C74 C75 1.369(10) . ? C74 Br2 1.923(8) . ? C75 C76 1.398(10) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? C81 C82 1.699(15) . ? C81 O85 1.709(15) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C82 C83 1.663(14) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 C84 1.781(15) . ? C83 H83A 0.9700 . ? C83 H83B 0.9700 . ? C84 O85 1.706(16) . ? C84 H84A 0.9700 . ? C84 H84B 0.9700 . ? 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 C4 Fe1 C1 93.0(4) . . ? C4 Fe1 P1 94.9(3) . . ? C1 Fe1 P1 96.0(2) . . ? C4 Fe1 S2 156.7(3) . . ? C1 Fe1 S2 87.0(3) . . ? P1 Fe1 S2 108.27(8) . . ? C4 Fe1 S1 85.3(3) . . ? C1 Fe1 S1 150.1(2) . . ? P1 Fe1 S1 113.85(8) . . ? S2 Fe1 S1 83.24(8) . . ? C4 Fe1 Fe2 100.5(3) . . ? C1 Fe1 Fe2 94.9(2) . . ? P1 Fe1 Fe2 160.58(8) . . ? S2 Fe1 Fe2 56.35(6) . . ? S1 Fe1 Fe2 56.39(6) . . ? C3 Fe2 C2 92.0(4) . . ? C3 Fe2 P2 96.6(3) . . ? C2 Fe2 P2 94.0(2) . . ? C3 Fe2 S2 89.0(3) . . ? C2 Fe2 S2 159.3(2) . . ? P2 Fe2 S2 106.50(8) . . ? C3 Fe2 S1 154.9(3) . . ? C2 Fe2 S1 87.1(2) . . ? P2 Fe2 S1 108.54(8) . . ? S2 Fe2 S1 83.28(8) . . ? C3 Fe2 Fe1 99.6(2) . . ? C2 Fe2 Fe1 103.1(2) . . ? P2 Fe2 Fe1 155.95(7) . . ? S2 Fe2 Fe1 56.36(6) . . ? S1 Fe2 Fe1 56.45(6) . . ? C13 S1 Fe2 114.9(3) . . ? C13 S1 Fe1 114.9(3) . . ? Fe2 S1 Fe1 67.16(6) . . ? C12 C11 S2 116.3(5) . . ? C12 C11 H11A 108.2 . . ? S2 C11 H11A 108.2 . . ? C12 C11 H11B 108.2 . . ? S2 C11 H11B 108.2 . . ? H11A C11 H11B 107.4 . . ? C13 C12 C11 114.6(7) . . ? C13 C12 H12A 108.6 . . ? C11 C12 H12A 108.6 . . ? C13 C12 H12B 108.6 . . ? C11 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? C12 C13 S1 115.5(6) . . ? C12 C13 H13A 108.4 . . ? S1 C13 H13A 108.4 . . ? C12 C13 H13B 108.4 . . ? S1 C13 H13B 108.4 . . ? H13A C13 H13B 107.5 . . ? C11 S2 Fe2 110.4(3) . . ? C11 S2 Fe1 116.1(3) . . ? Fe2 S2 Fe1 67.28(7) . . ? O1 C1 Fe1 176.0(7) . . ? O2 C2 Fe2 174.4(7) . . ? O3 C3 Fe2 179.1(8) . . ? O4 C4 Fe1 178.8(9) . . ? C41 P1 C31 102.6(4) . . ? C41 P1 C21 101.5(4) . . ? C31 P1 C21 101.9(3) . . ? C41 P1 Fe1 117.3(3) . . ? C31 P1 Fe1 117.5(3) . . ? C21 P1 Fe1 113.6(3) . . ? C26 C21 C22 117.7(8) . . ? C26 C21 P1 119.7(6) . . ? C22 C21 P1 122.5(7) . . ? C23 C22 C21 121.0(9) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C24 C23 C22 119.6(10) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 121.4(9) . . ? C23 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? C24 C25 C26 120.0(10) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C21 119.9(9) . . ? C25 C26 H26 120.0 . . ? C21 C26 H26 120.0 . . ? C32 C31 C36 119.0(8) . . ? C32 C31 P1 120.2(6) . . ? C36 C31 P1 120.7(6) . . ? C31 C32 C33 122.5(8) . . ? C31 C32 H32 118.8 . . ? C33 C32 H32 118.8 . . ? C34 C33 C32 120.4(9) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 118.2(9) . . ? C33 C34 H34 120.9 . . ? C35 C34 H34 120.9 . . ? C36 C35 C34 122.9(9) . . ? C36 C35 H35 118.6 . . ? C34 C35 H35 118.6 . . ? C35 C36 C31 117.0(9) . . ? C35 C36 H36 121.5 . . ? C31 C36 H36 121.5 . . ? C42 C41 C46 116.7(7) . . ? C42 C41 P1 118.5(6) . . ? C46 C41 P1 124.7(6) . . ? C43 C42 C41 121.3(8) . . ? C43 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? C42 C43 C44 120.4(8) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C45 C44 C43 118.2(8) . . ? C45 C44 Br1 123.0(7) . . ? C43 C44 Br1 118.7(7) . . ? C44 C45 C46 121.3(8) . . ? C44 C45 H45 119.3 . . ? C46 C45 H45 119.3 . . ? C45 C46 C41 122.1(8) . . ? C45 C46 H46 119.0 . . ? C41 C46 H46 119.0 . . ? C71 P2 C51 105.5(3) . . ? C71 P2 C61 100.9(3) . . ? C51 P2 C61 101.5(3) . . ? C71 P2 Fe2 117.9(2) . . ? C51 P2 Fe2 115.5(2) . . ? C61 P2 Fe2 113.3(2) . . ? C56 C51 C52 118.3(7) . . ? C56 C51 P2 118.7(6) . . ? C52 C51 P2 123.0(6) . . ? C53 C52 C51 120.4(8) . . ? C53 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C52 C53 C54 118.7(8) . . ? C52 C53 H53 120.7 . . ? C54 C53 H53 120.7 . . ? C55 C54 C53 122.2(8) . . ? C55 C54 H54 118.9 . . ? C53 C54 H54 118.9 . . ? C56 C55 C54 117.5(8) . . ? C56 C55 H55 121.2 . . ? C54 C55 H55 121.2 . . ? C55 C56 C51 122.8(8) . . ? C55 C56 H56 118.6 . . ? C51 C56 H56 118.6 . . ? C62 C61 C66 117.6(7) . . ? C62 C61 P2 123.2(6) . . ? C66 C61 P2 119.0(5) . . ? C61 C62 C63 120.5(8) . . ? C61 C62 H62 119.7 . . ? C63 C62 H62 119.7 . . ? C64 C63 C62 119.9(8) . . ? C64 C63 H63 120.1 . . ? C62 C63 H63 120.1 . . ? C65 C64 C63 119.6(8) . . ? C65 C64 H64 120.2 . . ? C63 C64 H64 120.2 . . ? C64 C65 C66 120.4(8) . . ? C64 C65 H65 119.8 . . ? C66 C65 H65 119.8 . . ? C65 C66 C61 121.8(7) . . ? C65 C66 H66 119.1 . . ? C61 C66 H66 119.1 . . ? C72 C71 C76 118.0(7) . . ? C72 C71 P2 122.2(5) . . ? C76 C71 P2 119.8(6) . . ? C73 C72 C71 122.7(7) . . ? C73 C72 H72 118.6 . . ? C71 C72 H72 118.6 . . ? C74 C73 C72 118.0(7) . . ? C74 C73 H73 121.0 . . ? C72 C73 H73 121.0 . . ? C75 C74 C73 122.3(7) . . ? C75 C74 Br2 119.6(6) . . ? C73 C74 Br2 118.1(6) . . ? C74 C75 C76 119.2(7) . . ? C74 C75 H75 120.4 . . ? C76 C75 H75 120.4 . . ? C75 C76 C71 119.7(7) . . ? C75 C76 H76 120.1 . . ? C71 C76 H76 120.1 . . ? C82 C81 O85 88.4(10) . . ? C82 C81 H81A 113.9 . . ? O85 C81 H81A 113.9 . . ? C82 C81 H81B 113.9 . . ? O85 C81 H81B 113.9 . . ? H81A C81 H81B 111.1 . . ? C83 C82 C81 113.8(11) . . ? C83 C82 H82A 108.8 . . ? C81 C82 H82A 108.8 . . ? C83 C82 H82B 108.8 . . ? C81 C82 H82B 108.8 . . ? H82A C82 H82B 107.7 . . ? C82 C83 C84 117.5(12) . . ? C82 C83 H83A 107.9 . . ? C84 C83 H83A 107.9 . . ? C82 C83 H83B 107.9 . . ? C84 C83 H83B 107.9 . . ? H83A C83 H83B 107.2 . . ? O85 C84 C83 83.8(9) . . ? O85 C84 H84A 114.7 . . ? C83 C84 H84A 114.7 . . ? O85 C84 H84B 114.7 . . ? C83 C84 H84B 114.7 . . ? H84A C84 H84B 111.8 . . ? C84 O85 C81 136.5(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Fe1 Fe2 C3 94.8(4) . . . . ? C1 Fe1 Fe2 C3 0.8(4) . . . . ? P1 Fe1 Fe2 C3 -123.3(4) . . . . ? S2 Fe1 Fe2 C3 -82.3(3) . . . . ? S1 Fe1 Fe2 C3 171.9(3) . . . . ? C4 Fe1 Fe2 C2 0.5(4) . . . . ? C1 Fe1 Fe2 C2 -93.5(4) . . . . ? P1 Fe1 Fe2 C2 142.4(3) . . . . ? S2 Fe1 Fe2 C2 -176.7(3) . . . . ? S1 Fe1 Fe2 C2 77.5(3) . . . . ? C4 Fe1 Fe2 P2 -133.7(3) . . . . ? C1 Fe1 Fe2 P2 132.3(3) . . . . ? P1 Fe1 Fe2 P2 8.2(3) . . . . ? S2 Fe1 Fe2 P2 49.19(18) . . . . ? S1 Fe1 Fe2 P2 -56.63(18) . . . . ? C4 Fe1 Fe2 S2 177.1(3) . . . . ? C1 Fe1 Fe2 S2 83.1(3) . . . . ? P1 Fe1 Fe2 S2 -40.9(2) . . . . ? S1 Fe1 Fe2 S2 -105.82(9) . . . . ? C4 Fe1 Fe2 S1 -77.1(3) . . . . ? C1 Fe1 Fe2 S1 -171.1(3) . . . . ? P1 Fe1 Fe2 S1 64.9(2) . . . . ? S2 Fe1 Fe2 S1 105.82(9) . . . . ? C3 Fe2 S1 C13 -127.1(7) . . . . ? C2 Fe2 S1 C13 144.3(4) . . . . ? P2 Fe2 S1 C13 51.0(3) . . . . ? S2 Fe2 S1 C13 -54.2(3) . . . . ? Fe1 Fe2 S1 C13 -107.9(3) . . . . ? C3 Fe2 S1 Fe1 -19.2(6) . . . . ? C2 Fe2 S1 Fe1 -107.8(2) . . . . ? P2 Fe2 S1 Fe1 158.96(8) . . . . ? S2 Fe2 S1 Fe1 53.76(7) . . . . ? C4 Fe1 S1 C13 -146.1(4) . . . . ? C1 Fe1 S1 C13 126.0(6) . . . . ? P1 Fe1 S1 C13 -52.8(3) . . . . ? S2 Fe1 S1 C13 54.2(3) . . . . ? Fe2 Fe1 S1 C13 107.9(3) . . . . ? C4 Fe1 S1 Fe2 105.9(3) . . . . ? C1 Fe1 S1 Fe2 18.1(5) . . . . ? P1 Fe1 S1 Fe2 -160.78(8) . . . . ? S2 Fe1 S1 Fe2 -53.76(7) . . . . ? S2 C11 C12 C13 64.7(8) . . . . ? C11 C12 C13 S1 -57.1(8) . . . . ? Fe2 S1 C13 C12 61.4(6) . . . . ? Fe1 S1 C13 C12 -13.7(7) . . . . ? C12 C11 S2 Fe2 -72.4(6) . . . . ? C12 C11 S2 Fe1 1.5(7) . . . . ? C3 Fe2 S2 C11 -147.1(4) . . . . ? C2 Fe2 S2 C11 119.9(8) . . . . ? P2 Fe2 S2 C11 -50.5(3) . . . . ? S1 Fe2 S2 C11 56.9(3) . . . . ? Fe1 Fe2 S2 C11 110.7(3) . . . . ? C3 Fe2 S2 Fe1 102.2(3) . . . . ? C2 Fe2 S2 Fe1 9.2(8) . . . . ? P2 Fe2 S2 Fe1 -161.23(8) . . . . ? S1 Fe2 S2 Fe1 -53.84(7) . . . . ? C4 Fe1 S2 C11 -109.6(8) . . . . ? C1 Fe1 S2 C11 159.7(4) . . . . ? P1 Fe1 S2 C11 64.3(3) . . . . ? S1 Fe1 S2 C11 -48.6(3) . . . . ? Fe2 Fe1 S2 C11 -102.4(3) . . . . ? C4 Fe1 S2 Fe2 -7.2(7) . . . . ? C1 Fe1 S2 Fe2 -97.9(3) . . . . ? P1 Fe1 S2 Fe2 166.73(8) . . . . ? S1 Fe1 S2 Fe2 53.79(7) . . . . ? C4 Fe1 C1 O1 -101(12) . . . . ? P1 Fe1 C1 O1 164(12) . . . . ? S2 Fe1 C1 O1 55(12) . . . . ? S1 Fe1 C1 O1 -15(12) . . . . ? Fe2 Fe1 C1 O1 0(12) . . . . ? C3 Fe2 C2 O2 -129(8) . . . . ? P2 Fe2 C2 O2 135(8) . . . . ? S2 Fe2 C2 O2 -36(8) . . . . ? S1 Fe2 C2 O2 26(8) . . . . ? Fe1 Fe2 C2 O2 -28(8) . . . . ? C2 Fe2 C3 O3 -5(43) . . . . ? P2 Fe2 C3 O3 89(42) . . . . ? S2 Fe2 C3 O3 -164(100) . . . . ? S1 Fe2 C3 O3 -92(42) . . . . ? Fe1 Fe2 C3 O3 -108(42) . . . . ? C1 Fe1 C4 O4 168(100) . . . . ? P1 Fe1 C4 O4 -96(44) . . . . ? S2 Fe1 C4 O4 78(44) . . . . ? S1 Fe1 C4 O4 18(44) . . . . ? Fe2 Fe1 C4 O4 72(44) . . . . ? C4 Fe1 P1 C41 86.5(4) . . . . ? C1 Fe1 P1 C41 -179.9(4) . . . . ? S2 Fe1 P1 C41 -91.1(3) . . . . ? S1 Fe1 P1 C41 -0.5(3) . . . . ? Fe2 Fe1 P1 C41 -56.0(4) . . . . ? C4 Fe1 P1 C31 -150.4(4) . . . . ? C1 Fe1 P1 C31 -56.8(4) . . . . ? S2 Fe1 P1 C31 32.0(3) . . . . ? S1 Fe1 P1 C31 122.6(3) . . . . ? Fe2 Fe1 P1 C31 67.1(4) . . . . ? C4 Fe1 P1 C21 -31.6(4) . . . . ? C1 Fe1 P1 C21 62.0(4) . . . . ? S2 Fe1 P1 C21 150.8(3) . . . . ? S1 Fe1 P1 C21 -118.6(3) . . . . ? Fe2 Fe1 P1 C21 -174.1(3) . . . . ? C41 P1 C21 C26 -172.8(7) . . . . ? C31 P1 C21 C26 81.5(7) . . . . ? Fe1 P1 C21 C26 -46.0(7) . . . . ? C41 P1 C21 C22 11.1(8) . . . . ? C31 P1 C21 C22 -94.6(7) . . . . ? Fe1 P1 C21 C22 137.9(6) . . . . ? C26 C21 C22 C23 1.8(13) . . . . ? P1 C21 C22 C23 178.0(7) . . . . ? C21 C22 C23 C24 -3.2(16) . . . . ? C22 C23 C24 C25 5.4(18) . . . . ? C23 C24 C25 C26 -6.2(17) . . . . ? C24 C25 C26 C21 4.7(15) . . . . ? C22 C21 C26 C25 -2.6(13) . . . . ? P1 C21 C26 C25 -178.9(7) . . . . ? C41 P1 C31 C32 77.6(7) . . . . ? C21 P1 C31 C32 -177.6(7) . . . . ? Fe1 P1 C31 C32 -52.7(8) . . . . ? C41 P1 C31 C36 -102.9(7) . . . . ? C21 P1 C31 C36 1.9(8) . . . . ? Fe1 P1 C31 C36 126.8(7) . . . . ? C36 C31 C32 C33 2.6(14) . . . . ? P1 C31 C32 C33 -177.9(7) . . . . ? C31 C32 C33 C34 -2.8(15) . . . . ? C32 C33 C34 C35 1.8(16) . . . . ? C33 C34 C35 C36 -1.0(18) . . . . ? C34 C35 C36 C31 0.8(18) . . . . ? C32 C31 C36 C35 -1.6(14) . . . . ? P1 C31 C36 C35 178.9(8) . . . . ? C31 P1 C41 C42 -168.6(6) . . . . ? C21 P1 C41 C42 86.2(6) . . . . ? Fe1 P1 C41 C42 -38.2(7) . . . . ? C31 P1 C41 C46 14.0(8) . . . . ? C21 P1 C41 C46 -91.2(7) . . . . ? Fe1 P1 C41 C46 144.4(6) . . . . ? C46 C41 C42 C43 1.9(11) . . . . ? P1 C41 C42 C43 -175.7(6) . . . . ? C41 C42 C43 C44 -2.3(12) . . . . ? C42 C43 C44 C45 2.4(13) . . . . ? C42 C43 C44 Br1 178.8(6) . . . . ? C43 C44 C45 C46 -2.2(13) . . . . ? Br1 C44 C45 C46 -178.5(6) . . . . ? C44 C45 C46 C41 1.9(13) . . . . ? C42 C41 C46 C45 -1.7(12) . . . . ? P1 C41 C46 C45 175.7(6) . . . . ? C3 Fe2 P2 C71 52.2(4) . . . . ? C2 Fe2 P2 C71 144.7(4) . . . . ? S2 Fe2 P2 C71 -38.7(3) . . . . ? S1 Fe2 P2 C71 -127.0(3) . . . . ? Fe1 Fe2 P2 C71 -79.8(3) . . . . ? C3 Fe2 P2 C51 178.2(4) . . . . ? C2 Fe2 P2 C51 -89.3(4) . . . . ? S2 Fe2 P2 C51 87.3(3) . . . . ? S1 Fe2 P2 C51 -1.0(3) . . . . ? Fe1 Fe2 P2 C51 46.3(4) . . . . ? C3 Fe2 P2 C61 -65.2(4) . . . . ? C2 Fe2 P2 C61 27.2(4) . . . . ? S2 Fe2 P2 C61 -156.1(3) . . . . ? S1 Fe2 P2 C61 115.5(3) . . . . ? Fe1 Fe2 P2 C61 162.8(3) . . . . ? C71 P2 C51 C56 -166.3(5) . . . . ? C61 P2 C51 C56 -61.4(6) . . . . ? Fe2 P2 C51 C56 61.6(6) . . . . ? C71 P2 C51 C52 16.4(7) . . . . ? C61 P2 C51 C52 121.3(6) . . . . ? Fe2 P2 C51 C52 -115.7(6) . . . . ? C56 C51 C52 C53 3.1(11) . . . . ? P2 C51 C52 C53 -179.5(6) . . . . ? C51 C52 C53 C54 -0.6(12) . . . . ? C52 C53 C54 C55 -0.8(13) . . . . ? C53 C54 C55 C56 -0.4(13) . . . . ? C54 C55 C56 C51 3.1(12) . . . . ? C52 C51 C56 C55 -4.5(11) . . . . ? P2 C51 C56 C55 178.1(6) . . . . ? C71 P2 C61 C62 92.3(8) . . . . ? C51 P2 C61 C62 -16.1(8) . . . . ? Fe2 P2 C61 C62 -140.7(7) . . . . ? C71 P2 C61 C66 -82.8(6) . . . . ? C51 P2 C61 C66 168.7(6) . . . . ? Fe2 P2 C61 C66 44.2(7) . . . . ? C66 C61 C62 C63 -3.9(13) . . . . ? P2 C61 C62 C63 -179.1(7) . . . . ? C61 C62 C63 C64 2.2(14) . . . . ? C62 C63 C64 C65 -0.1(13) . . . . ? C63 C64 C65 C66 -0.1(13) . . . . ? C64 C65 C66 C61 -1.7(13) . . . . ? C62 C61 C66 C65 3.7(12) . . . . ? P2 C61 C66 C65 179.1(6) . . . . ? C51 P2 C71 C72 -124.2(6) . . . . ? C61 P2 C71 C72 130.5(6) . . . . ? Fe2 P2 C71 C72 6.5(7) . . . . ? C51 P2 C71 C76 55.9(6) . . . . ? C61 P2 C71 C76 -49.4(6) . . . . ? Fe2 P2 C71 C76 -173.3(5) . . . . ? C76 C71 C72 C73 -0.1(11) . . . . ? P2 C71 C72 C73 -180.0(6) . . . . ? C71 C72 C73 C74 1.8(12) . . . . ? C72 C73 C74 C75 -3.3(12) . . . . ? C72 C73 C74 Br2 178.6(6) . . . . ? C73 C74 C75 C76 3.1(13) . . . . ? Br2 C74 C75 C76 -178.9(6) . . . . ? C74 C75 C76 C71 -1.2(12) . . . . ? C72 C71 C76 C75 -0.2(11) . . . . ? P2 C71 C76 C75 179.7(6) . . . . ? O85 C81 C82 C83 1.2(14) . . . . ? C81 C82 C83 C84 -1.0(18) . . . . ? C82 C83 C84 O85 0.1(14) . . . . ? C83 C84 O85 C81 1.0(19) . . . . ? C82 C81 O85 C84 -1.5(19) . . . . ? _diffrn_measured_fraction_theta_max 0.798 _diffrn_reflns_theta_full 33.38 _diffrn_measured_fraction_theta_full 0.798 _refine_diff_density_max 1.180 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.113 # Attachment 'complex 4.CIF' _publ_section_references ; Bergerhoff, G. (1996). DIAMOND - Visual Crystal Structure Information System Gerhard-Domagk-str. 1, 53121 Bonn, Germany Oxford Diffraction. (2003). Oxford Diffraction Ltd., Xcalibur CCD system, CrysAlis Software system, Version 1.170 Sheldrick, G.M. (1990). Acta Cryst. A46, 467-473 Sheldrick, G.M. (1997). SHELXL-97, University of G\"ottingen, Germany. Stoe. (1997). X-RED Data reduction program, version 1.09, X-SHAPE Crystal Optimisation for Numerical Absorption Correction, version 1.2, Stoe & CIE GmbH, Hilpertstra\&se 10, D-64295 Darmstadt, Germany ; data_j2b2r2 _database_code_depnum_ccdc_archive 'CCDC 607113' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H29 Fe2 O5 P S2 Si' _chemical_formula_sum 'C31 H29 Fe2 O5 P S2 Si' _chemical_formula_weight 716.42 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' Fe Fe 0.3463 0.8444 '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' Si Si 0.0817 0.0704 '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 13.001(13) _cell_length_b 8.539(5) _cell_length_c 14.994(10) _cell_angle_alpha 90.09(5) _cell_angle_beta 92.35(7) _cell_angle_gamma 90.09(6) _cell_volume 1663(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16952 _cell_measurement_theta_min 4.24 _cell_measurement_theta_max 31.76 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 1.118 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details 'X-RED (Stoe, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Xcalibur-3 kappa-diffractometer with Sapphire-III CCD' _diffrn_measurement_method '\w scans at different \f' _diffrn_detector_area_resol_mean 12 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% . _diffrn_reflns_number 16952 _diffrn_reflns_av_R_equivalents 0.0930 _diffrn_reflns_av_sigmaI/netI 0.1808 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.24 _diffrn_reflns_theta_max 31.76 _reflns_number_total 7707 _reflns_number_gt 2716 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlis CCD(Oxford Diffraction, 2003)' _computing_cell_refinement 'CrysAlis RED(Oxford Diffraction, 2003)' _computing_data_reduction 'CrysAlis RED(Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Bergerhoff, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1719P)^2^] 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 7707 _refine_ls_number_parameters 344 _refine_ls_number_restraints 131 _refine_ls_R_factor_all 0.2356 _refine_ls_R_factor_gt 0.1015 _refine_ls_wR_factor_ref 0.3295 _refine_ls_wR_factor_gt 0.2732 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.931 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe -0.21453(12) -0.0660(2) 0.10706(11) 0.0628(5) Uani 1 1 d U . . Fe2 Fe -0.22668(14) -0.2597(2) -0.02006(11) 0.0726(6) Uani 1 1 d U . . S1 S -0.2055(2) -0.3282(4) 0.1236(2) 0.0714(9) Uani 1 1 d U . . S2 S -0.3607(2) -0.1194(4) 0.0262(2) 0.0771(10) Uani 1 1 d U . . P1 P -0.2390(2) 0.0263(4) 0.2439(2) 0.0654(9) Uani 1 1 d U . . C1 C -0.2928(13) -0.4308(19) -0.0642(10) 0.096(4) Uani 1 1 d U . . O1 O -0.3322(11) -0.5306(15) -0.0946(8) 0.135(5) Uani 1 1 d U . . C2 C -0.2233(10) -0.135(2) -0.1143(9) 0.091(4) Uani 1 1 d U . . O2 O -0.2289(10) -0.0615(19) -0.1755(8) 0.137(5) Uani 1 1 d U . . C3 C -0.0954(12) -0.305(2) -0.0361(9) 0.091(4) Uani 1 1 d U . . O3 O -0.0083(9) -0.3371(18) -0.0410(8) 0.128(4) Uani 1 1 d U . . C4 C -0.2207(10) 0.1150(16) 0.0523(8) 0.072(3) Uani 1 1 d U . . O4 O -0.2241(10) 0.2305(13) 0.0144(8) 0.118(4) Uani 1 1 d U . . C5 C -0.0777(9) -0.0570(18) 0.1151(8) 0.073(3) Uani 1 1 d U . . O5 O 0.0083(7) -0.0586(14) 0.1184(7) 0.101(3) Uani 1 1 d U . . C11 C -0.3189(10) -0.416(2) 0.1658(10) 0.098(4) Uani 1 1 d U . . H11A H -0.3313 -0.5129 0.1335 0.118 Uiso 1 1 calc R . . H11B H -0.3038 -0.4432 0.2277 0.118 Uiso 1 1 calc R . . C12 C -0.4167(11) -0.325(3) 0.1620(12) 0.129(7) Uani 1 1 d U . . H12A H -0.4704 -0.3934 0.1826 0.155 Uiso 1 1 calc R . . H12B H -0.4090 -0.2406 0.2052 0.155 Uiso 1 1 calc R . . C13 C -0.4542(10) -0.257(2) 0.0795(9) 0.092(4) Uani 1 1 d U . . H13A H -0.5170 -0.2000 0.0903 0.110 Uiso 1 1 calc R . . H13B H -0.4714 -0.3406 0.0377 0.110 Uiso 1 1 calc R . . C21 C -0.2481(6) -0.1245(9) 0.3298(5) 0.064(3) Uani 1 1 d GU . . C22 C -0.1682(5) -0.2323(10) 0.3379(5) 0.073(3) Uani 1 1 d GU . . H22 H -0.1118 -0.2235 0.3021 0.087 Uiso 1 1 calc R . . C23 C -0.1728(6) -0.3533(9) 0.3995(6) 0.083(4) Uani 1 1 d GU . . H23 H -0.1194 -0.4254 0.4049 0.100 Uiso 1 1 calc R . . C24 C -0.2571(7) -0.3665(9) 0.4530(5) 0.080(3) Uani 1 1 d GU . . C25 C -0.3370(5) -0.2588(11) 0.4449(5) 0.090(4) Uani 1 1 d GU . . H25 H -0.3934 -0.2676 0.4807 0.108 Uiso 1 1 calc R . . C26 C -0.3324(5) -0.1378(10) 0.3833(6) 0.085(4) Uani 1 1 d GU . . H26 H -0.3858 -0.0657 0.3779 0.101 Uiso 1 1 calc R . . C27 C -0.2584(11) -0.4954(19) 0.5186(9) 0.086(4) Uani 1 1 d U . . C28 C -0.2664(14) -0.5981(19) 0.5696(10) 0.097(5) Uani 1 1 d U . . Si1 Si -0.2559(3) -0.7613(6) 0.6481(3) 0.0831(11) Uani 1 1 d U . . C51 C -0.185(3) -0.701(3) 0.7462(19) 0.31(2) Uani 1 1 d U . . H51A H -0.2193 -0.6155 0.7735 0.465 Uiso 1 1 calc R . . H51B H -0.1170 -0.6687 0.7307 0.465 Uiso 1 1 calc R . . H51C H -0.1793 -0.7872 0.7873 0.465 Uiso 1 1 calc R . . C52 C -0.183(4) -0.921(4) 0.599(2) 0.34(2) Uani 1 1 d U . . H52A H -0.2200 -0.9594 0.5465 0.515 Uiso 1 1 calc R . . H52B H -0.1743 -1.0041 0.6414 0.515 Uiso 1 1 calc R . . H52C H -0.1169 -0.8828 0.5828 0.515 Uiso 1 1 calc R . . C53 C -0.3811(17) -0.816(5) 0.675(2) 0.33(2) Uani 1 1 d U . . H53A H -0.4191 -0.8490 0.6222 0.496 Uiso 1 1 calc R . . H53B H -0.4151 -0.7288 0.7014 0.496 Uiso 1 1 calc R . . H53C H -0.3776 -0.9014 0.7171 0.496 Uiso 1 1 calc R . . C31 C -0.3497(5) 0.1514(10) 0.2642(5) 0.073(3) Uani 1 1 d GU . . C32 C -0.3524(5) 0.2416(12) 0.3413(5) 0.080(3) Uani 1 1 d GU . . H32 H -0.2962 0.2426 0.3817 0.097 Uiso 1 1 calc . . . C33 C -0.4390(7) 0.3305(11) 0.3580(5) 0.092(4) Uani 1 1 d GU . . H33 H -0.4408 0.3908 0.4095 0.110 Uiso 1 1 calc R . . C34 C -0.5230(5) 0.3290(11) 0.2975(7) 0.086(3) Uani 1 1 d GU . . H34 H -0.5810 0.3884 0.3087 0.103 Uiso 1 1 calc R . . C35 C -0.5203(5) 0.2387(12) 0.2204(6) 0.097(4) Uani 1 1 d GU . . H35 H -0.5765 0.2378 0.1800 0.117 Uiso 1 1 calc R . . C36 C -0.4337(6) 0.1499(11) 0.2038(5) 0.072(3) Uani 1 1 d GU . . H36 H -0.4319 0.0895 0.1522 0.086 Uiso 1 1 calc R . . C41 C -0.1339(6) 0.1475(10) 0.2871(6) 0.071(3) Uani 1 1 d GU . . C42 C -0.1038(7) 0.2728(11) 0.2351(5) 0.087(4) Uani 1 1 d GU . . H42 H -0.1372 0.2916 0.1802 0.105 Uiso 1 1 calc R . . C43 C -0.0238(8) 0.3700(11) 0.2653(7) 0.104(5) Uani 1 1 d GU . . H43 H -0.0037 0.4539 0.2305 0.125 Uiso 1 1 calc R . . C44 C 0.0261(7) 0.3419(13) 0.3475(7) 0.108(5) Uani 1 1 d GU . . H44 H 0.0796 0.4070 0.3676 0.129 Uiso 1 1 calc R . . C45 C -0.0040(8) 0.2166(14) 0.3995(6) 0.124(6) Uani 1 1 d GU . . H45 H 0.0294 0.1978 0.4544 0.148 Uiso 1 1 calc R . . C46 C -0.0840(7) 0.1194(11) 0.3693(6) 0.094(5) Uani 1 1 d GU . . H46 H -0.1041 0.0356 0.4041 0.113 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0636(9) 0.0609(11) 0.0632(9) 0.0069(9) -0.0058(7) -0.0151(10) Fe2 0.0803(11) 0.0708(14) 0.0658(10) 0.0076(10) -0.0091(8) -0.0164(12) S1 0.0757(18) 0.064(2) 0.0741(19) 0.0184(17) -0.0036(14) -0.0096(19) S2 0.0687(17) 0.073(2) 0.088(2) 0.0142(17) -0.0186(14) -0.0148(17) P1 0.0553(15) 0.073(2) 0.0669(17) 0.0100(15) -0.0081(12) -0.0076(16) C1 0.127(10) 0.053(7) 0.104(9) 0.006(6) -0.041(8) 0.004(7) O1 0.187(12) 0.098(9) 0.115(9) 0.021(7) -0.035(8) -0.066(9) C2 0.071(7) 0.121(12) 0.078(6) 0.037(7) -0.015(5) -0.020(7) O2 0.147(9) 0.165(13) 0.097(8) 0.050(8) -0.020(7) -0.048(10) C3 0.088(6) 0.112(12) 0.073(7) 0.014(7) -0.001(5) 0.010(7) O3 0.105(7) 0.138(11) 0.143(10) 0.033(9) 0.035(7) 0.044(8) C4 0.095(8) 0.059(5) 0.059(6) 0.019(5) -0.007(6) -0.011(6) O4 0.155(10) 0.071(7) 0.125(8) 0.033(6) -0.038(7) -0.007(8) C5 0.053(4) 0.080(9) 0.087(8) 0.001(7) 0.008(4) -0.009(6) O5 0.065(4) 0.108(9) 0.132(8) -0.008(7) 0.021(5) -0.018(6) C11 0.089(7) 0.101(10) 0.105(9) 0.015(9) 0.017(7) -0.038(7) C12 0.078(7) 0.149(17) 0.160(14) 0.073(13) 0.005(8) -0.030(9) C13 0.072(6) 0.115(12) 0.089(8) -0.007(8) 0.005(5) -0.037(7) C21 0.068(6) 0.052(6) 0.070(6) 0.002(5) 0.000(5) 0.003(5) C22 0.069(6) 0.077(9) 0.072(7) 0.013(6) -0.001(5) 0.014(6) C23 0.091(8) 0.071(9) 0.087(9) 0.019(7) -0.011(5) 0.033(7) C24 0.077(7) 0.066(8) 0.095(9) 0.012(6) -0.010(6) -0.020(6) C25 0.072(7) 0.088(10) 0.109(10) 0.022(8) -0.001(6) -0.003(6) C26 0.057(6) 0.087(10) 0.111(10) 0.024(7) 0.014(5) -0.008(6) C27 0.101(9) 0.079(9) 0.077(8) 0.009(6) -0.011(7) 0.000(8) C28 0.136(12) 0.077(9) 0.077(8) 0.008(6) -0.010(8) -0.018(9) Si1 0.087(2) 0.075(3) 0.088(2) 0.018(2) 0.0035(18) 0.002(2) C51 0.57(5) 0.15(2) 0.19(2) 0.094(15) -0.21(3) -0.13(3) C52 0.60(5) 0.26(3) 0.19(2) 0.097(18) 0.19(3) 0.30(4) C53 0.095(11) 0.39(5) 0.51(5) 0.35(4) 0.045(16) 0.018(17) C31 0.061(5) 0.084(9) 0.074(6) 0.021(5) -0.005(5) 0.005(5) C32 0.068(6) 0.074(10) 0.098(8) 0.006(6) -0.004(6) 0.000(6) C33 0.094(8) 0.065(10) 0.114(10) 0.002(8) -0.007(6) 0.007(7) C34 0.068(7) 0.062(9) 0.129(10) 0.031(7) 0.010(6) 0.010(7) C35 0.083(8) 0.092(12) 0.114(10) 0.026(7) -0.030(7) 0.028(8) C36 0.075(6) 0.049(8) 0.090(7) 0.014(6) -0.024(5) 0.010(6) C41 0.064(6) 0.056(7) 0.091(7) 0.000(5) -0.016(5) -0.007(6) C42 0.092(8) 0.078(10) 0.090(8) -0.001(7) -0.011(6) -0.017(7) C43 0.113(11) 0.109(13) 0.091(9) -0.015(8) 0.025(7) -0.058(9) C44 0.085(9) 0.088(11) 0.148(12) -0.028(9) -0.028(9) -0.012(9) C45 0.122(12) 0.121(15) 0.124(12) 0.001(9) -0.049(10) -0.026(11) C46 0.073(8) 0.106(12) 0.101(9) 0.004(8) -0.035(7) -0.003(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C4 1.752(13) . ? Fe1 C5 1.780(11) . ? Fe1 P1 2.232(4) . ? Fe1 S1 2.255(4) . ? Fe1 S2 2.257(4) . ? Fe1 Fe2 2.521(3) . ? Fe2 C2 1.775(14) . ? Fe2 C3 1.776(16) . ? Fe2 C1 1.805(17) . ? Fe2 S1 2.240(4) . ? Fe2 S2 2.248(5) . ? S1 C11 1.791(13) . ? S2 C13 1.889(14) . ? P1 C41 1.811(7) . ? P1 C31 1.828(7) . ? P1 C21 1.830(7) . ? C1 O1 1.083(17) . ? C2 O2 1.110(16) . ? C3 O3 1.172(16) . ? C4 O4 1.139(15) . ? C5 O5 1.117(13) . ? C11 C12 1.49(2) . ? C12 C13 1.43(2) . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C24 C27 1.477(16) . ? C25 C26 1.3900 . ? C27 C28 1.172(19) . ? C28 Si1 1.827(16) . ? Si1 C53 1.76(2) . ? Si1 C51 1.78(2) . ? Si1 C52 1.83(3) . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? 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 C4 Fe1 C5 91.3(6) . . ? C4 Fe1 P1 96.6(5) . . ? C5 Fe1 P1 95.9(4) . . ? C4 Fe1 S1 158.4(4) . . ? C5 Fe1 S1 89.2(5) . . ? P1 Fe1 S1 104.89(15) . . ? C4 Fe1 S2 84.4(4) . . ? C5 Fe1 S2 149.5(4) . . ? P1 Fe1 S2 114.52(16) . . ? S1 Fe1 S2 84.26(15) . . ? C4 Fe1 Fe2 102.9(4) . . ? C5 Fe1 Fe2 96.3(5) . . ? P1 Fe1 Fe2 156.70(12) . . ? S1 Fe1 Fe2 55.59(11) . . ? S2 Fe1 Fe2 55.81(13) . . ? C2 Fe2 C3 88.2(7) . . ? C2 Fe2 C1 102.8(7) . . ? C3 Fe2 C1 102.7(8) . . ? C2 Fe2 S1 156.7(6) . . ? C3 Fe2 S1 89.5(4) . . ? C1 Fe2 S1 100.3(5) . . ? C2 Fe2 S2 88.2(6) . . ? C3 Fe2 S2 156.8(6) . . ? C1 Fe2 S2 100.4(6) . . ? S1 Fe2 S2 84.81(16) . . ? C2 Fe2 Fe1 101.8(6) . . ? C3 Fe2 Fe1 102.4(5) . . ? C1 Fe2 Fe1 145.1(6) . . ? S1 Fe2 Fe1 56.17(12) . . ? S2 Fe2 Fe1 56.13(11) . . ? C11 S1 Fe2 112.2(5) . . ? C11 S1 Fe1 114.4(6) . . ? Fe2 S1 Fe1 68.24(12) . . ? C13 S2 Fe2 108.6(6) . . ? C13 S2 Fe1 116.0(4) . . ? Fe2 S2 Fe1 68.06(13) . . ? C41 P1 C31 101.2(5) . . ? C41 P1 C21 102.7(4) . . ? C31 P1 C21 102.8(4) . . ? C41 P1 Fe1 113.3(4) . . ? C31 P1 Fe1 120.1(3) . . ? C21 P1 Fe1 114.5(3) . . ? O1 C1 Fe2 176.7(15) . . ? O2 C2 Fe2 174.2(12) . . ? O3 C3 Fe2 175.7(12) . . ? O4 C4 Fe1 178.0(14) . . ? O5 C5 Fe1 176.5(15) . . ? C12 C11 S1 118.9(12) . . ? C13 C12 C11 120.3(16) . . ? C12 C13 S2 114.6(9) . . ? C22 C21 C26 120.0 . . ? C22 C21 P1 117.4(5) . . ? C26 C21 P1 122.6(4) . . ? C23 C22 C21 120.0 . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 C27 121.6(9) . . ? C23 C24 C27 118.4(9) . . ? C26 C25 C24 120.0 . . ? C25 C26 C21 120.0 . . ? C28 C27 C24 175.5(16) . . ? C27 C28 Si1 170.6(17) . . ? C53 Si1 C51 110(2) . . ? C53 Si1 C28 107.9(11) . . ? C51 Si1 C28 109.7(9) . . ? C53 Si1 C52 113(2) . . ? C51 Si1 C52 107(2) . . ? C28 Si1 C52 109.6(10) . . ? C32 C31 C36 120.0 . . ? C32 C31 P1 120.6(5) . . ? C36 C31 P1 119.4(5) . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C36 C31 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 P1 117.6(5) . . ? C46 C41 P1 122.4(5) . . ? C41 C42 C43 120.0 . . ? C42 C43 C44 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 C46 120.0 . . ? C45 C46 C41 120.0 . . ? _diffrn_measured_fraction_theta_max 0.681 _diffrn_reflns_theta_full 31.76 _diffrn_measured_fraction_theta_full 0.681 _refine_diff_density_max 0.870 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.111