# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_str0540 _database_code_depnum_ccdc_archive 'CCDC 639866' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H33 Fe2 N O4 P2 S2' _chemical_formula_weight 757.37 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' Fe Fe 0.3463 0.8444 '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 9.7227(10) _cell_length_b 10.3859(11) _cell_length_c 18.5263(19) _cell_angle_alpha 84.913(2) _cell_angle_beta 80.645(2) _cell_angle_gamma 63.569(2) _cell_volume 1652.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 1.141 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7714 _exptl_absorpt_correction_T_max 0.8566 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14333 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 28.31 _reflns_number_total 7563 _reflns_number_gt 6917 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0557P)^2^+2.8501P] 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 7563 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.1095 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.51744(4) 0.36202(3) 0.272386(17) 0.01089(9) Uani 1 1 d . . . Fe2 Fe 0.44438(4) 0.27286(4) 0.403438(18) 0.01320(9) Uani 1 1 d . . . P1 P 0.77021(7) 0.29495(6) 0.24932(3) 0.01170(12) Uani 1 1 d . . . P2 P 0.62387(7) 0.17397(6) 0.19995(3) 0.01232(13) Uani 1 1 d . . . S1 S 0.29936(7) 0.34150(6) 0.31094(3) 0.01587(13) Uani 1 1 d . . . S2 S 0.47348(7) 0.47571(6) 0.37575(3) 0.01588(13) Uani 1 1 d . . . N1 N 0.8103(2) 0.1518(2) 0.19667(11) 0.0148(4) Uani 1 1 d . . . O1 O 0.3750(2) 0.6158(2) 0.18172(10) 0.0232(4) Uani 1 1 d . . . O2 O 0.2227(2) 0.3484(2) 0.53867(11) 0.0288(4) Uani 1 1 d . . . O3 O 0.7204(3) 0.1534(3) 0.47764(13) 0.0345(5) Uani 1 1 d . . . O4 O 0.4666(3) -0.0185(2) 0.40865(11) 0.0270(4) Uani 1 1 d . . . C1 C 0.4404(3) 0.5110(3) 0.21455(13) 0.0146(4) Uani 1 1 d . . . C2 C 0.3075(3) 0.3215(3) 0.48557(13) 0.0178(5) Uani 1 1 d . . . C3 C 0.6167(3) 0.2016(3) 0.44650(14) 0.0212(5) Uani 1 1 d . . . C4 C 0.4596(3) 0.0941(3) 0.40197(13) 0.0174(5) Uani 1 1 d . . . C5 C 0.1388(3) 0.5205(3) 0.3247(2) 0.0318(7) Uani 1 1 d . . . H5A H 0.1364 0.5759 0.2782 0.038 Uiso 1 1 calc R . . H5B H 0.0411 0.5098 0.3345 0.038 Uiso 1 1 calc R . . C6 C 0.1392(4) 0.6052(4) 0.3825(2) 0.0379(7) Uani 1 1 d . . . H6A H 0.1224 0.5580 0.4296 0.045 Uiso 1 1 calc R . . H6B H 0.0484 0.7002 0.3811 0.045 Uiso 1 1 calc R . . C7 C 0.2825(3) 0.6322(3) 0.38309(17) 0.0287(6) Uani 1 1 d . . . H7A H 0.2677 0.6816 0.4290 0.034 Uiso 1 1 calc R . . H7B H 0.2849 0.6996 0.3422 0.034 Uiso 1 1 calc R . . C8 C 0.9547(3) 0.0757(3) 0.14429(15) 0.0287(6) Uani 1 1 d . . . H8A H 1.0362 0.0888 0.1651 0.034 Uiso 1 1 calc R . . C9 C 0.9512(3) 0.1483(3) 0.06958(14) 0.0222(5) Uani 1 1 d . . . H9A H 1.0488 0.0939 0.0381 0.033 Uiso 1 1 calc R . . H9B H 0.9381 0.2464 0.0746 0.033 Uiso 1 1 calc R . . H9C H 0.8645 0.1517 0.0476 0.033 Uiso 1 1 calc R . . C10 C 1.0131(4) -0.0809(4) 0.1419(2) 0.0435(8) Uani 1 1 d . . . H10A H 1.0128 -0.1205 0.1919 0.065 Uiso 1 1 calc R . . H10B H 1.1192 -0.1229 0.1160 0.065 Uiso 1 1 calc R . . H10C H 0.9464 -0.1038 0.1163 0.065 Uiso 1 1 calc R . . C11 C 0.8607(3) 0.3998(3) 0.19396(13) 0.0152(4) Uani 1 1 d . . . C12 C 1.0157(3) 0.3696(3) 0.19598(15) 0.0228(5) Uani 1 1 d . . . H12A H 1.0729 0.2993 0.2297 0.027 Uiso 1 1 calc R . . C13 C 1.0862(3) 0.4415(4) 0.14912(16) 0.0307(7) Uani 1 1 d . . . H13A H 1.1915 0.4194 0.1507 0.037 Uiso 1 1 calc R . . C14 C 1.0040(4) 0.5451(4) 0.10003(16) 0.0303(6) Uani 1 1 d . . . H14A H 1.0526 0.5944 0.0683 0.036 Uiso 1 1 calc R . . C15 C 0.8503(4) 0.5766(3) 0.09744(16) 0.0276(6) Uani 1 1 d . . . H15A H 0.7934 0.6473 0.0638 0.033 Uiso 1 1 calc R . . C16 C 0.7800(3) 0.5044(3) 0.14412(14) 0.0208(5) Uani 1 1 d . . . H16A H 0.6747 0.5266 0.1421 0.025 Uiso 1 1 calc R . . C17 C 0.8908(3) 0.2296(3) 0.32218(13) 0.0146(4) Uani 1 1 d . . . C18 C 0.9848(4) 0.0857(3) 0.33491(17) 0.0285(6) Uani 1 1 d . . . H18A H 0.9889 0.0149 0.3044 0.034 Uiso 1 1 calc R . . C19 C 1.0729(4) 0.0444(3) 0.39202(18) 0.0335(7) Uani 1 1 d . . . H19A H 1.1375 -0.0546 0.4002 0.040 Uiso 1 1 calc R . . C20 C 1.0675(3) 0.1466(3) 0.43731(15) 0.0226(5) Uani 1 1 d . . . H20A H 1.1277 0.1180 0.4765 0.027 Uiso 1 1 calc R . . C21 C 0.9739(3) 0.2904(3) 0.42483(13) 0.0171(5) Uani 1 1 d . . . H21A H 0.9701 0.3608 0.4555 0.020 Uiso 1 1 calc R . . C22 C 0.8852(3) 0.3326(3) 0.36783(13) 0.0147(4) Uani 1 1 d . . . H22A H 0.8207 0.4317 0.3598 0.018 Uiso 1 1 calc R . . C23 C 0.5890(3) 0.1809(3) 0.10479(13) 0.0155(5) Uani 1 1 d . . . C24 C 0.6396(3) 0.0560(3) 0.06480(14) 0.0195(5) Uani 1 1 d . . . H24A H 0.6860 -0.0355 0.0881 0.023 Uiso 1 1 calc R . . C25 C 0.6225(3) 0.0646(3) -0.00891(14) 0.0220(5) Uani 1 1 d . . . H25A H 0.6591 -0.0210 -0.0357 0.026 Uiso 1 1 calc R . . C26 C 0.5525(4) 0.1969(3) -0.04319(14) 0.0258(6) Uani 1 1 d . . . H26A H 0.5407 0.2025 -0.0934 0.031 Uiso 1 1 calc R . . C27 C 0.4997(4) 0.3210(3) -0.00392(15) 0.0278(6) Uani 1 1 d . . . H27A H 0.4507 0.4121 -0.0273 0.033 Uiso 1 1 calc R . . C28 C 0.5178(3) 0.3137(3) 0.06962(14) 0.0211(5) Uani 1 1 d . . . H28A H 0.4813 0.3998 0.0960 0.025 Uiso 1 1 calc R . . C29 C 0.6148(3) 0.0063(3) 0.23047(13) 0.0160(5) Uani 1 1 d . . . C30 C 0.4810(3) -0.0069(3) 0.22290(14) 0.0204(5) Uani 1 1 d . . . H30A H 0.4001 0.0695 0.2011 0.024 Uiso 1 1 calc R . . C31 C 0.4654(4) -0.1306(3) 0.24701(15) 0.0250(6) Uani 1 1 d . . . H31A H 0.3738 -0.1386 0.2420 0.030 Uiso 1 1 calc R . . C32 C 0.5835(4) -0.2424(3) 0.27833(16) 0.0268(6) Uani 1 1 d . . . H32A H 0.5741 -0.3282 0.2939 0.032 Uiso 1 1 calc R . . C33 C 0.7155(3) -0.2293(3) 0.28700(17) 0.0299(6) Uani 1 1 d . . . H33A H 0.7961 -0.3057 0.3089 0.036 Uiso 1 1 calc R . . C34 C 0.7304(3) -0.1047(3) 0.26377(15) 0.0235(5) Uani 1 1 d . . . H34A H 0.8203 -0.0956 0.2707 0.028 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 0.01041(16) 0.01068(16) 0.01018(16) 0.00089(11) -0.00100(12) -0.00368(13) Fe2 0.01536(17) 0.01292(17) 0.01098(17) 0.00079(12) -0.00041(12) -0.00654(14) P1 0.0107(3) 0.0125(3) 0.0105(3) -0.0007(2) -0.0011(2) -0.0038(2) P2 0.0139(3) 0.0121(3) 0.0110(3) 0.0002(2) -0.0024(2) -0.0055(2) S1 0.0113(3) 0.0157(3) 0.0191(3) 0.0035(2) -0.0024(2) -0.0051(2) S2 0.0195(3) 0.0136(3) 0.0139(3) -0.0026(2) 0.0025(2) -0.0079(2) N1 0.0143(9) 0.0142(9) 0.0134(9) -0.0031(7) -0.0002(7) -0.0041(8) O1 0.0250(10) 0.0168(9) 0.0234(10) 0.0056(7) -0.0064(8) -0.0054(8) O2 0.0281(11) 0.0318(11) 0.0188(10) -0.0004(8) 0.0038(8) -0.0087(9) O3 0.0322(11) 0.0435(13) 0.0381(12) 0.0191(10) -0.0175(10) -0.0251(10) O4 0.0393(12) 0.0197(10) 0.0230(10) 0.0003(7) 0.0004(8) -0.0154(9) C1 0.0139(11) 0.0144(11) 0.0143(11) -0.0013(8) -0.0014(8) -0.0053(9) C2 0.0199(12) 0.0164(11) 0.0152(11) 0.0009(9) -0.0022(9) -0.0067(10) C3 0.0258(13) 0.0239(13) 0.0191(12) 0.0058(10) -0.0045(10) -0.0163(11) C4 0.0187(12) 0.0198(12) 0.0127(11) -0.0005(9) -0.0005(9) -0.0080(10) C5 0.0112(12) 0.0193(13) 0.057(2) 0.0061(13) -0.0018(12) -0.0016(10) C6 0.0307(16) 0.0303(16) 0.0410(18) -0.0075(13) -0.0082(14) -0.0005(13) C7 0.0261(14) 0.0122(12) 0.0383(16) -0.0062(11) 0.0126(12) -0.0046(11) C8 0.0229(14) 0.0267(14) 0.0192(13) -0.0046(10) 0.0059(11) 0.0023(11) C9 0.0213(13) 0.0253(13) 0.0185(12) -0.0065(10) 0.0059(10) -0.0108(11) C10 0.0384(19) 0.0377(19) 0.044(2) -0.0084(15) 0.0050(15) -0.0095(16) C11 0.0164(11) 0.0194(12) 0.0114(10) -0.0013(8) 0.0000(8) -0.0096(10) C12 0.0197(12) 0.0322(15) 0.0191(12) 0.0028(10) -0.0037(10) -0.0139(11) C13 0.0225(14) 0.0492(19) 0.0270(15) 0.0048(13) -0.0026(11) -0.0229(14) C14 0.0332(16) 0.0440(18) 0.0221(14) 0.0063(12) 0.0002(12) -0.0270(14) C15 0.0293(15) 0.0323(15) 0.0216(13) 0.0075(11) -0.0032(11) -0.0153(13) C16 0.0179(12) 0.0252(13) 0.0195(12) 0.0036(10) -0.0032(10) -0.0100(10) C17 0.0140(11) 0.0164(11) 0.0126(10) 0.0001(8) -0.0029(8) -0.0056(9) C18 0.0346(16) 0.0159(13) 0.0338(16) -0.0031(11) -0.0188(13) -0.0049(12) C19 0.0409(18) 0.0169(13) 0.0403(17) 0.0035(12) -0.0268(14) -0.0042(12) C20 0.0238(13) 0.0243(13) 0.0210(13) 0.0035(10) -0.0107(10) -0.0099(11) C21 0.0176(11) 0.0217(12) 0.0147(11) -0.0018(9) -0.0013(9) -0.0112(10) C22 0.0143(11) 0.0141(11) 0.0142(11) -0.0004(8) 0.0003(8) -0.0055(9) C23 0.0168(11) 0.0216(12) 0.0109(10) 0.0000(9) -0.0027(8) -0.0107(10) C24 0.0210(12) 0.0213(12) 0.0172(12) -0.0012(9) -0.0029(9) -0.0100(10) C25 0.0221(13) 0.0297(14) 0.0181(12) -0.0053(10) -0.0021(10) -0.0141(11) C26 0.0349(15) 0.0378(16) 0.0135(12) 0.0025(10) -0.0059(11) -0.0233(13) C27 0.0422(17) 0.0265(14) 0.0185(13) 0.0067(10) -0.0123(12) -0.0171(13) C28 0.0294(14) 0.0197(12) 0.0168(12) 0.0013(9) -0.0066(10) -0.0123(11) C29 0.0216(12) 0.0123(11) 0.0148(11) -0.0006(8) 0.0000(9) -0.0089(9) C30 0.0267(13) 0.0200(12) 0.0181(12) 0.0015(9) -0.0063(10) -0.0129(11) C31 0.0341(15) 0.0260(14) 0.0216(13) -0.0048(10) 0.0005(11) -0.0197(12) C32 0.0348(15) 0.0167(12) 0.0268(14) -0.0011(10) 0.0076(12) -0.0133(12) C33 0.0254(14) 0.0163(13) 0.0377(16) 0.0094(11) 0.0002(12) -0.0033(11) C34 0.0177(12) 0.0196(13) 0.0293(14) 0.0047(10) 0.0000(10) -0.0067(10) _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 C1 1.743(2) . ? Fe1 P1 2.2124(7) . ? Fe1 P2 2.2137(7) . ? Fe1 S2 2.2203(7) . ? Fe1 S1 2.2214(7) . ? Fe1 Fe2 2.6236(5) . ? Fe2 C3 1.793(3) . ? Fe2 C2 1.794(3) . ? Fe2 C4 1.798(3) . ? Fe2 S2 2.2524(7) . ? Fe2 S1 2.2598(7) . ? P1 N1 1.712(2) . ? P1 C17 1.817(2) . ? P1 C11 1.837(2) . ? P1 P2 2.5803(8) . ? P2 N1 1.714(2) . ? P2 C29 1.818(2) . ? P2 C23 1.838(2) . ? S1 C5 1.825(3) . ? S2 C7 1.838(3) . ? N1 C8 1.498(3) . ? O1 C1 1.163(3) . ? O2 C2 1.143(3) . ? O3 C3 1.136(3) . ? O4 C4 1.138(3) . ? C5 C6 1.446(5) . ? C6 C7 1.540(5) . ? C8 C10 1.466(5) . ? C8 C9 1.514(4) . ? C11 C16 1.395(3) . ? C11 C12 1.401(3) . ? C12 C13 1.389(4) . ? C13 C14 1.386(4) . ? C14 C15 1.389(4) . ? C15 C16 1.388(4) . ? C17 C18 1.384(4) . ? C17 C22 1.399(3) . ? C18 C19 1.388(4) . ? C19 C20 1.389(4) . ? C20 C21 1.382(4) . ? C21 C22 1.388(3) . ? C23 C28 1.394(3) . ? C23 C24 1.399(3) . ? C24 C25 1.393(4) . ? C25 C26 1.381(4) . ? C26 C27 1.382(4) . ? C27 C28 1.393(4) . ? C29 C34 1.386(4) . ? C29 C30 1.397(4) . ? C30 C31 1.388(4) . ? C31 C32 1.383(4) . ? C32 C33 1.385(4) . ? C33 C34 1.388(4) . ? 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 C1 Fe1 P1 103.57(8) . . ? C1 Fe1 P2 105.18(8) . . ? P1 Fe1 P2 71.32(2) . . ? C1 Fe1 S2 98.94(8) . . ? P1 Fe1 S2 97.43(2) . . ? P2 Fe1 S2 155.14(3) . . ? C1 Fe1 S1 97.35(8) . . ? P1 Fe1 S1 157.69(3) . . ? P2 Fe1 S1 95.92(3) . . ? S2 Fe1 S1 86.77(3) . . ? C1 Fe1 Fe2 138.66(8) . . ? P1 Fe1 Fe2 110.44(2) . . ? P2 Fe1 Fe2 107.44(2) . . ? S2 Fe1 Fe2 54.656(19) . . ? S1 Fe1 Fe2 54.848(18) . . ? C3 Fe2 C2 97.06(12) . . ? C3 Fe2 C4 89.11(12) . . ? C2 Fe2 C4 94.50(11) . . ? C3 Fe2 S2 89.11(8) . . ? C2 Fe2 S2 101.91(8) . . ? C4 Fe2 S2 163.59(8) . . ? C3 Fe2 S1 157.61(9) . . ? C2 Fe2 S1 105.29(8) . . ? C4 Fe2 S1 90.40(8) . . ? S2 Fe2 S1 85.09(2) . . ? C3 Fe2 Fe1 106.30(8) . . ? C2 Fe2 Fe1 144.71(8) . . ? C4 Fe2 Fe1 111.62(8) . . ? S2 Fe2 Fe1 53.519(18) . . ? S1 Fe2 Fe1 53.488(18) . . ? N1 P1 C17 108.07(11) . . ? N1 P1 C11 105.35(10) . . ? C17 P1 C11 100.33(11) . . ? N1 P1 Fe1 95.50(7) . . ? C17 P1 Fe1 121.02(8) . . ? C11 P1 Fe1 124.68(8) . . ? N1 P1 P2 41.16(7) . . ? C17 P1 P2 127.57(8) . . ? C11 P1 P2 125.21(8) . . ? Fe1 P1 P2 54.36(2) . . ? N1 P2 C29 109.20(11) . . ? N1 P2 C23 106.81(10) . . ? C29 P2 C23 99.69(11) . . ? N1 P2 Fe1 95.40(7) . . ? C29 P2 Fe1 120.60(8) . . ? C23 P2 Fe1 124.02(8) . . ? N1 P2 P1 41.10(7) . . ? C29 P2 P1 128.33(8) . . ? C23 P2 P1 126.14(8) . . ? Fe1 P2 P1 54.32(2) . . ? C5 S1 Fe1 109.21(10) . . ? C5 S1 Fe2 111.89(12) . . ? Fe1 S1 Fe2 71.66(2) . . ? C7 S2 Fe1 109.92(11) . . ? C7 S2 Fe2 109.84(9) . . ? Fe1 S2 Fe2 71.83(2) . . ? C8 N1 P1 126.24(19) . . ? C8 N1 P2 132.32(19) . . ? P1 N1 P2 97.74(10) . . ? O1 C1 Fe1 172.6(2) . . ? O2 C2 Fe2 177.9(2) . . ? O3 C3 Fe2 175.3(2) . . ? O4 C4 Fe2 173.0(2) . . ? C6 C5 S1 117.5(2) . . ? C5 C6 C7 119.0(3) . . ? C6 C7 S2 117.8(2) . . ? C10 C8 N1 115.7(3) . . ? C10 C8 C9 113.9(3) . . ? N1 C8 C9 113.5(2) . . ? C16 C11 C12 118.1(2) . . ? C16 C11 P1 120.32(18) . . ? C12 C11 P1 121.3(2) . . ? C13 C12 C11 120.5(3) . . ? C14 C13 C12 120.5(3) . . ? C13 C14 C15 119.7(3) . . ? C16 C15 C14 119.8(3) . . ? C15 C16 C11 121.4(2) . . ? C18 C17 C22 119.2(2) . . ? C18 C17 P1 123.82(19) . . ? C22 C17 P1 116.99(18) . . ? C17 C18 C19 120.4(3) . . ? C18 C19 C20 120.5(3) . . ? C21 C20 C19 119.4(2) . . ? C20 C21 C22 120.5(2) . . ? C21 C22 C17 120.1(2) . . ? C28 C23 C24 118.5(2) . . ? C28 C23 P2 119.63(19) . . ? C24 C23 P2 121.82(19) . . ? C25 C24 C23 120.6(2) . . ? C26 C25 C24 120.3(2) . . ? C25 C26 C27 119.6(2) . . ? C26 C27 C28 120.6(3) . . ? C27 C28 C23 120.4(2) . . ? C34 C29 C30 119.1(2) . . ? C34 C29 P2 123.0(2) . . ? C30 C29 P2 117.81(19) . . ? C31 C30 C29 120.5(3) . . ? C32 C31 C30 119.9(3) . . ? C31 C32 C33 119.9(3) . . ? C32 C33 C34 120.3(3) . . ? C29 C34 C33 120.3(3) . . ? 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 C1 Fe1 Fe2 C3 -135.15(15) . . . . ? P1 Fe1 Fe2 C3 8.22(9) . . . . ? P2 Fe1 Fe2 C3 84.26(9) . . . . ? S2 Fe1 Fe2 C3 -76.33(9) . . . . ? S1 Fe1 Fe2 C3 169.15(9) . . . . ? C1 Fe1 Fe2 C2 -5.74(19) . . . . ? P1 Fe1 Fe2 C2 137.64(15) . . . . ? P2 Fe1 Fe2 C2 -146.32(15) . . . . ? S2 Fe1 Fe2 C2 53.09(15) . . . . ? S1 Fe1 Fe2 C2 -61.43(15) . . . . ? C1 Fe1 Fe2 C4 129.20(15) . . . . ? P1 Fe1 Fe2 C4 -87.43(9) . . . . ? P2 Fe1 Fe2 C4 -11.39(9) . . . . ? S2 Fe1 Fe2 C4 -171.98(9) . . . . ? S1 Fe1 Fe2 C4 73.50(9) . . . . ? C1 Fe1 Fe2 S2 -58.82(12) . . . . ? P1 Fe1 Fe2 S2 84.55(3) . . . . ? P2 Fe1 Fe2 S2 160.59(3) . . . . ? S1 Fe1 Fe2 S2 -114.52(3) . . . . ? C1 Fe1 Fe2 S1 55.70(12) . . . . ? P1 Fe1 Fe2 S1 -160.93(3) . . . . ? P2 Fe1 Fe2 S1 -84.89(3) . . . . ? S2 Fe1 Fe2 S1 114.52(3) . . . . ? C1 Fe1 P1 N1 -103.15(11) . . . . ? P2 Fe1 P1 N1 -1.45(7) . . . . ? S2 Fe1 P1 N1 155.74(7) . . . . ? S1 Fe1 P1 N1 56.04(10) . . . . ? Fe2 Fe1 P1 N1 100.76(7) . . . . ? C1 Fe1 P1 C17 141.92(12) . . . . ? P2 Fe1 P1 C17 -116.38(10) . . . . ? S2 Fe1 P1 C17 40.81(10) . . . . ? S1 Fe1 P1 C17 -58.89(12) . . . . ? Fe2 Fe1 P1 C17 -14.16(10) . . . . ? C1 Fe1 P1 C11 9.81(13) . . . . ? P2 Fe1 P1 C11 111.51(10) . . . . ? S2 Fe1 P1 C11 -91.30(10) . . . . ? S1 Fe1 P1 C11 169.00(10) . . . . ? Fe2 Fe1 P1 C11 -146.28(9) . . . . ? C1 Fe1 P1 P2 -101.70(8) . . . . ? S2 Fe1 P1 P2 157.19(3) . . . . ? S1 Fe1 P1 P2 57.49(7) . . . . ? Fe2 Fe1 P1 P2 102.22(2) . . . . ? C1 Fe1 P2 N1 100.94(11) . . . . ? P1 Fe1 P2 N1 1.45(7) . . . . ? S2 Fe1 P2 N1 -64.67(10) . . . . ? S1 Fe1 P2 N1 -159.77(7) . . . . ? Fe2 Fe1 P2 N1 -104.82(7) . . . . ? C1 Fe1 P2 C29 -142.98(13) . . . . ? P1 Fe1 P2 C29 117.54(10) . . . . ? S2 Fe1 P2 C29 51.42(12) . . . . ? S1 Fe1 P2 C29 -43.69(10) . . . . ? Fe2 Fe1 P2 C29 11.27(10) . . . . ? C1 Fe1 P2 C23 -13.54(13) . . . . ? P1 Fe1 P2 C23 -113.03(10) . . . . ? S2 Fe1 P2 C23 -179.15(10) . . . . ? S1 Fe1 P2 C23 85.74(10) . . . . ? Fe2 Fe1 P2 C23 140.70(9) . . . . ? C1 Fe1 P2 P1 99.49(8) . . . . ? S2 Fe1 P2 P1 -66.12(6) . . . . ? S1 Fe1 P2 P1 -161.23(3) . . . . ? Fe2 Fe1 P2 P1 -106.27(2) . . . . ? C17 P1 P2 N1 -73.41(14) . . . . ? C11 P1 P2 N1 71.65(14) . . . . ? Fe1 P1 P2 N1 -177.80(11) . . . . ? N1 P1 P2 C29 74.43(15) . . . . ? C17 P1 P2 C29 1.02(15) . . . . ? C11 P1 P2 C29 146.08(14) . . . . ? Fe1 P1 P2 C29 -103.37(10) . . . . ? N1 P1 P2 C23 -73.01(15) . . . . ? C17 P1 P2 C23 -146.43(14) . . . . ? C11 P1 P2 C23 -1.36(15) . . . . ? Fe1 P1 P2 C23 109.18(10) . . . . ? N1 P1 P2 Fe1 177.80(11) . . . . ? C17 P1 P2 Fe1 104.39(10) . . . . ? C11 P1 P2 Fe1 -110.55(10) . . . . ? C1 Fe1 S1 C5 -39.13(15) . . . . ? P1 Fe1 S1 C5 161.25(13) . . . . ? P2 Fe1 S1 C5 -145.32(12) . . . . ? S2 Fe1 S1 C5 59.48(12) . . . . ? Fe2 Fe1 S1 C5 107.49(12) . . . . ? C1 Fe1 S1 Fe2 -146.62(8) . . . . ? P1 Fe1 S1 Fe2 53.76(7) . . . . ? P2 Fe1 S1 Fe2 107.19(2) . . . . ? S2 Fe1 S1 Fe2 -48.01(2) . . . . ? C3 Fe2 S1 C5 -132.2(2) . . . . ? C2 Fe2 S1 C5 44.36(13) . . . . ? C4 Fe2 S1 C5 139.14(13) . . . . ? S2 Fe2 S1 C5 -56.66(11) . . . . ? Fe1 Fe2 S1 C5 -103.91(11) . . . . ? C3 Fe2 S1 Fe1 -28.3(2) . . . . ? C2 Fe2 S1 Fe1 148.27(8) . . . . ? C4 Fe2 S1 Fe1 -116.95(8) . . . . ? S2 Fe2 S1 Fe1 47.24(2) . . . . ? C1 Fe1 S2 C7 39.98(13) . . . . ? P1 Fe1 S2 C7 145.05(10) . . . . ? P2 Fe1 S2 C7 -154.08(11) . . . . ? S1 Fe1 S2 C7 -56.96(10) . . . . ? Fe2 Fe1 S2 C7 -105.13(10) . . . . ? C1 Fe1 S2 Fe2 145.11(8) . . . . ? P1 Fe1 S2 Fe2 -109.82(2) . . . . ? P2 Fe1 S2 Fe2 -48.95(7) . . . . ? S1 Fe1 S2 Fe2 48.17(2) . . . . ? C3 Fe2 S2 C7 -143.63(14) . . . . ? C2 Fe2 S2 C7 -46.60(14) . . . . ? C4 Fe2 S2 C7 132.6(3) . . . . ? S1 Fe2 S2 C7 58.02(11) . . . . ? Fe1 Fe2 S2 C7 105.24(11) . . . . ? C3 Fe2 S2 Fe1 111.13(9) . . . . ? C2 Fe2 S2 Fe1 -151.83(8) . . . . ? C4 Fe2 S2 Fe1 27.3(3) . . . . ? S1 Fe2 S2 Fe1 -47.22(2) . . . . ? C17 P1 N1 C8 -72.7(2) . . . . ? C11 P1 N1 C8 33.9(2) . . . . ? Fe1 P1 N1 C8 162.2(2) . . . . ? P2 P1 N1 C8 160.4(3) . . . . ? C17 P1 N1 P2 126.96(11) . . . . ? C11 P1 N1 P2 -126.46(11) . . . . ? Fe1 P1 N1 P2 1.79(9) . . . . ? C29 P2 N1 C8 74.6(2) . . . . ? C23 P2 N1 C8 -32.3(3) . . . . ? Fe1 P2 N1 C8 -160.3(2) . . . . ? P1 P2 N1 C8 -158.5(3) . . . . ? C29 P2 N1 P1 -126.85(11) . . . . ? C23 P2 N1 P1 126.21(11) . . . . ? Fe1 P2 N1 P1 -1.79(9) . . . . ? P1 Fe1 C1 O1 -149.4(17) . . . . ? P2 Fe1 C1 O1 136.7(17) . . . . ? S2 Fe1 C1 O1 -49.4(17) . . . . ? S1 Fe1 C1 O1 38.4(17) . . . . ? Fe2 Fe1 C1 O1 -4.5(18) . . . . ? C3 Fe2 C2 O2 -53(7) . . . . ? C4 Fe2 C2 O2 37(7) . . . . ? S2 Fe2 C2 O2 -143(7) . . . . ? S1 Fe2 C2 O2 129(7) . . . . ? Fe1 Fe2 C2 O2 176(100) . . . . ? C2 Fe2 C3 O3 34(3) . . . . ? C4 Fe2 C3 O3 -61(3) . . . . ? S2 Fe2 C3 O3 135(3) . . . . ? S1 Fe2 C3 O3 -150(3) . . . . ? Fe1 Fe2 C3 O3 -173(3) . . . . ? C3 Fe2 C4 O4 65.6(19) . . . . ? C2 Fe2 C4 O4 -31.4(19) . . . . ? S2 Fe2 C4 O4 149.4(17) . . . . ? S1 Fe2 C4 O4 -136.8(19) . . . . ? Fe1 Fe2 C4 O4 172.8(19) . . . . ? Fe1 S1 C5 C6 -66.2(3) . . . . ? Fe2 S1 C5 C6 11.1(3) . . . . ? S1 C5 C6 C7 54.7(4) . . . . ? C5 C6 C7 S2 -51.2(4) . . . . ? Fe1 S2 C7 C6 59.1(3) . . . . ? Fe2 S2 C7 C6 -18.1(3) . . . . ? P1 N1 C8 C10 141.7(3) . . . . ? P2 N1 C8 C10 -65.0(4) . . . . ? P1 N1 C8 C9 -83.8(3) . . . . ? P2 N1 C8 C9 69.5(3) . . . . ? N1 P1 C11 C16 87.1(2) . . . . ? C17 P1 C11 C16 -160.8(2) . . . . ? Fe1 P1 C11 C16 -21.0(2) . . . . ? P2 P1 C11 C16 46.7(2) . . . . ? N1 P1 C11 C12 -87.6(2) . . . . ? C17 P1 C11 C12 24.5(2) . . . . ? Fe1 P1 C11 C12 164.28(18) . . . . ? P2 P1 C11 C12 -127.98(19) . . . . ? C16 C11 C12 C13 -0.5(4) . . . . ? P1 C11 C12 C13 174.3(2) . . . . ? C11 C12 C13 C14 0.5(5) . . . . ? C12 C13 C14 C15 -0.4(5) . . . . ? C13 C14 C15 C16 0.2(5) . . . . ? C14 C15 C16 C11 -0.1(4) . . . . ? C12 C11 C16 C15 0.3(4) . . . . ? P1 C11 C16 C15 -174.6(2) . . . . ? N1 P1 C17 C18 -6.1(3) . . . . ? C11 P1 C17 C18 -116.1(2) . . . . ? Fe1 P1 C17 C18 102.2(2) . . . . ? P2 P1 C17 C18 35.5(3) . . . . ? N1 P1 C17 C22 174.62(18) . . . . ? C11 P1 C17 C22 64.6(2) . . . . ? Fe1 P1 C17 C22 -77.1(2) . . . . ? P2 P1 C17 C22 -143.81(15) . . . . ? C22 C17 C18 C19 -0.4(4) . . . . ? P1 C17 C18 C19 -179.7(3) . . . . ? C17 C18 C19 C20 0.3(5) . . . . ? C18 C19 C20 C21 -0.3(5) . . . . ? C19 C20 C21 C22 0.3(4) . . . . ? C20 C21 C22 C17 -0.4(4) . . . . ? C18 C17 C22 C21 0.4(4) . . . . ? P1 C17 C22 C21 179.74(18) . . . . ? N1 P2 C23 C28 -95.4(2) . . . . ? C29 P2 C23 C28 151.0(2) . . . . ? Fe1 P2 C23 C28 13.4(2) . . . . ? P1 P2 C23 C28 -54.3(2) . . . . ? N1 P2 C23 C24 81.1(2) . . . . ? C29 P2 C23 C24 -32.5(2) . . . . ? Fe1 P2 C23 C24 -170.09(17) . . . . ? P1 P2 C23 C24 122.15(19) . . . . ? C28 C23 C24 C25 1.6(4) . . . . ? P2 C23 C24 C25 -174.9(2) . . . . ? C23 C24 C25 C26 -1.3(4) . . . . ? C24 C25 C26 C27 0.2(4) . . . . ? C25 C26 C27 C28 0.6(5) . . . . ? C26 C27 C28 C23 -0.2(4) . . . . ? C24 C23 C28 C27 -0.9(4) . . . . ? P2 C23 C28 C27 175.7(2) . . . . ? N1 P2 C29 C34 15.7(2) . . . . ? C23 P2 C29 C34 127.5(2) . . . . ? Fe1 P2 C29 C34 -93.0(2) . . . . ? P1 P2 C29 C34 -26.4(3) . . . . ? N1 P2 C29 C30 -167.48(19) . . . . ? C23 P2 C29 C30 -55.8(2) . . . . ? Fe1 P2 C29 C30 83.7(2) . . . . ? P1 P2 C29 C30 150.40(16) . . . . ? C34 C29 C30 C31 -1.3(4) . . . . ? P2 C29 C30 C31 -178.2(2) . . . . ? C29 C30 C31 C32 -0.5(4) . . . . ? C30 C31 C32 C33 1.4(4) . . . . ? C31 C32 C33 C34 -0.6(5) . . . . ? C30 C29 C34 C33 2.2(4) . . . . ? P2 C29 C34 C33 178.9(2) . . . . ? C32 C33 C34 C29 -1.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.451 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.099 #===END data_str0540 _database_code_depnum_ccdc_archive 'CCDC 639866' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H33 Fe2 N O4 P2 S2' _chemical_formula_weight 757.37 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' Fe Fe 0.3463 0.8444 '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 9.7227(10) _cell_length_b 10.3859(11) _cell_length_c 18.5263(19) _cell_angle_alpha 84.913(2) _cell_angle_beta 80.645(2) _cell_angle_gamma 63.569(2) _cell_volume 1652.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 1.141 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7714 _exptl_absorpt_correction_T_max 0.8566 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14333 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 28.31 _reflns_number_total 7563 _reflns_number_gt 6917 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0557P)^2^+2.8501P] 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 7563 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.1095 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.51744(4) 0.36202(3) 0.272386(17) 0.01089(9) Uani 1 1 d . . . Fe2 Fe 0.44438(4) 0.27286(4) 0.403438(18) 0.01320(9) Uani 1 1 d . . . P1 P 0.77021(7) 0.29495(6) 0.24932(3) 0.01170(12) Uani 1 1 d . . . P2 P 0.62387(7) 0.17397(6) 0.19995(3) 0.01232(13) Uani 1 1 d . . . S1 S 0.29936(7) 0.34150(6) 0.31094(3) 0.01587(13) Uani 1 1 d . . . S2 S 0.47348(7) 0.47571(6) 0.37575(3) 0.01588(13) Uani 1 1 d . . . N1 N 0.8103(2) 0.1518(2) 0.19667(11) 0.0148(4) Uani 1 1 d . . . O1 O 0.3750(2) 0.6158(2) 0.18172(10) 0.0232(4) Uani 1 1 d . . . O2 O 0.2227(2) 0.3484(2) 0.53867(11) 0.0288(4) Uani 1 1 d . . . O3 O 0.7204(3) 0.1534(3) 0.47764(13) 0.0345(5) Uani 1 1 d . . . O4 O 0.4666(3) -0.0185(2) 0.40865(11) 0.0270(4) Uani 1 1 d . . . C1 C 0.4404(3) 0.5110(3) 0.21455(13) 0.0146(4) Uani 1 1 d . . . C2 C 0.3075(3) 0.3215(3) 0.48557(13) 0.0178(5) Uani 1 1 d . . . C3 C 0.6167(3) 0.2016(3) 0.44650(14) 0.0212(5) Uani 1 1 d . . . C4 C 0.4596(3) 0.0941(3) 0.40197(13) 0.0174(5) Uani 1 1 d . . . C5 C 0.1388(3) 0.5205(3) 0.3247(2) 0.0318(7) Uani 1 1 d . . . H5A H 0.1364 0.5759 0.2782 0.038 Uiso 1 1 calc R . . H5B H 0.0411 0.5098 0.3345 0.038 Uiso 1 1 calc R . . C6 C 0.1392(4) 0.6052(4) 0.3825(2) 0.0379(7) Uani 1 1 d . . . H6A H 0.1224 0.5580 0.4296 0.045 Uiso 1 1 calc R . . H6B H 0.0484 0.7002 0.3811 0.045 Uiso 1 1 calc R . . C7 C 0.2825(3) 0.6322(3) 0.38309(17) 0.0287(6) Uani 1 1 d . . . H7A H 0.2677 0.6816 0.4290 0.034 Uiso 1 1 calc R . . H7B H 0.2849 0.6996 0.3422 0.034 Uiso 1 1 calc R . . C8 C 0.9547(3) 0.0757(3) 0.14429(15) 0.0287(6) Uani 1 1 d . . . H8A H 1.0362 0.0888 0.1651 0.034 Uiso 1 1 calc R . . C9 C 0.9512(3) 0.1483(3) 0.06958(14) 0.0222(5) Uani 1 1 d . . . H9A H 1.0488 0.0939 0.0381 0.033 Uiso 1 1 calc R . . H9B H 0.9381 0.2464 0.0746 0.033 Uiso 1 1 calc R . . H9C H 0.8645 0.1517 0.0476 0.033 Uiso 1 1 calc R . . C10 C 1.0131(4) -0.0809(4) 0.1419(2) 0.0435(8) Uani 1 1 d . . . H10A H 1.0128 -0.1205 0.1919 0.065 Uiso 1 1 calc R . . H10B H 1.1192 -0.1229 0.1160 0.065 Uiso 1 1 calc R . . H10C H 0.9464 -0.1038 0.1163 0.065 Uiso 1 1 calc R . . C11 C 0.8607(3) 0.3998(3) 0.19396(13) 0.0152(4) Uani 1 1 d . . . C12 C 1.0157(3) 0.3696(3) 0.19598(15) 0.0228(5) Uani 1 1 d . . . H12A H 1.0729 0.2993 0.2297 0.027 Uiso 1 1 calc R . . C13 C 1.0862(3) 0.4415(4) 0.14912(16) 0.0307(7) Uani 1 1 d . . . H13A H 1.1915 0.4194 0.1507 0.037 Uiso 1 1 calc R . . C14 C 1.0040(4) 0.5451(4) 0.10003(16) 0.0303(6) Uani 1 1 d . . . H14A H 1.0526 0.5944 0.0683 0.036 Uiso 1 1 calc R . . C15 C 0.8503(4) 0.5766(3) 0.09744(16) 0.0276(6) Uani 1 1 d . . . H15A H 0.7934 0.6473 0.0638 0.033 Uiso 1 1 calc R . . C16 C 0.7800(3) 0.5044(3) 0.14412(14) 0.0208(5) Uani 1 1 d . . . H16A H 0.6747 0.5266 0.1421 0.025 Uiso 1 1 calc R . . C17 C 0.8908(3) 0.2296(3) 0.32218(13) 0.0146(4) Uani 1 1 d . . . C18 C 0.9848(4) 0.0857(3) 0.33491(17) 0.0285(6) Uani 1 1 d . . . H18A H 0.9889 0.0149 0.3044 0.034 Uiso 1 1 calc R . . C19 C 1.0729(4) 0.0444(3) 0.39202(18) 0.0335(7) Uani 1 1 d . . . H19A H 1.1375 -0.0546 0.4002 0.040 Uiso 1 1 calc R . . C20 C 1.0675(3) 0.1466(3) 0.43731(15) 0.0226(5) Uani 1 1 d . . . H20A H 1.1277 0.1180 0.4765 0.027 Uiso 1 1 calc R . . C21 C 0.9739(3) 0.2904(3) 0.42483(13) 0.0171(5) Uani 1 1 d . . . H21A H 0.9701 0.3608 0.4555 0.020 Uiso 1 1 calc R . . C22 C 0.8852(3) 0.3326(3) 0.36783(13) 0.0147(4) Uani 1 1 d . . . H22A H 0.8207 0.4317 0.3598 0.018 Uiso 1 1 calc R . . C23 C 0.5890(3) 0.1809(3) 0.10479(13) 0.0155(5) Uani 1 1 d . . . C24 C 0.6396(3) 0.0560(3) 0.06480(14) 0.0195(5) Uani 1 1 d . . . H24A H 0.6860 -0.0355 0.0881 0.023 Uiso 1 1 calc R . . C25 C 0.6225(3) 0.0646(3) -0.00891(14) 0.0220(5) Uani 1 1 d . . . H25A H 0.6591 -0.0210 -0.0357 0.026 Uiso 1 1 calc R . . C26 C 0.5525(4) 0.1969(3) -0.04319(14) 0.0258(6) Uani 1 1 d . . . H26A H 0.5407 0.2025 -0.0934 0.031 Uiso 1 1 calc R . . C27 C 0.4997(4) 0.3210(3) -0.00392(15) 0.0278(6) Uani 1 1 d . . . H27A H 0.4507 0.4121 -0.0273 0.033 Uiso 1 1 calc R . . C28 C 0.5178(3) 0.3137(3) 0.06962(14) 0.0211(5) Uani 1 1 d . . . H28A H 0.4813 0.3998 0.0960 0.025 Uiso 1 1 calc R . . C29 C 0.6148(3) 0.0063(3) 0.23047(13) 0.0160(5) Uani 1 1 d . . . C30 C 0.4810(3) -0.0069(3) 0.22290(14) 0.0204(5) Uani 1 1 d . . . H30A H 0.4001 0.0695 0.2011 0.024 Uiso 1 1 calc R . . C31 C 0.4654(4) -0.1306(3) 0.24701(15) 0.0250(6) Uani 1 1 d . . . H31A H 0.3738 -0.1386 0.2420 0.030 Uiso 1 1 calc R . . C32 C 0.5835(4) -0.2424(3) 0.27833(16) 0.0268(6) Uani 1 1 d . . . H32A H 0.5741 -0.3282 0.2939 0.032 Uiso 1 1 calc R . . C33 C 0.7155(3) -0.2293(3) 0.28700(17) 0.0299(6) Uani 1 1 d . . . H33A H 0.7961 -0.3057 0.3089 0.036 Uiso 1 1 calc R . . C34 C 0.7304(3) -0.1047(3) 0.26377(15) 0.0235(5) Uani 1 1 d . . . H34A H 0.8203 -0.0956 0.2707 0.028 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 0.01041(16) 0.01068(16) 0.01018(16) 0.00089(11) -0.00100(12) -0.00368(13) Fe2 0.01536(17) 0.01292(17) 0.01098(17) 0.00079(12) -0.00041(12) -0.00654(14) P1 0.0107(3) 0.0125(3) 0.0105(3) -0.0007(2) -0.0011(2) -0.0038(2) P2 0.0139(3) 0.0121(3) 0.0110(3) 0.0002(2) -0.0024(2) -0.0055(2) S1 0.0113(3) 0.0157(3) 0.0191(3) 0.0035(2) -0.0024(2) -0.0051(2) S2 0.0195(3) 0.0136(3) 0.0139(3) -0.0026(2) 0.0025(2) -0.0079(2) N1 0.0143(9) 0.0142(9) 0.0134(9) -0.0031(7) -0.0002(7) -0.0041(8) O1 0.0250(10) 0.0168(9) 0.0234(10) 0.0056(7) -0.0064(8) -0.0054(8) O2 0.0281(11) 0.0318(11) 0.0188(10) -0.0004(8) 0.0038(8) -0.0087(9) O3 0.0322(11) 0.0435(13) 0.0381(12) 0.0191(10) -0.0175(10) -0.0251(10) O4 0.0393(12) 0.0197(10) 0.0230(10) 0.0003(7) 0.0004(8) -0.0154(9) C1 0.0139(11) 0.0144(11) 0.0143(11) -0.0013(8) -0.0014(8) -0.0053(9) C2 0.0199(12) 0.0164(11) 0.0152(11) 0.0009(9) -0.0022(9) -0.0067(10) C3 0.0258(13) 0.0239(13) 0.0191(12) 0.0058(10) -0.0045(10) -0.0163(11) C4 0.0187(12) 0.0198(12) 0.0127(11) -0.0005(9) -0.0005(9) -0.0080(10) C5 0.0112(12) 0.0193(13) 0.057(2) 0.0061(13) -0.0018(12) -0.0016(10) C6 0.0307(16) 0.0303(16) 0.0410(18) -0.0075(13) -0.0082(14) -0.0005(13) C7 0.0261(14) 0.0122(12) 0.0383(16) -0.0062(11) 0.0126(12) -0.0046(11) C8 0.0229(14) 0.0267(14) 0.0192(13) -0.0046(10) 0.0059(11) 0.0023(11) C9 0.0213(13) 0.0253(13) 0.0185(12) -0.0065(10) 0.0059(10) -0.0108(11) C10 0.0384(19) 0.0377(19) 0.044(2) -0.0084(15) 0.0050(15) -0.0095(16) C11 0.0164(11) 0.0194(12) 0.0114(10) -0.0013(8) 0.0000(8) -0.0096(10) C12 0.0197(12) 0.0322(15) 0.0191(12) 0.0028(10) -0.0037(10) -0.0139(11) C13 0.0225(14) 0.0492(19) 0.0270(15) 0.0048(13) -0.0026(11) -0.0229(14) C14 0.0332(16) 0.0440(18) 0.0221(14) 0.0063(12) 0.0002(12) -0.0270(14) C15 0.0293(15) 0.0323(15) 0.0216(13) 0.0075(11) -0.0032(11) -0.0153(13) C16 0.0179(12) 0.0252(13) 0.0195(12) 0.0036(10) -0.0032(10) -0.0100(10) C17 0.0140(11) 0.0164(11) 0.0126(10) 0.0001(8) -0.0029(8) -0.0056(9) C18 0.0346(16) 0.0159(13) 0.0338(16) -0.0031(11) -0.0188(13) -0.0049(12) C19 0.0409(18) 0.0169(13) 0.0403(17) 0.0035(12) -0.0268(14) -0.0042(12) C20 0.0238(13) 0.0243(13) 0.0210(13) 0.0035(10) -0.0107(10) -0.0099(11) C21 0.0176(11) 0.0217(12) 0.0147(11) -0.0018(9) -0.0013(9) -0.0112(10) C22 0.0143(11) 0.0141(11) 0.0142(11) -0.0004(8) 0.0003(8) -0.0055(9) C23 0.0168(11) 0.0216(12) 0.0109(10) 0.0000(9) -0.0027(8) -0.0107(10) C24 0.0210(12) 0.0213(12) 0.0172(12) -0.0012(9) -0.0029(9) -0.0100(10) C25 0.0221(13) 0.0297(14) 0.0181(12) -0.0053(10) -0.0021(10) -0.0141(11) C26 0.0349(15) 0.0378(16) 0.0135(12) 0.0025(10) -0.0059(11) -0.0233(13) C27 0.0422(17) 0.0265(14) 0.0185(13) 0.0067(10) -0.0123(12) -0.0171(13) C28 0.0294(14) 0.0197(12) 0.0168(12) 0.0013(9) -0.0066(10) -0.0123(11) C29 0.0216(12) 0.0123(11) 0.0148(11) -0.0006(8) 0.0000(9) -0.0089(9) C30 0.0267(13) 0.0200(12) 0.0181(12) 0.0015(9) -0.0063(10) -0.0129(11) C31 0.0341(15) 0.0260(14) 0.0216(13) -0.0048(10) 0.0005(11) -0.0197(12) C32 0.0348(15) 0.0167(12) 0.0268(14) -0.0011(10) 0.0076(12) -0.0133(12) C33 0.0254(14) 0.0163(13) 0.0377(16) 0.0094(11) 0.0002(12) -0.0033(11) C34 0.0177(12) 0.0196(13) 0.0293(14) 0.0047(10) 0.0000(10) -0.0067(10) _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 C1 1.743(2) . ? Fe1 P1 2.2124(7) . ? Fe1 P2 2.2137(7) . ? Fe1 S2 2.2203(7) . ? Fe1 S1 2.2214(7) . ? Fe1 Fe2 2.6236(5) . ? Fe2 C3 1.793(3) . ? Fe2 C2 1.794(3) . ? Fe2 C4 1.798(3) . ? Fe2 S2 2.2524(7) . ? Fe2 S1 2.2598(7) . ? P1 N1 1.712(2) . ? P1 C17 1.817(2) . ? P1 C11 1.837(2) . ? P1 P2 2.5803(8) . ? P2 N1 1.714(2) . ? P2 C29 1.818(2) . ? P2 C23 1.838(2) . ? S1 C5 1.825(3) . ? S2 C7 1.838(3) . ? N1 C8 1.498(3) . ? O1 C1 1.163(3) . ? O2 C2 1.143(3) . ? O3 C3 1.136(3) . ? O4 C4 1.138(3) . ? C5 C6 1.446(5) . ? C6 C7 1.540(5) . ? C8 C10 1.466(5) . ? C8 C9 1.514(4) . ? C11 C16 1.395(3) . ? C11 C12 1.401(3) . ? C12 C13 1.389(4) . ? C13 C14 1.386(4) . ? C14 C15 1.389(4) . ? C15 C16 1.388(4) . ? C17 C18 1.384(4) . ? C17 C22 1.399(3) . ? C18 C19 1.388(4) . ? C19 C20 1.389(4) . ? C20 C21 1.382(4) . ? C21 C22 1.388(3) . ? C23 C28 1.394(3) . ? C23 C24 1.399(3) . ? C24 C25 1.393(4) . ? C25 C26 1.381(4) . ? C26 C27 1.382(4) . ? C27 C28 1.393(4) . ? C29 C34 1.386(4) . ? C29 C30 1.397(4) . ? C30 C31 1.388(4) . ? C31 C32 1.383(4) . ? C32 C33 1.385(4) . ? C33 C34 1.388(4) . ? 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 C1 Fe1 P1 103.57(8) . . ? C1 Fe1 P2 105.18(8) . . ? P1 Fe1 P2 71.32(2) . . ? C1 Fe1 S2 98.94(8) . . ? P1 Fe1 S2 97.43(2) . . ? P2 Fe1 S2 155.14(3) . . ? C1 Fe1 S1 97.35(8) . . ? P1 Fe1 S1 157.69(3) . . ? P2 Fe1 S1 95.92(3) . . ? S2 Fe1 S1 86.77(3) . . ? C1 Fe1 Fe2 138.66(8) . . ? P1 Fe1 Fe2 110.44(2) . . ? P2 Fe1 Fe2 107.44(2) . . ? S2 Fe1 Fe2 54.656(19) . . ? S1 Fe1 Fe2 54.848(18) . . ? C3 Fe2 C2 97.06(12) . . ? C3 Fe2 C4 89.11(12) . . ? C2 Fe2 C4 94.50(11) . . ? C3 Fe2 S2 89.11(8) . . ? C2 Fe2 S2 101.91(8) . . ? C4 Fe2 S2 163.59(8) . . ? C3 Fe2 S1 157.61(9) . . ? C2 Fe2 S1 105.29(8) . . ? C4 Fe2 S1 90.40(8) . . ? S2 Fe2 S1 85.09(2) . . ? C3 Fe2 Fe1 106.30(8) . . ? C2 Fe2 Fe1 144.71(8) . . ? C4 Fe2 Fe1 111.62(8) . . ? S2 Fe2 Fe1 53.519(18) . . ? S1 Fe2 Fe1 53.488(18) . . ? N1 P1 C17 108.07(11) . . ? N1 P1 C11 105.35(10) . . ? C17 P1 C11 100.33(11) . . ? N1 P1 Fe1 95.50(7) . . ? C17 P1 Fe1 121.02(8) . . ? C11 P1 Fe1 124.68(8) . . ? N1 P1 P2 41.16(7) . . ? C17 P1 P2 127.57(8) . . ? C11 P1 P2 125.21(8) . . ? Fe1 P1 P2 54.36(2) . . ? N1 P2 C29 109.20(11) . . ? N1 P2 C23 106.81(10) . . ? C29 P2 C23 99.69(11) . . ? N1 P2 Fe1 95.40(7) . . ? C29 P2 Fe1 120.60(8) . . ? C23 P2 Fe1 124.02(8) . . ? N1 P2 P1 41.10(7) . . ? C29 P2 P1 128.33(8) . . ? C23 P2 P1 126.14(8) . . ? Fe1 P2 P1 54.32(2) . . ? C5 S1 Fe1 109.21(10) . . ? C5 S1 Fe2 111.89(12) . . ? Fe1 S1 Fe2 71.66(2) . . ? C7 S2 Fe1 109.92(11) . . ? C7 S2 Fe2 109.84(9) . . ? Fe1 S2 Fe2 71.83(2) . . ? C8 N1 P1 126.24(19) . . ? C8 N1 P2 132.32(19) . . ? P1 N1 P2 97.74(10) . . ? O1 C1 Fe1 172.6(2) . . ? O2 C2 Fe2 177.9(2) . . ? O3 C3 Fe2 175.3(2) . . ? O4 C4 Fe2 173.0(2) . . ? C6 C5 S1 117.5(2) . . ? C5 C6 C7 119.0(3) . . ? C6 C7 S2 117.8(2) . . ? C10 C8 N1 115.7(3) . . ? C10 C8 C9 113.9(3) . . ? N1 C8 C9 113.5(2) . . ? C16 C11 C12 118.1(2) . . ? C16 C11 P1 120.32(18) . . ? C12 C11 P1 121.3(2) . . ? C13 C12 C11 120.5(3) . . ? C14 C13 C12 120.5(3) . . ? C13 C14 C15 119.7(3) . . ? C16 C15 C14 119.8(3) . . ? C15 C16 C11 121.4(2) . . ? C18 C17 C22 119.2(2) . . ? C18 C17 P1 123.82(19) . . ? C22 C17 P1 116.99(18) . . ? C17 C18 C19 120.4(3) . . ? C18 C19 C20 120.5(3) . . ? C21 C20 C19 119.4(2) . . ? C20 C21 C22 120.5(2) . . ? C21 C22 C17 120.1(2) . . ? C28 C23 C24 118.5(2) . . ? C28 C23 P2 119.63(19) . . ? C24 C23 P2 121.82(19) . . ? C25 C24 C23 120.6(2) . . ? C26 C25 C24 120.3(2) . . ? C25 C26 C27 119.6(2) . . ? C26 C27 C28 120.6(3) . . ? C27 C28 C23 120.4(2) . . ? C34 C29 C30 119.1(2) . . ? C34 C29 P2 123.0(2) . . ? C30 C29 P2 117.81(19) . . ? C31 C30 C29 120.5(3) . . ? C32 C31 C30 119.9(3) . . ? C31 C32 C33 119.9(3) . . ? C32 C33 C34 120.3(3) . . ? C29 C34 C33 120.3(3) . . ? 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 C1 Fe1 Fe2 C3 -135.15(15) . . . . ? P1 Fe1 Fe2 C3 8.22(9) . . . . ? P2 Fe1 Fe2 C3 84.26(9) . . . . ? S2 Fe1 Fe2 C3 -76.33(9) . . . . ? S1 Fe1 Fe2 C3 169.15(9) . . . . ? C1 Fe1 Fe2 C2 -5.74(19) . . . . ? P1 Fe1 Fe2 C2 137.64(15) . . . . ? P2 Fe1 Fe2 C2 -146.32(15) . . . . ? S2 Fe1 Fe2 C2 53.09(15) . . . . ? S1 Fe1 Fe2 C2 -61.43(15) . . . . ? C1 Fe1 Fe2 C4 129.20(15) . . . . ? P1 Fe1 Fe2 C4 -87.43(9) . . . . ? P2 Fe1 Fe2 C4 -11.39(9) . . . . ? S2 Fe1 Fe2 C4 -171.98(9) . . . . ? S1 Fe1 Fe2 C4 73.50(9) . . . . ? C1 Fe1 Fe2 S2 -58.82(12) . . . . ? P1 Fe1 Fe2 S2 84.55(3) . . . . ? P2 Fe1 Fe2 S2 160.59(3) . . . . ? S1 Fe1 Fe2 S2 -114.52(3) . . . . ? C1 Fe1 Fe2 S1 55.70(12) . . . . ? P1 Fe1 Fe2 S1 -160.93(3) . . . . ? P2 Fe1 Fe2 S1 -84.89(3) . . . . ? S2 Fe1 Fe2 S1 114.52(3) . . . . ? C1 Fe1 P1 N1 -103.15(11) . . . . ? P2 Fe1 P1 N1 -1.45(7) . . . . ? S2 Fe1 P1 N1 155.74(7) . . . . ? S1 Fe1 P1 N1 56.04(10) . . . . ? Fe2 Fe1 P1 N1 100.76(7) . . . . ? C1 Fe1 P1 C17 141.92(12) . . . . ? P2 Fe1 P1 C17 -116.38(10) . . . . ? S2 Fe1 P1 C17 40.81(10) . . . . ? S1 Fe1 P1 C17 -58.89(12) . . . . ? Fe2 Fe1 P1 C17 -14.16(10) . . . . ? C1 Fe1 P1 C11 9.81(13) . . . . ? P2 Fe1 P1 C11 111.51(10) . . . . ? S2 Fe1 P1 C11 -91.30(10) . . . . ? S1 Fe1 P1 C11 169.00(10) . . . . ? Fe2 Fe1 P1 C11 -146.28(9) . . . . ? C1 Fe1 P1 P2 -101.70(8) . . . . ? S2 Fe1 P1 P2 157.19(3) . . . . ? S1 Fe1 P1 P2 57.49(7) . . . . ? Fe2 Fe1 P1 P2 102.22(2) . . . . ? C1 Fe1 P2 N1 100.94(11) . . . . ? P1 Fe1 P2 N1 1.45(7) . . . . ? S2 Fe1 P2 N1 -64.67(10) . . . . ? S1 Fe1 P2 N1 -159.77(7) . . . . ? Fe2 Fe1 P2 N1 -104.82(7) . . . . ? C1 Fe1 P2 C29 -142.98(13) . . . . ? P1 Fe1 P2 C29 117.54(10) . . . . ? S2 Fe1 P2 C29 51.42(12) . . . . ? S1 Fe1 P2 C29 -43.69(10) . . . . ? Fe2 Fe1 P2 C29 11.27(10) . . . . ? C1 Fe1 P2 C23 -13.54(13) . . . . ? P1 Fe1 P2 C23 -113.03(10) . . . . ? S2 Fe1 P2 C23 -179.15(10) . . . . ? S1 Fe1 P2 C23 85.74(10) . . . . ? Fe2 Fe1 P2 C23 140.70(9) . . . . ? C1 Fe1 P2 P1 99.49(8) . . . . ? S2 Fe1 P2 P1 -66.12(6) . . . . ? S1 Fe1 P2 P1 -161.23(3) . . . . ? Fe2 Fe1 P2 P1 -106.27(2) . . . . ? C17 P1 P2 N1 -73.41(14) . . . . ? C11 P1 P2 N1 71.65(14) . . . . ? Fe1 P1 P2 N1 -177.80(11) . . . . ? N1 P1 P2 C29 74.43(15) . . . . ? C17 P1 P2 C29 1.02(15) . . . . ? C11 P1 P2 C29 146.08(14) . . . . ? Fe1 P1 P2 C29 -103.37(10) . . . . ? N1 P1 P2 C23 -73.01(15) . . . . ? C17 P1 P2 C23 -146.43(14) . . . . ? C11 P1 P2 C23 -1.36(15) . . . . ? Fe1 P1 P2 C23 109.18(10) . . . . ? N1 P1 P2 Fe1 177.80(11) . . . . ? C17 P1 P2 Fe1 104.39(10) . . . . ? C11 P1 P2 Fe1 -110.55(10) . . . . ? C1 Fe1 S1 C5 -39.13(15) . . . . ? P1 Fe1 S1 C5 161.25(13) . . . . ? P2 Fe1 S1 C5 -145.32(12) . . . . ? S2 Fe1 S1 C5 59.48(12) . . . . ? Fe2 Fe1 S1 C5 107.49(12) . . . . ? C1 Fe1 S1 Fe2 -146.62(8) . . . . ? P1 Fe1 S1 Fe2 53.76(7) . . . . ? P2 Fe1 S1 Fe2 107.19(2) . . . . ? S2 Fe1 S1 Fe2 -48.01(2) . . . . ? C3 Fe2 S1 C5 -132.2(2) . . . . ? C2 Fe2 S1 C5 44.36(13) . . . . ? C4 Fe2 S1 C5 139.14(13) . . . . ? S2 Fe2 S1 C5 -56.66(11) . . . . ? Fe1 Fe2 S1 C5 -103.91(11) . . . . ? C3 Fe2 S1 Fe1 -28.3(2) . . . . ? C2 Fe2 S1 Fe1 148.27(8) . . . . ? C4 Fe2 S1 Fe1 -116.95(8) . . . . ? S2 Fe2 S1 Fe1 47.24(2) . . . . ? C1 Fe1 S2 C7 39.98(13) . . . . ? P1 Fe1 S2 C7 145.05(10) . . . . ? P2 Fe1 S2 C7 -154.08(11) . . . . ? S1 Fe1 S2 C7 -56.96(10) . . . . ? Fe2 Fe1 S2 C7 -105.13(10) . . . . ? C1 Fe1 S2 Fe2 145.11(8) . . . . ? P1 Fe1 S2 Fe2 -109.82(2) . . . . ? P2 Fe1 S2 Fe2 -48.95(7) . . . . ? S1 Fe1 S2 Fe2 48.17(2) . . . . ? C3 Fe2 S2 C7 -143.63(14) . . . . ? C2 Fe2 S2 C7 -46.60(14) . . . . ? C4 Fe2 S2 C7 132.6(3) . . . . ? S1 Fe2 S2 C7 58.02(11) . . . . ? Fe1 Fe2 S2 C7 105.24(11) . . . . ? C3 Fe2 S2 Fe1 111.13(9) . . . . ? C2 Fe2 S2 Fe1 -151.83(8) . . . . ? C4 Fe2 S2 Fe1 27.3(3) . . . . ? S1 Fe2 S2 Fe1 -47.22(2) . . . . ? C17 P1 N1 C8 -72.7(2) . . . . ? C11 P1 N1 C8 33.9(2) . . . . ? Fe1 P1 N1 C8 162.2(2) . . . . ? P2 P1 N1 C8 160.4(3) . . . . ? C17 P1 N1 P2 126.96(11) . . . . ? C11 P1 N1 P2 -126.46(11) . . . . ? Fe1 P1 N1 P2 1.79(9) . . . . ? C29 P2 N1 C8 74.6(2) . . . . ? C23 P2 N1 C8 -32.3(3) . . . . ? Fe1 P2 N1 C8 -160.3(2) . . . . ? P1 P2 N1 C8 -158.5(3) . . . . ? C29 P2 N1 P1 -126.85(11) . . . . ? C23 P2 N1 P1 126.21(11) . . . . ? Fe1 P2 N1 P1 -1.79(9) . . . . ? P1 Fe1 C1 O1 -149.4(17) . . . . ? P2 Fe1 C1 O1 136.7(17) . . . . ? S2 Fe1 C1 O1 -49.4(17) . . . . ? S1 Fe1 C1 O1 38.4(17) . . . . ? Fe2 Fe1 C1 O1 -4.5(18) . . . . ? C3 Fe2 C2 O2 -53(7) . . . . ? C4 Fe2 C2 O2 37(7) . . . . ? S2 Fe2 C2 O2 -143(7) . . . . ? S1 Fe2 C2 O2 129(7) . . . . ? Fe1 Fe2 C2 O2 176(100) . . . . ? C2 Fe2 C3 O3 34(3) . . . . ? C4 Fe2 C3 O3 -61(3) . . . . ? S2 Fe2 C3 O3 135(3) . . . . ? S1 Fe2 C3 O3 -150(3) . . . . ? Fe1 Fe2 C3 O3 -173(3) . . . . ? C3 Fe2 C4 O4 65.6(19) . . . . ? C2 Fe2 C4 O4 -31.4(19) . . . . ? S2 Fe2 C4 O4 149.4(17) . . . . ? S1 Fe2 C4 O4 -136.8(19) . . . . ? Fe1 Fe2 C4 O4 172.8(19) . . . . ? Fe1 S1 C5 C6 -66.2(3) . . . . ? Fe2 S1 C5 C6 11.1(3) . . . . ? S1 C5 C6 C7 54.7(4) . . . . ? C5 C6 C7 S2 -51.2(4) . . . . ? Fe1 S2 C7 C6 59.1(3) . . . . ? Fe2 S2 C7 C6 -18.1(3) . . . . ? P1 N1 C8 C10 141.7(3) . . . . ? P2 N1 C8 C10 -65.0(4) . . . . ? P1 N1 C8 C9 -83.8(3) . . . . ? P2 N1 C8 C9 69.5(3) . . . . ? N1 P1 C11 C16 87.1(2) . . . . ? C17 P1 C11 C16 -160.8(2) . . . . ? Fe1 P1 C11 C16 -21.0(2) . . . . ? P2 P1 C11 C16 46.7(2) . . . . ? N1 P1 C11 C12 -87.6(2) . . . . ? C17 P1 C11 C12 24.5(2) . . . . ? Fe1 P1 C11 C12 164.28(18) . . . . ? P2 P1 C11 C12 -127.98(19) . . . . ? C16 C11 C12 C13 -0.5(4) . . . . ? P1 C11 C12 C13 174.3(2) . . . . ? C11 C12 C13 C14 0.5(5) . . . . ? C12 C13 C14 C15 -0.4(5) . . . . ? C13 C14 C15 C16 0.2(5) . . . . ? C14 C15 C16 C11 -0.1(4) . . . . ? C12 C11 C16 C15 0.3(4) . . . . ? P1 C11 C16 C15 -174.6(2) . . . . ? N1 P1 C17 C18 -6.1(3) . . . . ? C11 P1 C17 C18 -116.1(2) . . . . ? Fe1 P1 C17 C18 102.2(2) . . . . ? P2 P1 C17 C18 35.5(3) . . . . ? N1 P1 C17 C22 174.62(18) . . . . ? C11 P1 C17 C22 64.6(2) . . . . ? Fe1 P1 C17 C22 -77.1(2) . . . . ? P2 P1 C17 C22 -143.81(15) . . . . ? C22 C17 C18 C19 -0.4(4) . . . . ? P1 C17 C18 C19 -179.7(3) . . . . ? C17 C18 C19 C20 0.3(5) . . . . ? C18 C19 C20 C21 -0.3(5) . . . . ? C19 C20 C21 C22 0.3(4) . . . . ? C20 C21 C22 C17 -0.4(4) . . . . ? C18 C17 C22 C21 0.4(4) . . . . ? P1 C17 C22 C21 179.74(18) . . . . ? N1 P2 C23 C28 -95.4(2) . . . . ? C29 P2 C23 C28 151.0(2) . . . . ? Fe1 P2 C23 C28 13.4(2) . . . . ? P1 P2 C23 C28 -54.3(2) . . . . ? N1 P2 C23 C24 81.1(2) . . . . ? C29 P2 C23 C24 -32.5(2) . . . . ? Fe1 P2 C23 C24 -170.09(17) . . . . ? P1 P2 C23 C24 122.15(19) . . . . ? C28 C23 C24 C25 1.6(4) . . . . ? P2 C23 C24 C25 -174.9(2) . . . . ? C23 C24 C25 C26 -1.3(4) . . . . ? C24 C25 C26 C27 0.2(4) . . . . ? C25 C26 C27 C28 0.6(5) . . . . ? C26 C27 C28 C23 -0.2(4) . . . . ? C24 C23 C28 C27 -0.9(4) . . . . ? P2 C23 C28 C27 175.7(2) . . . . ? N1 P2 C29 C34 15.7(2) . . . . ? C23 P2 C29 C34 127.5(2) . . . . ? Fe1 P2 C29 C34 -93.0(2) . . . . ? P1 P2 C29 C34 -26.4(3) . . . . ? N1 P2 C29 C30 -167.48(19) . . . . ? C23 P2 C29 C30 -55.8(2) . . . . ? Fe1 P2 C29 C30 83.7(2) . . . . ? P1 P2 C29 C30 150.40(16) . . . . ? C34 C29 C30 C31 -1.3(4) . . . . ? P2 C29 C30 C31 -178.2(2) . . . . ? C29 C30 C31 C32 -0.5(4) . . . . ? C30 C31 C32 C33 1.4(4) . . . . ? C31 C32 C33 C34 -0.6(5) . . . . ? C30 C29 C34 C33 2.2(4) . . . . ? P2 C29 C34 C33 178.9(2) . . . . ? C32 C33 C34 C29 -1.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.451 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.099 #===END data_str0459 _database_code_depnum_ccdc_archive 'CCDC 639870' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H31 Fe2 N O4 P2 S2' _chemical_formula_weight 755.36 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' 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 P21/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 9.8036(6) _cell_length_b 17.9672(12) _cell_length_c 18.4965(12) _cell_angle_alpha 90.00 _cell_angle_beta 100.9190(10) _cell_angle_gamma 90.00 _cell_volume 3199.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 423(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 1.178 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8159 _exptl_absorpt_correction_T_max 0.9544 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 423(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 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27778 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7641 _reflns_number_gt 6556 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0451P)^2^+1.2266P] 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 7641 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 0.65872(3) 0.678835(14) 0.215303(14) 0.01544(7) Uani 1 1 d . . . Fe2 Fe 0.54249(3) 0.614895(15) 0.092700(14) 0.01765(7) Uani 1 1 d . . . P1 P 0.87033(5) 0.63464(3) 0.25595(2) 0.01520(10) Uani 1 1 d . . . P2 P 0.65150(5) 0.60552(3) 0.31093(2) 0.01530(10) Uani 1 1 d . . . S1 S 0.43198(5) 0.67838(3) 0.17030(3) 0.02083(11) Uani 1 1 d . . . S2 S 0.68892(5) 0.71357(3) 0.10416(3) 0.02077(10) Uani 1 1 d . . . N1 N 0.82373(15) 0.58311(8) 0.32540(8) 0.0167(3) Uani 1 1 d . . . O1 O 0.67460(19) 0.83051(8) 0.26881(9) 0.0364(4) Uani 1 1 d . . . O2 O 0.32712(17) 0.62616(9) -0.04110(8) 0.0354(4) Uani 1 1 d . . . O3 O 0.74895(16) 0.53793(10) 0.02516(9) 0.0374(4) Uani 1 1 d . . . O4 O 0.4524(2) 0.46845(9) 0.13421(9) 0.0448(5) Uani 1 1 d . . . C1 C 0.6728(2) 0.76839(11) 0.25248(10) 0.0234(4) Uani 1 1 d . . . C2 C 0.4128(2) 0.62311(11) 0.01039(11) 0.0238(4) Uani 1 1 d . . . C3 C 0.6710(2) 0.56772(11) 0.05337(11) 0.0243(4) Uani 1 1 d . . . C4 C 0.4871(2) 0.52699(12) 0.12230(11) 0.0269(4) Uani 1 1 d . . . C5 C 0.3799(2) 0.77099(12) 0.13309(12) 0.0309(5) Uani 1 1 d . . . H5A H 0.2793 0.7723 0.1203 0.037 Uiso 1 1 calc R . . H5B H 0.4080 0.8072 0.1719 0.037 Uiso 1 1 calc R . . C6 C 0.4371(2) 0.79567(12) 0.06620(12) 0.0312(5) Uani 1 1 d . . . H6A H 0.4041 0.7615 0.0261 0.037 Uiso 1 1 calc R . . H6B H 0.3994 0.8444 0.0513 0.037 Uiso 1 1 calc R . . C7 C 0.5940(2) 0.79988(11) 0.07695(12) 0.0297(5) Uani 1 1 d . . . H7A H 0.6260 0.8373 0.1141 0.036 Uiso 1 1 calc R . . H7B H 0.6182 0.8170 0.0313 0.036 Uiso 1 1 calc R . . C8 C 0.9092(2) 0.56109(11) 0.39669(10) 0.0225(4) Uani 1 1 d . . . H8A H 0.8498 0.5369 0.4260 0.027 Uiso 1 1 calc R . . H8B H 0.9464 0.6057 0.4228 0.027 Uiso 1 1 calc R . . C9 C 1.0264(2) 0.51031(13) 0.39082(11) 0.0301(5) Uani 1 1 d . . . H9A H 1.0067 0.4664 0.3642 0.036 Uiso 1 1 calc R . . C10 C 1.1563(3) 0.52407(17) 0.42118(13) 0.0465(7) Uani 1 1 d . . . H10A H 1.1790 0.5675 0.4481 0.056 Uiso 1 1 calc R . . H10B H 1.2257 0.4903 0.4158 0.056 Uiso 1 1 calc R . . C11 C 0.95009(18) 0.57279(10) 0.19785(10) 0.0175(4) Uani 1 1 d . . . C12 C 1.0222(2) 0.60296(11) 0.14641(11) 0.0256(4) Uani 1 1 d . . . H12A H 1.0319 0.6543 0.1433 0.031 Uiso 1 1 calc R . . C13 C 1.0793(2) 0.55693(13) 0.10000(12) 0.0304(5) Uani 1 1 d . . . H13A H 1.1287 0.5775 0.0666 0.036 Uiso 1 1 calc R . . C14 C 1.0635(2) 0.48107(13) 0.10306(12) 0.0302(5) Uani 1 1 d . . . H14A H 1.1037 0.4503 0.0725 0.036 Uiso 1 1 calc R . . C15 C 0.9880(2) 0.45061(12) 0.15150(12) 0.0288(4) Uani 1 1 d . . . H15A H 0.9753 0.3994 0.1527 0.035 Uiso 1 1 calc R . . C16 C 0.9308(2) 0.49641(11) 0.19860(11) 0.0229(4) Uani 1 1 d . . . H16A H 0.8793 0.4756 0.2308 0.028 Uiso 1 1 calc R . . C17 C 1.01622(19) 0.69144(10) 0.30270(10) 0.0183(4) Uani 1 1 d . . . C18 C 1.1532(2) 0.68114(12) 0.29400(14) 0.0336(5) Uani 1 1 d . . . H18A H 1.1734 0.6451 0.2615 0.040 Uiso 1 1 calc R . . C19 C 1.2597(2) 0.72415(14) 0.33339(15) 0.0404(6) Uani 1 1 d . . . H19A H 1.3504 0.7176 0.3263 0.048 Uiso 1 1 calc R . . C20 C 1.2313(2) 0.77651(12) 0.38289(12) 0.0318(5) Uani 1 1 d . . . H20A H 1.3031 0.8039 0.4107 0.038 Uiso 1 1 calc R . . C21 C 1.0963(2) 0.78825(12) 0.39107(12) 0.0291(5) Uani 1 1 d . . . H21A H 1.0767 0.8244 0.4236 0.035 Uiso 1 1 calc R . . C22 C 0.9895(2) 0.74636(12) 0.35085(11) 0.0271(4) Uani 1 1 d . . . H22A H 0.8984 0.7552 0.3562 0.032 Uiso 1 1 calc R . . C23 C 0.61247(19) 0.64100(10) 0.39814(10) 0.0183(4) Uani 1 1 d . . . C24 C 0.6223(2) 0.71694(11) 0.41415(11) 0.0229(4) Uani 1 1 d . . . H24A H 0.6570 0.7490 0.3825 0.028 Uiso 1 1 calc R . . C25 C 0.5815(2) 0.74529(12) 0.47611(11) 0.0255(4) Uani 1 1 d . . . H25A H 0.5887 0.7961 0.4856 0.031 Uiso 1 1 calc R . . C26 C 0.5302(2) 0.69884(12) 0.52399(11) 0.0276(4) Uani 1 1 d . . . H26A H 0.4995 0.7183 0.5647 0.033 Uiso 1 1 calc R . . C27 C 0.5249(3) 0.62334(13) 0.51090(12) 0.0352(5) Uani 1 1 d . . . H27A H 0.4946 0.5914 0.5442 0.042 Uiso 1 1 calc R . . C28 C 0.5646(3) 0.59464(12) 0.44808(11) 0.0308(5) Uani 1 1 d . . . H28A H 0.5590 0.5436 0.4394 0.037 Uiso 1 1 calc R . . C29 C 0.55785(19) 0.51755(10) 0.30414(10) 0.0182(4) Uani 1 1 d . . . C30 C 0.6243(2) 0.44875(11) 0.30741(10) 0.0219(4) Uani 1 1 d . . . H30A H 0.7207 0.4467 0.3150 0.026 Uiso 1 1 calc R . . C31 C 0.5479(2) 0.38329(11) 0.29942(11) 0.0276(4) Uani 1 1 d . . . H31A H 0.5933 0.3376 0.3023 0.033 Uiso 1 1 calc R . . C32 C 0.4042(2) 0.38577(12) 0.28721(11) 0.0300(5) Uani 1 1 d . . . H32A H 0.3530 0.3419 0.2814 0.036 Uiso 1 1 calc R . . C33 C 0.3368(2) 0.45377(13) 0.28369(12) 0.0309(5) Uani 1 1 d . . . H33A H 0.2403 0.4555 0.2754 0.037 Uiso 1 1 calc R . . C34 C 0.4132(2) 0.51938(12) 0.29250(11) 0.0255(4) Uani 1 1 d . . . H34A H 0.3674 0.5649 0.2906 0.031 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 0.01582(14) 0.01547(13) 0.01419(13) -0.00013(9) 0.00073(10) 0.00192(9) Fe2 0.01809(14) 0.01946(14) 0.01535(13) -0.00074(10) 0.00300(10) 0.00024(10) P1 0.0145(2) 0.0157(2) 0.0149(2) -0.00003(17) 0.00173(16) 0.00069(17) P2 0.0153(2) 0.0168(2) 0.0138(2) -0.00076(17) 0.00263(17) 0.00238(17) S1 0.0160(2) 0.0269(2) 0.0192(2) -0.00088(18) 0.00228(17) 0.00450(18) S2 0.0235(2) 0.0204(2) 0.0178(2) 0.00299(18) 0.00219(17) -0.00137(18) N1 0.0151(7) 0.0196(7) 0.0151(7) 0.0026(6) 0.0021(6) 0.0028(6) O1 0.0563(11) 0.0196(7) 0.0333(9) -0.0031(6) 0.0088(8) 0.0025(7) O2 0.0342(9) 0.0388(9) 0.0282(8) -0.0022(7) -0.0069(7) 0.0012(7) O3 0.0292(8) 0.0494(10) 0.0351(9) -0.0131(8) 0.0100(7) 0.0063(7) O4 0.0799(14) 0.0290(9) 0.0281(9) -0.0025(7) 0.0165(9) -0.0158(9) C1 0.0277(10) 0.0229(10) 0.0187(9) 0.0019(7) 0.0023(8) 0.0036(8) C2 0.0253(10) 0.0234(10) 0.0229(10) -0.0017(8) 0.0050(8) -0.0002(8) C3 0.0249(10) 0.0268(10) 0.0201(9) -0.0031(8) 0.0016(8) -0.0015(8) C4 0.0367(12) 0.0278(11) 0.0173(9) -0.0033(8) 0.0077(8) -0.0010(9) C5 0.0282(11) 0.0316(11) 0.0292(11) -0.0022(9) -0.0035(9) 0.0157(9) C6 0.0382(12) 0.0223(10) 0.0279(11) 0.0027(8) -0.0069(9) 0.0080(9) C7 0.0385(12) 0.0198(9) 0.0273(11) 0.0071(8) -0.0023(9) 0.0002(9) C8 0.0209(9) 0.0306(10) 0.0153(9) 0.0041(8) 0.0017(7) 0.0040(8) C9 0.0346(12) 0.0325(11) 0.0219(10) 0.0055(9) 0.0023(9) 0.0144(9) C10 0.0280(12) 0.077(2) 0.0336(13) 0.0062(13) 0.0043(10) 0.0212(13) C11 0.0141(8) 0.0213(9) 0.0167(8) -0.0009(7) 0.0020(7) 0.0017(7) C12 0.0253(10) 0.0246(10) 0.0291(10) 0.0031(8) 0.0104(8) -0.0013(8) C13 0.0289(11) 0.0369(12) 0.0297(11) 0.0036(9) 0.0166(9) 0.0006(9) C14 0.0297(11) 0.0362(12) 0.0274(11) -0.0068(9) 0.0121(9) 0.0044(9) C15 0.0375(12) 0.0227(10) 0.0287(11) -0.0044(8) 0.0124(9) -0.0007(9) C16 0.0268(10) 0.0229(9) 0.0211(9) -0.0013(8) 0.0097(8) -0.0026(8) C17 0.0169(9) 0.0174(8) 0.0187(9) 0.0015(7) -0.0012(7) 0.0001(7) C18 0.0203(10) 0.0307(11) 0.0467(14) -0.0151(10) -0.0018(9) 0.0052(8) C19 0.0160(10) 0.0438(14) 0.0578(16) -0.0159(12) -0.0020(10) 0.0028(9) C20 0.0258(11) 0.0292(11) 0.0355(12) -0.0062(9) -0.0066(9) -0.0031(9) C21 0.0301(11) 0.0297(11) 0.0269(11) -0.0105(9) 0.0034(9) -0.0015(9) C22 0.0198(10) 0.0348(11) 0.0275(10) -0.0079(9) 0.0067(8) -0.0007(8) C23 0.0171(9) 0.0224(9) 0.0152(8) -0.0028(7) 0.0026(7) 0.0018(7) C24 0.0236(10) 0.0241(10) 0.0213(9) -0.0027(8) 0.0049(8) -0.0028(8) C25 0.0257(10) 0.0264(10) 0.0241(10) -0.0078(8) 0.0044(8) -0.0011(8) C26 0.0289(11) 0.0359(11) 0.0190(9) -0.0087(8) 0.0067(8) -0.0020(9) C27 0.0538(15) 0.0347(12) 0.0215(11) -0.0024(9) 0.0184(10) -0.0083(11) C28 0.0505(14) 0.0220(10) 0.0220(10) -0.0018(8) 0.0122(9) -0.0013(9) C29 0.0208(9) 0.0214(9) 0.0130(8) -0.0005(7) 0.0051(7) -0.0008(7) C30 0.0221(10) 0.0225(9) 0.0227(10) -0.0001(8) 0.0085(8) 0.0010(8) C31 0.0383(12) 0.0214(10) 0.0259(10) -0.0017(8) 0.0131(9) -0.0030(9) C32 0.0380(13) 0.0327(11) 0.0213(10) -0.0045(8) 0.0105(9) -0.0158(9) C33 0.0219(10) 0.0436(13) 0.0272(11) -0.0021(9) 0.0047(8) -0.0088(9) C34 0.0211(10) 0.0298(11) 0.0255(10) -0.0008(8) 0.0039(8) 0.0000(8) _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 C1 1.745(2) . ? Fe1 P1 2.2156(5) . ? Fe1 P2 2.2172(5) . ? Fe1 S1 2.2211(5) . ? Fe1 S2 2.2212(5) . ? Fe1 Fe2 2.6042(4) . ? Fe2 C3 1.784(2) . ? Fe2 C4 1.789(2) . ? Fe2 C2 1.795(2) . ? Fe2 S1 2.2637(5) . ? Fe2 S2 2.2657(5) . ? P1 N1 1.7143(15) . ? P1 C11 1.8218(18) . ? P1 C17 1.8348(19) . ? P1 P2 2.5956(7) . ? P2 N1 1.7069(15) . ? P2 C29 1.8202(19) . ? P2 C23 1.8408(18) . ? S1 C5 1.836(2) . ? S2 C7 1.830(2) . ? N1 C8 1.476(2) . ? O1 C1 1.156(2) . ? O2 C2 1.146(2) . ? O3 C3 1.137(2) . ? O4 C4 1.140(3) . ? C5 C6 1.518(3) . ? C6 C7 1.514(3) . ? C8 C9 1.487(3) . ? C9 C10 1.315(3) . ? C11 C16 1.386(3) . ? C11 C12 1.398(3) . ? C12 C13 1.384(3) . ? C13 C14 1.374(3) . ? C14 C15 1.379(3) . ? C15 C16 1.391(3) . ? C17 C22 1.387(3) . ? C17 C18 1.394(3) . ? C18 C19 1.390(3) . ? C19 C20 1.378(3) . ? C20 C21 1.376(3) . ? C21 C22 1.386(3) . ? C23 C28 1.390(3) . ? C23 C24 1.396(3) . ? C24 C25 1.381(3) . ? C25 C26 1.379(3) . ? C26 C27 1.377(3) . ? C27 C28 1.392(3) . ? C29 C30 1.393(3) . ? C29 C34 1.394(3) . ? C30 C31 1.387(3) . ? C31 C32 1.385(3) . ? C32 C33 1.384(3) . ? C33 C34 1.389(3) . ? 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 C1 Fe1 P1 101.41(7) . . ? C1 Fe1 P2 104.21(6) . . ? P1 Fe1 P2 71.683(18) . . ? C1 Fe1 S1 98.62(7) . . ? P1 Fe1 S1 158.77(2) . . ? P2 Fe1 S1 96.65(2) . . ? C1 Fe1 S2 95.24(7) . . ? P1 Fe1 S2 97.72(2) . . ? P2 Fe1 S2 159.26(2) . . ? S1 Fe1 S2 87.34(2) . . ? C1 Fe1 Fe2 137.63(6) . . ? P1 Fe1 Fe2 111.375(16) . . ? P2 Fe1 Fe2 110.960(17) . . ? S1 Fe1 Fe2 55.269(14) . . ? S2 Fe1 Fe2 55.323(15) . . ? C3 Fe2 C4 89.09(9) . . ? C3 Fe2 C2 97.74(9) . . ? C4 Fe2 C2 97.17(9) . . ? C3 Fe2 S1 163.30(6) . . ? C4 Fe2 S1 92.37(7) . . ? C2 Fe2 S1 98.58(7) . . ? C3 Fe2 S2 85.75(7) . . ? C4 Fe2 S2 152.33(7) . . ? C2 Fe2 S2 110.45(7) . . ? S1 Fe2 S2 85.25(2) . . ? C3 Fe2 Fe1 109.78(6) . . ? C4 Fe2 Fe1 103.36(6) . . ? C2 Fe2 Fe1 145.59(6) . . ? S1 Fe2 Fe1 53.742(15) . . ? S2 Fe2 Fe1 53.728(14) . . ? N1 P1 C11 108.52(8) . . ? N1 P1 C17 103.99(8) . . ? C11 P1 C17 103.53(9) . . ? N1 P1 Fe1 94.73(5) . . ? C11 P1 Fe1 119.83(6) . . ? C17 P1 Fe1 123.83(6) . . ? N1 P1 P2 40.55(5) . . ? C11 P1 P2 125.95(6) . . ? C17 P1 P2 123.77(6) . . ? Fe1 P1 P2 54.188(16) . . ? N1 P2 C29 106.08(8) . . ? N1 P2 C23 107.93(8) . . ? C29 P2 C23 100.10(8) . . ? N1 P2 Fe1 94.89(5) . . ? C29 P2 Fe1 123.56(6) . . ? C23 P2 Fe1 122.45(6) . . ? N1 P2 P1 40.76(5) . . ? C29 P2 P1 126.26(6) . . ? C23 P2 P1 126.72(6) . . ? Fe1 P2 P1 54.129(16) . . ? C5 S1 Fe1 108.95(8) . . ? C5 S1 Fe2 110.58(7) . . ? Fe1 S1 Fe2 70.989(17) . . ? C7 S2 Fe1 110.04(8) . . ? C7 S2 Fe2 110.92(7) . . ? Fe1 S2 Fe2 70.949(17) . . ? C8 N1 P2 125.49(12) . . ? C8 N1 P1 128.87(13) . . ? P2 N1 P1 98.70(8) . . ? O1 C1 Fe1 171.82(18) . . ? O2 C2 Fe2 177.29(19) . . ? O3 C3 Fe2 176.78(18) . . ? O4 C4 Fe2 173.09(18) . . ? C6 C5 S1 116.78(15) . . ? C7 C6 C5 115.50(17) . . ? C6 C7 S2 116.42(15) . . ? N1 C8 C9 114.51(16) . . ? C10 C9 C8 123.6(2) . . ? C16 C11 C12 118.57(17) . . ? C16 C11 P1 121.58(14) . . ? C12 C11 P1 119.60(15) . . ? C13 C12 C11 120.44(19) . . ? C14 C13 C12 120.33(19) . . ? C13 C14 C15 119.93(19) . . ? C14 C15 C16 120.1(2) . . ? C11 C16 C15 120.51(18) . . ? C22 C17 C18 118.15(18) . . ? C22 C17 P1 118.22(15) . . ? C18 C17 P1 123.60(15) . . ? C19 C18 C17 120.7(2) . . ? C20 C19 C18 120.1(2) . . ? C21 C20 C19 119.8(2) . . ? C20 C21 C22 120.15(19) . . ? C21 C22 C17 121.01(19) . . ? C28 C23 C24 117.60(17) . . ? C28 C23 P2 121.83(15) . . ? C24 C23 P2 120.46(14) . . ? C25 C24 C23 121.15(18) . . ? C26 C25 C24 120.53(19) . . ? C27 C26 C25 119.30(19) . . ? C26 C27 C28 120.3(2) . . ? C23 C28 C27 121.05(19) . . ? C30 C29 C34 118.76(18) . . ? C30 C29 P2 122.82(14) . . ? C34 C29 P2 118.38(15) . . ? C31 C30 C29 120.63(19) . . ? C32 C31 C30 120.1(2) . . ? C33 C32 C31 119.82(19) . . ? C32 C33 C34 120.1(2) . . ? C33 C34 C29 120.53(19) . . ? 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 C1 Fe1 Fe2 C3 122.38(12) . . . . ? P1 Fe1 Fe2 C3 -15.72(7) . . . . ? P2 Fe1 Fe2 C3 -93.51(7) . . . . ? S1 Fe1 Fe2 C3 -176.92(7) . . . . ? S2 Fe1 Fe2 C3 68.81(7) . . . . ? C1 Fe1 Fe2 C4 -143.71(12) . . . . ? P1 Fe1 Fe2 C4 78.19(7) . . . . ? P2 Fe1 Fe2 C4 0.40(7) . . . . ? S1 Fe1 Fe2 C4 -83.02(7) . . . . ? S2 Fe1 Fe2 C4 162.71(8) . . . . ? C1 Fe1 Fe2 C2 -18.71(16) . . . . ? P1 Fe1 Fe2 C2 -156.81(12) . . . . ? P2 Fe1 Fe2 C2 125.40(12) . . . . ? S1 Fe1 Fe2 C2 41.98(12) . . . . ? S2 Fe1 Fe2 C2 -72.28(12) . . . . ? C1 Fe1 Fe2 S1 -60.69(10) . . . . ? P1 Fe1 Fe2 S1 161.21(2) . . . . ? P2 Fe1 Fe2 S1 83.42(2) . . . . ? S2 Fe1 Fe2 S1 -114.26(2) . . . . ? C1 Fe1 Fe2 S2 53.57(10) . . . . ? P1 Fe1 Fe2 S2 -84.53(2) . . . . ? P2 Fe1 Fe2 S2 -162.32(2) . . . . ? S1 Fe1 Fe2 S2 114.26(2) . . . . ? C1 Fe1 P1 N1 101.73(8) . . . . ? P2 Fe1 P1 N1 0.37(5) . . . . ? S1 Fe1 P1 N1 -58.61(8) . . . . ? S2 Fe1 P1 N1 -161.30(5) . . . . ? Fe2 Fe1 P1 N1 -105.60(5) . . . . ? C1 Fe1 P1 C11 -143.75(10) . . . . ? P2 Fe1 P1 C11 114.88(7) . . . . ? S1 Fe1 P1 C11 55.91(10) . . . . ? S2 Fe1 P1 C11 -46.78(7) . . . . ? Fe2 Fe1 P1 C11 8.92(7) . . . . ? C1 Fe1 P1 C17 -8.60(10) . . . . ? P2 Fe1 P1 C17 -109.97(8) . . . . ? S1 Fe1 P1 C17 -168.95(8) . . . . ? S2 Fe1 P1 C17 88.36(8) . . . . ? Fe2 Fe1 P1 C17 144.07(7) . . . . ? C1 Fe1 P1 P2 101.37(7) . . . . ? S1 Fe1 P1 P2 -58.98(6) . . . . ? S2 Fe1 P1 P2 -161.67(2) . . . . ? Fe2 Fe1 P1 P2 -105.966(19) . . . . ? C1 Fe1 P2 N1 -97.90(9) . . . . ? P1 Fe1 P2 N1 -0.37(5) . . . . ? S1 Fe1 P2 N1 161.43(5) . . . . ? S2 Fe1 P2 N1 61.29(8) . . . . ? Fe2 Fe1 P2 N1 106.15(5) . . . . ? C1 Fe1 P2 C29 149.12(10) . . . . ? P1 Fe1 P2 C29 -113.35(8) . . . . ? S1 Fe1 P2 C29 48.45(8) . . . . ? S2 Fe1 P2 C29 -51.69(10) . . . . ? Fe2 Fe1 P2 C29 -6.83(8) . . . . ? C1 Fe1 P2 C23 16.96(10) . . . . ? P1 Fe1 P2 C23 114.49(7) . . . . ? S1 Fe1 P2 C23 -83.71(7) . . . . ? S2 Fe1 P2 C23 176.15(8) . . . . ? Fe2 Fe1 P2 C23 -138.99(7) . . . . ? C1 Fe1 P2 P1 -97.53(7) . . . . ? S1 Fe1 P2 P1 161.80(2) . . . . ? S2 Fe1 P2 P1 61.66(6) . . . . ? Fe2 Fe1 P2 P1 106.518(18) . . . . ? C11 P1 P2 N1 75.88(11) . . . . ? C17 P1 P2 N1 -70.48(11) . . . . ? Fe1 P1 P2 N1 179.43(8) . . . . ? N1 P1 P2 C29 -71.04(11) . . . . ? C11 P1 P2 C29 4.84(11) . . . . ? C17 P1 P2 C29 -141.52(10) . . . . ? Fe1 P1 P2 C29 108.39(8) . . . . ? N1 P1 P2 C23 73.90(11) . . . . ? C11 P1 P2 C23 149.78(10) . . . . ? C17 P1 P2 C23 3.42(11) . . . . ? Fe1 P1 P2 C23 -106.66(8) . . . . ? N1 P1 P2 Fe1 -179.43(8) . . . . ? C11 P1 P2 Fe1 -103.56(7) . . . . ? C17 P1 P2 Fe1 110.09(7) . . . . ? C1 Fe1 S1 C5 37.58(10) . . . . ? P1 Fe1 S1 C5 -161.90(9) . . . . ? P2 Fe1 S1 C5 143.11(7) . . . . ? S2 Fe1 S1 C5 -57.32(8) . . . . ? Fe2 Fe1 S1 C5 -105.95(8) . . . . ? C1 Fe1 S1 Fe2 143.53(7) . . . . ? P1 Fe1 S1 Fe2 -55.95(6) . . . . ? P2 Fe1 S1 Fe2 -110.939(19) . . . . ? S2 Fe1 S1 Fe2 48.637(17) . . . . ? C3 Fe2 S1 C5 113.9(2) . . . . ? C4 Fe2 S1 C5 -151.40(10) . . . . ? C2 Fe2 S1 C5 -53.78(10) . . . . ? S2 Fe2 S1 C5 56.22(8) . . . . ? Fe1 Fe2 S1 C5 103.74(8) . . . . ? C3 Fe2 S1 Fe1 10.1(2) . . . . ? C4 Fe2 S1 Fe1 104.86(7) . . . . ? C2 Fe2 S1 Fe1 -157.52(7) . . . . ? S2 Fe2 S1 Fe1 -47.521(17) . . . . ? C1 Fe1 S2 C7 -40.98(10) . . . . ? P1 Fe1 S2 C7 -143.27(8) . . . . ? P2 Fe1 S2 C7 159.25(9) . . . . ? S1 Fe1 S2 C7 57.44(8) . . . . ? Fe2 Fe1 S2 C7 106.03(8) . . . . ? C1 Fe1 S2 Fe2 -147.01(7) . . . . ? P1 Fe1 S2 Fe2 110.700(18) . . . . ? P2 Fe1 S2 Fe2 53.22(6) . . . . ? S1 Fe1 S2 Fe2 -48.594(17) . . . . ? C3 Fe2 S2 C7 136.78(10) . . . . ? C4 Fe2 S2 C7 -143.34(17) . . . . ? C2 Fe2 S2 C7 40.09(11) . . . . ? S1 Fe2 S2 C7 -57.30(8) . . . . ? Fe1 Fe2 S2 C7 -104.84(8) . . . . ? C3 Fe2 S2 Fe1 -118.38(6) . . . . ? C4 Fe2 S2 Fe1 -38.51(15) . . . . ? C2 Fe2 S2 Fe1 144.93(7) . . . . ? S1 Fe2 S2 Fe1 47.532(17) . . . . ? C29 P2 N1 C8 -79.81(16) . . . . ? C23 P2 N1 C8 26.76(17) . . . . ? Fe1 P2 N1 C8 153.18(15) . . . . ? P1 P2 N1 C8 152.72(19) . . . . ? C29 P2 N1 P1 127.48(8) . . . . ? C23 P2 N1 P1 -125.96(8) . . . . ? Fe1 P2 N1 P1 0.46(7) . . . . ? C11 P1 N1 C8 84.54(17) . . . . ? C17 P1 N1 C8 -25.20(17) . . . . ? Fe1 P1 N1 C8 -151.82(15) . . . . ? P2 P1 N1 C8 -151.4(2) . . . . ? C11 P1 N1 P2 -124.11(8) . . . . ? C17 P1 N1 P2 126.15(8) . . . . ? Fe1 P1 N1 P2 -0.46(7) . . . . ? P1 Fe1 C1 O1 132.7(14) . . . . ? P2 Fe1 C1 O1 -153.6(14) . . . . ? S1 Fe1 C1 O1 -54.4(14) . . . . ? S2 Fe1 C1 O1 33.7(14) . . . . ? Fe2 Fe1 C1 O1 -7.9(14) . . . . ? C3 Fe2 C2 O2 105(4) . . . . ? C4 Fe2 C2 O2 15(4) . . . . ? S1 Fe2 C2 O2 -78(4) . . . . ? S2 Fe2 C2 O2 -166(4) . . . . ? Fe1 Fe2 C2 O2 -111(4) . . . . ? C4 Fe2 C3 O3 100(3) . . . . ? C2 Fe2 C3 O3 3(3) . . . . ? S1 Fe2 C3 O3 -164(3) . . . . ? S2 Fe2 C3 O3 -107(3) . . . . ? Fe1 Fe2 C3 O3 -156(3) . . . . ? C3 Fe2 C4 O4 -45.8(18) . . . . ? C2 Fe2 C4 O4 51.9(18) . . . . ? S1 Fe2 C4 O4 150.8(18) . . . . ? S2 Fe2 C4 O4 -124.9(17) . . . . ? Fe1 Fe2 C4 O4 -155.9(18) . . . . ? Fe1 S1 C5 C6 66.23(17) . . . . ? Fe2 S1 C5 C6 -9.95(19) . . . . ? S1 C5 C6 C7 -60.1(2) . . . . ? C5 C6 C7 S2 59.0(2) . . . . ? Fe1 S2 C7 C6 -65.04(17) . . . . ? Fe2 S2 C7 C6 11.51(19) . . . . ? P2 N1 C8 C9 150.91(15) . . . . ? P1 N1 C8 C9 -64.7(2) . . . . ? N1 C8 C9 C10 125.6(2) . . . . ? N1 P1 C11 C16 18.77(18) . . . . ? C17 P1 C11 C16 128.82(16) . . . . ? Fe1 P1 C11 C16 -88.23(16) . . . . ? P2 P1 C11 C16 -22.90(19) . . . . ? N1 P1 C11 C12 -167.09(15) . . . . ? C17 P1 C11 C12 -57.03(17) . . . . ? Fe1 P1 C11 C12 85.91(16) . . . . ? P2 P1 C11 C12 151.24(13) . . . . ? C16 C11 C12 C13 -3.4(3) . . . . ? P1 C11 C12 C13 -177.73(16) . . . . ? C11 C12 C13 C14 1.2(3) . . . . ? C12 C13 C14 C15 1.3(3) . . . . ? C13 C14 C15 C16 -1.7(3) . . . . ? C12 C11 C16 C15 3.1(3) . . . . ? P1 C11 C16 C15 177.29(16) . . . . ? C14 C15 C16 C11 -0.6(3) . . . . ? N1 P1 C17 C22 -67.94(17) . . . . ? C11 P1 C17 C22 178.68(16) . . . . ? Fe1 P1 C17 C22 37.68(18) . . . . ? P2 P1 C17 C22 -28.79(18) . . . . ? N1 P1 C17 C18 110.28(18) . . . . ? C11 P1 C17 C18 -3.1(2) . . . . ? Fe1 P1 C17 C18 -144.09(16) . . . . ? P2 P1 C17 C18 149.44(16) . . . . ? C22 C17 C18 C19 0.9(3) . . . . ? P1 C17 C18 C19 -177.34(19) . . . . ? C17 C18 C19 C20 1.5(4) . . . . ? C18 C19 C20 C21 -2.6(4) . . . . ? C19 C20 C21 C22 1.5(4) . . . . ? C20 C21 C22 C17 0.9(3) . . . . ? C18 C17 C22 C21 -2.1(3) . . . . ? P1 C17 C22 C21 176.25(17) . . . . ? N1 P2 C23 C28 -92.89(18) . . . . ? C29 P2 C23 C28 17.81(19) . . . . ? Fe1 P2 C23 C28 158.94(15) . . . . ? P1 P2 C23 C28 -134.13(16) . . . . ? N1 P2 C23 C24 91.02(16) . . . . ? C29 P2 C23 C24 -158.29(16) . . . . ? Fe1 P2 C23 C24 -17.15(18) . . . . ? P1 P2 C23 C24 49.77(18) . . . . ? C28 C23 C24 C25 -2.1(3) . . . . ? P2 C23 C24 C25 174.11(16) . . . . ? C23 C24 C25 C26 0.2(3) . . . . ? C24 C25 C26 C27 2.4(3) . . . . ? C25 C26 C27 C28 -3.1(4) . . . . ? C24 C23 C28 C27 1.5(3) . . . . ? P2 C23 C28 C27 -174.72(19) . . . . ? C26 C27 C28 C23 1.1(4) . . . . ? N1 P2 C29 C30 -2.68(17) . . . . ? C23 P2 C29 C30 -114.81(16) . . . . ? Fe1 P2 C29 C30 104.64(15) . . . . ? P1 P2 C29 C30 37.31(18) . . . . ? N1 P2 C29 C34 179.71(14) . . . . ? C23 P2 C29 C34 67.58(16) . . . . ? Fe1 P2 C29 C34 -72.98(16) . . . . ? P1 P2 C29 C34 -140.31(13) . . . . ? C34 C29 C30 C31 -0.2(3) . . . . ? P2 C29 C30 C31 -177.76(15) . . . . ? C29 C30 C31 C32 0.7(3) . . . . ? C30 C31 C32 C33 -0.6(3) . . . . ? C31 C32 C33 C34 -0.1(3) . . . . ? C32 C33 C34 C29 0.7(3) . . . . ? C30 C29 C34 C33 -0.6(3) . . . . ? P2 C29 C34 C33 177.14(15) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.746 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.078 data_str0459 _database_code_depnum_ccdc_archive 'CCDC 639870' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H31 Fe2 N O4 P2 S2' _chemical_formula_weight 755.36 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' 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 P21/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 9.8036(6) _cell_length_b 17.9672(12) _cell_length_c 18.4965(12) _cell_angle_alpha 90.00 _cell_angle_beta 100.9190(10) _cell_angle_gamma 90.00 _cell_volume 3199.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 423(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 1.178 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8159 _exptl_absorpt_correction_T_max 0.9544 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 423(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 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27778 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7641 _reflns_number_gt 6556 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0451P)^2^+1.2266P] 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 7641 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 0.65872(3) 0.678835(14) 0.215303(14) 0.01544(7) Uani 1 1 d . . . Fe2 Fe 0.54249(3) 0.614895(15) 0.092700(14) 0.01765(7) Uani 1 1 d . . . P1 P 0.87033(5) 0.63464(3) 0.25595(2) 0.01520(10) Uani 1 1 d . . . P2 P 0.65150(5) 0.60552(3) 0.31093(2) 0.01530(10) Uani 1 1 d . . . S1 S 0.43198(5) 0.67838(3) 0.17030(3) 0.02083(11) Uani 1 1 d . . . S2 S 0.68892(5) 0.71357(3) 0.10416(3) 0.02077(10) Uani 1 1 d . . . N1 N 0.82373(15) 0.58311(8) 0.32540(8) 0.0167(3) Uani 1 1 d . . . O1 O 0.67460(19) 0.83051(8) 0.26881(9) 0.0364(4) Uani 1 1 d . . . O2 O 0.32712(17) 0.62616(9) -0.04110(8) 0.0354(4) Uani 1 1 d . . . O3 O 0.74895(16) 0.53793(10) 0.02516(9) 0.0374(4) Uani 1 1 d . . . O4 O 0.4524(2) 0.46845(9) 0.13421(9) 0.0448(5) Uani 1 1 d . . . C1 C 0.6728(2) 0.76839(11) 0.25248(10) 0.0234(4) Uani 1 1 d . . . C2 C 0.4128(2) 0.62311(11) 0.01039(11) 0.0238(4) Uani 1 1 d . . . C3 C 0.6710(2) 0.56772(11) 0.05337(11) 0.0243(4) Uani 1 1 d . . . C4 C 0.4871(2) 0.52699(12) 0.12230(11) 0.0269(4) Uani 1 1 d . . . C5 C 0.3799(2) 0.77099(12) 0.13309(12) 0.0309(5) Uani 1 1 d . . . H5A H 0.2793 0.7723 0.1203 0.037 Uiso 1 1 calc R . . H5B H 0.4080 0.8072 0.1719 0.037 Uiso 1 1 calc R . . C6 C 0.4371(2) 0.79567(12) 0.06620(12) 0.0312(5) Uani 1 1 d . . . H6A H 0.4041 0.7615 0.0261 0.037 Uiso 1 1 calc R . . H6B H 0.3994 0.8444 0.0513 0.037 Uiso 1 1 calc R . . C7 C 0.5940(2) 0.79988(11) 0.07695(12) 0.0297(5) Uani 1 1 d . . . H7A H 0.6260 0.8373 0.1141 0.036 Uiso 1 1 calc R . . H7B H 0.6182 0.8170 0.0313 0.036 Uiso 1 1 calc R . . C8 C 0.9092(2) 0.56109(11) 0.39669(10) 0.0225(4) Uani 1 1 d . . . H8A H 0.8498 0.5369 0.4260 0.027 Uiso 1 1 calc R . . H8B H 0.9464 0.6057 0.4228 0.027 Uiso 1 1 calc R . . C9 C 1.0264(2) 0.51031(13) 0.39082(11) 0.0301(5) Uani 1 1 d . . . H9A H 1.0067 0.4664 0.3642 0.036 Uiso 1 1 calc R . . C10 C 1.1563(3) 0.52407(17) 0.42118(13) 0.0465(7) Uani 1 1 d . . . H10A H 1.1790 0.5675 0.4481 0.056 Uiso 1 1 calc R . . H10B H 1.2257 0.4903 0.4158 0.056 Uiso 1 1 calc R . . C11 C 0.95009(18) 0.57279(10) 0.19785(10) 0.0175(4) Uani 1 1 d . . . C12 C 1.0222(2) 0.60296(11) 0.14641(11) 0.0256(4) Uani 1 1 d . . . H12A H 1.0319 0.6543 0.1433 0.031 Uiso 1 1 calc R . . C13 C 1.0793(2) 0.55693(13) 0.10000(12) 0.0304(5) Uani 1 1 d . . . H13A H 1.1287 0.5775 0.0666 0.036 Uiso 1 1 calc R . . C14 C 1.0635(2) 0.48107(13) 0.10306(12) 0.0302(5) Uani 1 1 d . . . H14A H 1.1037 0.4503 0.0725 0.036 Uiso 1 1 calc R . . C15 C 0.9880(2) 0.45061(12) 0.15150(12) 0.0288(4) Uani 1 1 d . . . H15A H 0.9753 0.3994 0.1527 0.035 Uiso 1 1 calc R . . C16 C 0.9308(2) 0.49641(11) 0.19860(11) 0.0229(4) Uani 1 1 d . . . H16A H 0.8793 0.4756 0.2308 0.028 Uiso 1 1 calc R . . C17 C 1.01622(19) 0.69144(10) 0.30270(10) 0.0183(4) Uani 1 1 d . . . C18 C 1.1532(2) 0.68114(12) 0.29400(14) 0.0336(5) Uani 1 1 d . . . H18A H 1.1734 0.6451 0.2615 0.040 Uiso 1 1 calc R . . C19 C 1.2597(2) 0.72415(14) 0.33339(15) 0.0404(6) Uani 1 1 d . . . H19A H 1.3504 0.7176 0.3263 0.048 Uiso 1 1 calc R . . C20 C 1.2313(2) 0.77651(12) 0.38289(12) 0.0318(5) Uani 1 1 d . . . H20A H 1.3031 0.8039 0.4107 0.038 Uiso 1 1 calc R . . C21 C 1.0963(2) 0.78825(12) 0.39107(12) 0.0291(5) Uani 1 1 d . . . H21A H 1.0767 0.8244 0.4236 0.035 Uiso 1 1 calc R . . C22 C 0.9895(2) 0.74636(12) 0.35085(11) 0.0271(4) Uani 1 1 d . . . H22A H 0.8984 0.7552 0.3562 0.032 Uiso 1 1 calc R . . C23 C 0.61247(19) 0.64100(10) 0.39814(10) 0.0183(4) Uani 1 1 d . . . C24 C 0.6223(2) 0.71694(11) 0.41415(11) 0.0229(4) Uani 1 1 d . . . H24A H 0.6570 0.7490 0.3825 0.028 Uiso 1 1 calc R . . C25 C 0.5815(2) 0.74529(12) 0.47611(11) 0.0255(4) Uani 1 1 d . . . H25A H 0.5887 0.7961 0.4856 0.031 Uiso 1 1 calc R . . C26 C 0.5302(2) 0.69884(12) 0.52399(11) 0.0276(4) Uani 1 1 d . . . H26A H 0.4995 0.7183 0.5647 0.033 Uiso 1 1 calc R . . C27 C 0.5249(3) 0.62334(13) 0.51090(12) 0.0352(5) Uani 1 1 d . . . H27A H 0.4946 0.5914 0.5442 0.042 Uiso 1 1 calc R . . C28 C 0.5646(3) 0.59464(12) 0.44808(11) 0.0308(5) Uani 1 1 d . . . H28A H 0.5590 0.5436 0.4394 0.037 Uiso 1 1 calc R . . C29 C 0.55785(19) 0.51755(10) 0.30414(10) 0.0182(4) Uani 1 1 d . . . C30 C 0.6243(2) 0.44875(11) 0.30741(10) 0.0219(4) Uani 1 1 d . . . H30A H 0.7207 0.4467 0.3150 0.026 Uiso 1 1 calc R . . C31 C 0.5479(2) 0.38329(11) 0.29942(11) 0.0276(4) Uani 1 1 d . . . H31A H 0.5933 0.3376 0.3023 0.033 Uiso 1 1 calc R . . C32 C 0.4042(2) 0.38577(12) 0.28721(11) 0.0300(5) Uani 1 1 d . . . H32A H 0.3530 0.3419 0.2814 0.036 Uiso 1 1 calc R . . C33 C 0.3368(2) 0.45377(13) 0.28369(12) 0.0309(5) Uani 1 1 d . . . H33A H 0.2403 0.4555 0.2754 0.037 Uiso 1 1 calc R . . C34 C 0.4132(2) 0.51938(12) 0.29250(11) 0.0255(4) Uani 1 1 d . . . H34A H 0.3674 0.5649 0.2906 0.031 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 0.01582(14) 0.01547(13) 0.01419(13) -0.00013(9) 0.00073(10) 0.00192(9) Fe2 0.01809(14) 0.01946(14) 0.01535(13) -0.00074(10) 0.00300(10) 0.00024(10) P1 0.0145(2) 0.0157(2) 0.0149(2) -0.00003(17) 0.00173(16) 0.00069(17) P2 0.0153(2) 0.0168(2) 0.0138(2) -0.00076(17) 0.00263(17) 0.00238(17) S1 0.0160(2) 0.0269(2) 0.0192(2) -0.00088(18) 0.00228(17) 0.00450(18) S2 0.0235(2) 0.0204(2) 0.0178(2) 0.00299(18) 0.00219(17) -0.00137(18) N1 0.0151(7) 0.0196(7) 0.0151(7) 0.0026(6) 0.0021(6) 0.0028(6) O1 0.0563(11) 0.0196(7) 0.0333(9) -0.0031(6) 0.0088(8) 0.0025(7) O2 0.0342(9) 0.0388(9) 0.0282(8) -0.0022(7) -0.0069(7) 0.0012(7) O3 0.0292(8) 0.0494(10) 0.0351(9) -0.0131(8) 0.0100(7) 0.0063(7) O4 0.0799(14) 0.0290(9) 0.0281(9) -0.0025(7) 0.0165(9) -0.0158(9) C1 0.0277(10) 0.0229(10) 0.0187(9) 0.0019(7) 0.0023(8) 0.0036(8) C2 0.0253(10) 0.0234(10) 0.0229(10) -0.0017(8) 0.0050(8) -0.0002(8) C3 0.0249(10) 0.0268(10) 0.0201(9) -0.0031(8) 0.0016(8) -0.0015(8) C4 0.0367(12) 0.0278(11) 0.0173(9) -0.0033(8) 0.0077(8) -0.0010(9) C5 0.0282(11) 0.0316(11) 0.0292(11) -0.0022(9) -0.0035(9) 0.0157(9) C6 0.0382(12) 0.0223(10) 0.0279(11) 0.0027(8) -0.0069(9) 0.0080(9) C7 0.0385(12) 0.0198(9) 0.0273(11) 0.0071(8) -0.0023(9) 0.0002(9) C8 0.0209(9) 0.0306(10) 0.0153(9) 0.0041(8) 0.0017(7) 0.0040(8) C9 0.0346(12) 0.0325(11) 0.0219(10) 0.0055(9) 0.0023(9) 0.0144(9) C10 0.0280(12) 0.077(2) 0.0336(13) 0.0062(13) 0.0043(10) 0.0212(13) C11 0.0141(8) 0.0213(9) 0.0167(8) -0.0009(7) 0.0020(7) 0.0017(7) C12 0.0253(10) 0.0246(10) 0.0291(10) 0.0031(8) 0.0104(8) -0.0013(8) C13 0.0289(11) 0.0369(12) 0.0297(11) 0.0036(9) 0.0166(9) 0.0006(9) C14 0.0297(11) 0.0362(12) 0.0274(11) -0.0068(9) 0.0121(9) 0.0044(9) C15 0.0375(12) 0.0227(10) 0.0287(11) -0.0044(8) 0.0124(9) -0.0007(9) C16 0.0268(10) 0.0229(9) 0.0211(9) -0.0013(8) 0.0097(8) -0.0026(8) C17 0.0169(9) 0.0174(8) 0.0187(9) 0.0015(7) -0.0012(7) 0.0001(7) C18 0.0203(10) 0.0307(11) 0.0467(14) -0.0151(10) -0.0018(9) 0.0052(8) C19 0.0160(10) 0.0438(14) 0.0578(16) -0.0159(12) -0.0020(10) 0.0028(9) C20 0.0258(11) 0.0292(11) 0.0355(12) -0.0062(9) -0.0066(9) -0.0031(9) C21 0.0301(11) 0.0297(11) 0.0269(11) -0.0105(9) 0.0034(9) -0.0015(9) C22 0.0198(10) 0.0348(11) 0.0275(10) -0.0079(9) 0.0067(8) -0.0007(8) C23 0.0171(9) 0.0224(9) 0.0152(8) -0.0028(7) 0.0026(7) 0.0018(7) C24 0.0236(10) 0.0241(10) 0.0213(9) -0.0027(8) 0.0049(8) -0.0028(8) C25 0.0257(10) 0.0264(10) 0.0241(10) -0.0078(8) 0.0044(8) -0.0011(8) C26 0.0289(11) 0.0359(11) 0.0190(9) -0.0087(8) 0.0067(8) -0.0020(9) C27 0.0538(15) 0.0347(12) 0.0215(11) -0.0024(9) 0.0184(10) -0.0083(11) C28 0.0505(14) 0.0220(10) 0.0220(10) -0.0018(8) 0.0122(9) -0.0013(9) C29 0.0208(9) 0.0214(9) 0.0130(8) -0.0005(7) 0.0051(7) -0.0008(7) C30 0.0221(10) 0.0225(9) 0.0227(10) -0.0001(8) 0.0085(8) 0.0010(8) C31 0.0383(12) 0.0214(10) 0.0259(10) -0.0017(8) 0.0131(9) -0.0030(9) C32 0.0380(13) 0.0327(11) 0.0213(10) -0.0045(8) 0.0105(9) -0.0158(9) C33 0.0219(10) 0.0436(13) 0.0272(11) -0.0021(9) 0.0047(8) -0.0088(9) C34 0.0211(10) 0.0298(11) 0.0255(10) -0.0008(8) 0.0039(8) 0.0000(8) _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 C1 1.745(2) . ? Fe1 P1 2.2156(5) . ? Fe1 P2 2.2172(5) . ? Fe1 S1 2.2211(5) . ? Fe1 S2 2.2212(5) . ? Fe1 Fe2 2.6042(4) . ? Fe2 C3 1.784(2) . ? Fe2 C4 1.789(2) . ? Fe2 C2 1.795(2) . ? Fe2 S1 2.2637(5) . ? Fe2 S2 2.2657(5) . ? P1 N1 1.7143(15) . ? P1 C11 1.8218(18) . ? P1 C17 1.8348(19) . ? P1 P2 2.5956(7) . ? P2 N1 1.7069(15) . ? P2 C29 1.8202(19) . ? P2 C23 1.8408(18) . ? S1 C5 1.836(2) . ? S2 C7 1.830(2) . ? N1 C8 1.476(2) . ? O1 C1 1.156(2) . ? O2 C2 1.146(2) . ? O3 C3 1.137(2) . ? O4 C4 1.140(3) . ? C5 C6 1.518(3) . ? C6 C7 1.514(3) . ? C8 C9 1.487(3) . ? C9 C10 1.315(3) . ? C11 C16 1.386(3) . ? C11 C12 1.398(3) . ? C12 C13 1.384(3) . ? C13 C14 1.374(3) . ? C14 C15 1.379(3) . ? C15 C16 1.391(3) . ? C17 C22 1.387(3) . ? C17 C18 1.394(3) . ? C18 C19 1.390(3) . ? C19 C20 1.378(3) . ? C20 C21 1.376(3) . ? C21 C22 1.386(3) . ? C23 C28 1.390(3) . ? C23 C24 1.396(3) . ? C24 C25 1.381(3) . ? C25 C26 1.379(3) . ? C26 C27 1.377(3) . ? C27 C28 1.392(3) . ? C29 C30 1.393(3) . ? C29 C34 1.394(3) . ? C30 C31 1.387(3) . ? C31 C32 1.385(3) . ? C32 C33 1.384(3) . ? C33 C34 1.389(3) . ? 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 C1 Fe1 P1 101.41(7) . . ? C1 Fe1 P2 104.21(6) . . ? P1 Fe1 P2 71.683(18) . . ? C1 Fe1 S1 98.62(7) . . ? P1 Fe1 S1 158.77(2) . . ? P2 Fe1 S1 96.65(2) . . ? C1 Fe1 S2 95.24(7) . . ? P1 Fe1 S2 97.72(2) . . ? P2 Fe1 S2 159.26(2) . . ? S1 Fe1 S2 87.34(2) . . ? C1 Fe1 Fe2 137.63(6) . . ? P1 Fe1 Fe2 111.375(16) . . ? P2 Fe1 Fe2 110.960(17) . . ? S1 Fe1 Fe2 55.269(14) . . ? S2 Fe1 Fe2 55.323(15) . . ? C3 Fe2 C4 89.09(9) . . ? C3 Fe2 C2 97.74(9) . . ? C4 Fe2 C2 97.17(9) . . ? C3 Fe2 S1 163.30(6) . . ? C4 Fe2 S1 92.37(7) . . ? C2 Fe2 S1 98.58(7) . . ? C3 Fe2 S2 85.75(7) . . ? C4 Fe2 S2 152.33(7) . . ? C2 Fe2 S2 110.45(7) . . ? S1 Fe2 S2 85.25(2) . . ? C3 Fe2 Fe1 109.78(6) . . ? C4 Fe2 Fe1 103.36(6) . . ? C2 Fe2 Fe1 145.59(6) . . ? S1 Fe2 Fe1 53.742(15) . . ? S2 Fe2 Fe1 53.728(14) . . ? N1 P1 C11 108.52(8) . . ? N1 P1 C17 103.99(8) . . ? C11 P1 C17 103.53(9) . . ? N1 P1 Fe1 94.73(5) . . ? C11 P1 Fe1 119.83(6) . . ? C17 P1 Fe1 123.83(6) . . ? N1 P1 P2 40.55(5) . . ? C11 P1 P2 125.95(6) . . ? C17 P1 P2 123.77(6) . . ? Fe1 P1 P2 54.188(16) . . ? N1 P2 C29 106.08(8) . . ? N1 P2 C23 107.93(8) . . ? C29 P2 C23 100.10(8) . . ? N1 P2 Fe1 94.89(5) . . ? C29 P2 Fe1 123.56(6) . . ? C23 P2 Fe1 122.45(6) . . ? N1 P2 P1 40.76(5) . . ? C29 P2 P1 126.26(6) . . ? C23 P2 P1 126.72(6) . . ? Fe1 P2 P1 54.129(16) . . ? C5 S1 Fe1 108.95(8) . . ? C5 S1 Fe2 110.58(7) . . ? Fe1 S1 Fe2 70.989(17) . . ? C7 S2 Fe1 110.04(8) . . ? C7 S2 Fe2 110.92(7) . . ? Fe1 S2 Fe2 70.949(17) . . ? C8 N1 P2 125.49(12) . . ? C8 N1 P1 128.87(13) . . ? P2 N1 P1 98.70(8) . . ? O1 C1 Fe1 171.82(18) . . ? O2 C2 Fe2 177.29(19) . . ? O3 C3 Fe2 176.78(18) . . ? O4 C4 Fe2 173.09(18) . . ? C6 C5 S1 116.78(15) . . ? C7 C6 C5 115.50(17) . . ? C6 C7 S2 116.42(15) . . ? N1 C8 C9 114.51(16) . . ? C10 C9 C8 123.6(2) . . ? C16 C11 C12 118.57(17) . . ? C16 C11 P1 121.58(14) . . ? C12 C11 P1 119.60(15) . . ? C13 C12 C11 120.44(19) . . ? C14 C13 C12 120.33(19) . . ? C13 C14 C15 119.93(19) . . ? C14 C15 C16 120.1(2) . . ? C11 C16 C15 120.51(18) . . ? C22 C17 C18 118.15(18) . . ? C22 C17 P1 118.22(15) . . ? C18 C17 P1 123.60(15) . . ? C19 C18 C17 120.7(2) . . ? C20 C19 C18 120.1(2) . . ? C21 C20 C19 119.8(2) . . ? C20 C21 C22 120.15(19) . . ? C21 C22 C17 121.01(19) . . ? C28 C23 C24 117.60(17) . . ? C28 C23 P2 121.83(15) . . ? C24 C23 P2 120.46(14) . . ? C25 C24 C23 121.15(18) . . ? C26 C25 C24 120.53(19) . . ? C27 C26 C25 119.30(19) . . ? C26 C27 C28 120.3(2) . . ? C23 C28 C27 121.05(19) . . ? C30 C29 C34 118.76(18) . . ? C30 C29 P2 122.82(14) . . ? C34 C29 P2 118.38(15) . . ? C31 C30 C29 120.63(19) . . ? C32 C31 C30 120.1(2) . . ? C33 C32 C31 119.82(19) . . ? C32 C33 C34 120.1(2) . . ? C33 C34 C29 120.53(19) . . ? 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 C1 Fe1 Fe2 C3 122.38(12) . . . . ? P1 Fe1 Fe2 C3 -15.72(7) . . . . ? P2 Fe1 Fe2 C3 -93.51(7) . . . . ? S1 Fe1 Fe2 C3 -176.92(7) . . . . ? S2 Fe1 Fe2 C3 68.81(7) . . . . ? C1 Fe1 Fe2 C4 -143.71(12) . . . . ? P1 Fe1 Fe2 C4 78.19(7) . . . . ? P2 Fe1 Fe2 C4 0.40(7) . . . . ? S1 Fe1 Fe2 C4 -83.02(7) . . . . ? S2 Fe1 Fe2 C4 162.71(8) . . . . ? C1 Fe1 Fe2 C2 -18.71(16) . . . . ? P1 Fe1 Fe2 C2 -156.81(12) . . . . ? P2 Fe1 Fe2 C2 125.40(12) . . . . ? S1 Fe1 Fe2 C2 41.98(12) . . . . ? S2 Fe1 Fe2 C2 -72.28(12) . . . . ? C1 Fe1 Fe2 S1 -60.69(10) . . . . ? P1 Fe1 Fe2 S1 161.21(2) . . . . ? P2 Fe1 Fe2 S1 83.42(2) . . . . ? S2 Fe1 Fe2 S1 -114.26(2) . . . . ? C1 Fe1 Fe2 S2 53.57(10) . . . . ? P1 Fe1 Fe2 S2 -84.53(2) . . . . ? P2 Fe1 Fe2 S2 -162.32(2) . . . . ? S1 Fe1 Fe2 S2 114.26(2) . . . . ? C1 Fe1 P1 N1 101.73(8) . . . . ? P2 Fe1 P1 N1 0.37(5) . . . . ? S1 Fe1 P1 N1 -58.61(8) . . . . ? S2 Fe1 P1 N1 -161.30(5) . . . . ? Fe2 Fe1 P1 N1 -105.60(5) . . . . ? C1 Fe1 P1 C11 -143.75(10) . . . . ? P2 Fe1 P1 C11 114.88(7) . . . . ? S1 Fe1 P1 C11 55.91(10) . . . . ? S2 Fe1 P1 C11 -46.78(7) . . . . ? Fe2 Fe1 P1 C11 8.92(7) . . . . ? C1 Fe1 P1 C17 -8.60(10) . . . . ? P2 Fe1 P1 C17 -109.97(8) . . . . ? S1 Fe1 P1 C17 -168.95(8) . . . . ? S2 Fe1 P1 C17 88.36(8) . . . . ? Fe2 Fe1 P1 C17 144.07(7) . . . . ? C1 Fe1 P1 P2 101.37(7) . . . . ? S1 Fe1 P1 P2 -58.98(6) . . . . ? S2 Fe1 P1 P2 -161.67(2) . . . . ? Fe2 Fe1 P1 P2 -105.966(19) . . . . ? C1 Fe1 P2 N1 -97.90(9) . . . . ? P1 Fe1 P2 N1 -0.37(5) . . . . ? S1 Fe1 P2 N1 161.43(5) . . . . ? S2 Fe1 P2 N1 61.29(8) . . . . ? Fe2 Fe1 P2 N1 106.15(5) . . . . ? C1 Fe1 P2 C29 149.12(10) . . . . ? P1 Fe1 P2 C29 -113.35(8) . . . . ? S1 Fe1 P2 C29 48.45(8) . . . . ? S2 Fe1 P2 C29 -51.69(10) . . . . ? Fe2 Fe1 P2 C29 -6.83(8) . . . . ? C1 Fe1 P2 C23 16.96(10) . . . . ? P1 Fe1 P2 C23 114.49(7) . . . . ? S1 Fe1 P2 C23 -83.71(7) . . . . ? S2 Fe1 P2 C23 176.15(8) . . . . ? Fe2 Fe1 P2 C23 -138.99(7) . . . . ? C1 Fe1 P2 P1 -97.53(7) . . . . ? S1 Fe1 P2 P1 161.80(2) . . . . ? S2 Fe1 P2 P1 61.66(6) . . . . ? Fe2 Fe1 P2 P1 106.518(18) . . . . ? C11 P1 P2 N1 75.88(11) . . . . ? C17 P1 P2 N1 -70.48(11) . . . . ? Fe1 P1 P2 N1 179.43(8) . . . . ? N1 P1 P2 C29 -71.04(11) . . . . ? C11 P1 P2 C29 4.84(11) . . . . ? C17 P1 P2 C29 -141.52(10) . . . . ? Fe1 P1 P2 C29 108.39(8) . . . . ? N1 P1 P2 C23 73.90(11) . . . . ? C11 P1 P2 C23 149.78(10) . . . . ? C17 P1 P2 C23 3.42(11) . . . . ? Fe1 P1 P2 C23 -106.66(8) . . . . ? N1 P1 P2 Fe1 -179.43(8) . . . . ? C11 P1 P2 Fe1 -103.56(7) . . . . ? C17 P1 P2 Fe1 110.09(7) . . . . ? C1 Fe1 S1 C5 37.58(10) . . . . ? P1 Fe1 S1 C5 -161.90(9) . . . . ? P2 Fe1 S1 C5 143.11(7) . . . . ? S2 Fe1 S1 C5 -57.32(8) . . . . ? Fe2 Fe1 S1 C5 -105.95(8) . . . . ? C1 Fe1 S1 Fe2 143.53(7) . . . . ? P1 Fe1 S1 Fe2 -55.95(6) . . . . ? P2 Fe1 S1 Fe2 -110.939(19) . . . . ? S2 Fe1 S1 Fe2 48.637(17) . . . . ? C3 Fe2 S1 C5 113.9(2) . . . . ? C4 Fe2 S1 C5 -151.40(10) . . . . ? C2 Fe2 S1 C5 -53.78(10) . . . . ? S2 Fe2 S1 C5 56.22(8) . . . . ? Fe1 Fe2 S1 C5 103.74(8) . . . . ? C3 Fe2 S1 Fe1 10.1(2) . . . . ? C4 Fe2 S1 Fe1 104.86(7) . . . . ? C2 Fe2 S1 Fe1 -157.52(7) . . . . ? S2 Fe2 S1 Fe1 -47.521(17) . . . . ? C1 Fe1 S2 C7 -40.98(10) . . . . ? P1 Fe1 S2 C7 -143.27(8) . . . . ? P2 Fe1 S2 C7 159.25(9) . . . . ? S1 Fe1 S2 C7 57.44(8) . . . . ? Fe2 Fe1 S2 C7 106.03(8) . . . . ? C1 Fe1 S2 Fe2 -147.01(7) . . . . ? P1 Fe1 S2 Fe2 110.700(18) . . . . ? P2 Fe1 S2 Fe2 53.22(6) . . . . ? S1 Fe1 S2 Fe2 -48.594(17) . . . . ? C3 Fe2 S2 C7 136.78(10) . . . . ? C4 Fe2 S2 C7 -143.34(17) . . . . ? C2 Fe2 S2 C7 40.09(11) . . . . ? S1 Fe2 S2 C7 -57.30(8) . . . . ? Fe1 Fe2 S2 C7 -104.84(8) . . . . ? C3 Fe2 S2 Fe1 -118.38(6) . . . . ? C4 Fe2 S2 Fe1 -38.51(15) . . . . ? C2 Fe2 S2 Fe1 144.93(7) . . . . ? S1 Fe2 S2 Fe1 47.532(17) . . . . ? C29 P2 N1 C8 -79.81(16) . . . . ? C23 P2 N1 C8 26.76(17) . . . . ? Fe1 P2 N1 C8 153.18(15) . . . . ? P1 P2 N1 C8 152.72(19) . . . . ? C29 P2 N1 P1 127.48(8) . . . . ? C23 P2 N1 P1 -125.96(8) . . . . ? Fe1 P2 N1 P1 0.46(7) . . . . ? C11 P1 N1 C8 84.54(17) . . . . ? C17 P1 N1 C8 -25.20(17) . . . . ? Fe1 P1 N1 C8 -151.82(15) . . . . ? P2 P1 N1 C8 -151.4(2) . . . . ? C11 P1 N1 P2 -124.11(8) . . . . ? C17 P1 N1 P2 126.15(8) . . . . ? Fe1 P1 N1 P2 -0.46(7) . . . . ? P1 Fe1 C1 O1 132.7(14) . . . . ? P2 Fe1 C1 O1 -153.6(14) . . . . ? S1 Fe1 C1 O1 -54.4(14) . . . . ? S2 Fe1 C1 O1 33.7(14) . . . . ? Fe2 Fe1 C1 O1 -7.9(14) . . . . ? C3 Fe2 C2 O2 105(4) . . . . ? C4 Fe2 C2 O2 15(4) . . . . ? S1 Fe2 C2 O2 -78(4) . . . . ? S2 Fe2 C2 O2 -166(4) . . . . ? Fe1 Fe2 C2 O2 -111(4) . . . . ? C4 Fe2 C3 O3 100(3) . . . . ? C2 Fe2 C3 O3 3(3) . . . . ? S1 Fe2 C3 O3 -164(3) . . . . ? S2 Fe2 C3 O3 -107(3) . . . . ? Fe1 Fe2 C3 O3 -156(3) . . . . ? C3 Fe2 C4 O4 -45.8(18) . . . . ? C2 Fe2 C4 O4 51.9(18) . . . . ? S1 Fe2 C4 O4 150.8(18) . . . . ? S2 Fe2 C4 O4 -124.9(17) . . . . ? Fe1 Fe2 C4 O4 -155.9(18) . . . . ? Fe1 S1 C5 C6 66.23(17) . . . . ? Fe2 S1 C5 C6 -9.95(19) . . . . ? S1 C5 C6 C7 -60.1(2) . . . . ? C5 C6 C7 S2 59.0(2) . . . . ? Fe1 S2 C7 C6 -65.04(17) . . . . ? Fe2 S2 C7 C6 11.51(19) . . . . ? P2 N1 C8 C9 150.91(15) . . . . ? P1 N1 C8 C9 -64.7(2) . . . . ? N1 C8 C9 C10 125.6(2) . . . . ? N1 P1 C11 C16 18.77(18) . . . . ? C17 P1 C11 C16 128.82(16) . . . . ? Fe1 P1 C11 C16 -88.23(16) . . . . ? P2 P1 C11 C16 -22.90(19) . . . . ? N1 P1 C11 C12 -167.09(15) . . . . ? C17 P1 C11 C12 -57.03(17) . . . . ? Fe1 P1 C11 C12 85.91(16) . . . . ? P2 P1 C11 C12 151.24(13) . . . . ? C16 C11 C12 C13 -3.4(3) . . . . ? P1 C11 C12 C13 -177.73(16) . . . . ? C11 C12 C13 C14 1.2(3) . . . . ? C12 C13 C14 C15 1.3(3) . . . . ? C13 C14 C15 C16 -1.7(3) . . . . ? C12 C11 C16 C15 3.1(3) . . . . ? P1 C11 C16 C15 177.29(16) . . . . ? C14 C15 C16 C11 -0.6(3) . . . . ? N1 P1 C17 C22 -67.94(17) . . . . ? C11 P1 C17 C22 178.68(16) . . . . ? Fe1 P1 C17 C22 37.68(18) . . . . ? P2 P1 C17 C22 -28.79(18) . . . . ? N1 P1 C17 C18 110.28(18) . . . . ? C11 P1 C17 C18 -3.1(2) . . . . ? Fe1 P1 C17 C18 -144.09(16) . . . . ? P2 P1 C17 C18 149.44(16) . . . . ? C22 C17 C18 C19 0.9(3) . . . . ? P1 C17 C18 C19 -177.34(19) . . . . ? C17 C18 C19 C20 1.5(4) . . . . ? C18 C19 C20 C21 -2.6(4) . . . . ? C19 C20 C21 C22 1.5(4) . . . . ? C20 C21 C22 C17 0.9(3) . . . . ? C18 C17 C22 C21 -2.1(3) . . . . ? P1 C17 C22 C21 176.25(17) . . . . ? N1 P2 C23 C28 -92.89(18) . . . . ? C29 P2 C23 C28 17.81(19) . . . . ? Fe1 P2 C23 C28 158.94(15) . . . . ? P1 P2 C23 C28 -134.13(16) . . . . ? N1 P2 C23 C24 91.02(16) . . . . ? C29 P2 C23 C24 -158.29(16) . . . . ? Fe1 P2 C23 C24 -17.15(18) . . . . ? P1 P2 C23 C24 49.77(18) . . . . ? C28 C23 C24 C25 -2.1(3) . . . . ? P2 C23 C24 C25 174.11(16) . . . . ? C23 C24 C25 C26 0.2(3) . . . . ? C24 C25 C26 C27 2.4(3) . . . . ? C25 C26 C27 C28 -3.1(4) . . . . ? C24 C23 C28 C27 1.5(3) . . . . ? P2 C23 C28 C27 -174.72(19) . . . . ? C26 C27 C28 C23 1.1(4) . . . . ? N1 P2 C29 C30 -2.68(17) . . . . ? C23 P2 C29 C30 -114.81(16) . . . . ? Fe1 P2 C29 C30 104.64(15) . . . . ? P1 P2 C29 C30 37.31(18) . . . . ? N1 P2 C29 C34 179.71(14) . . . . ? C23 P2 C29 C34 67.58(16) . . . . ? Fe1 P2 C29 C34 -72.98(16) . . . . ? P1 P2 C29 C34 -140.31(13) . . . . ? C34 C29 C30 C31 -0.2(3) . . . . ? P2 C29 C30 C31 -177.76(15) . . . . ? C29 C30 C31 C32 0.7(3) . . . . ? C30 C31 C32 C33 -0.6(3) . . . . ? C31 C32 C33 C34 -0.1(3) . . . . ? C32 C33 C34 C29 0.7(3) . . . . ? C30 C29 C34 C33 -0.6(3) . . . . ? P2 C29 C34 C33 177.14(15) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.746 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.078 data_str0451 _database_code_depnum_ccdc_archive 'CCDC 919233' #TrackingRef 'STR0451.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C127 H80 Cl2 Fe8 N4 O22 P8 S8' _chemical_formula_weight 3035.97 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' 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 orthorhombic _symmetry_space_group_name_H-M Pbam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' _cell_length_a 21.7006(12) _cell_length_b 15.3850(9) _cell_length_c 20.0483(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6693.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3160 _exptl_absorpt_coefficient_mu 1.170 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8724 _exptl_absorpt_correction_T_max 0.8724 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57217 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.31 _reflns_number_total 8411 _reflns_number_gt 6792 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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. the central carbon atoms of the dithiolate ligands, C4 and C21, were disordered over two sites (50:50) hydrogen atoms were not generated on the dithiolate ligands the carbon atom, C40, of the dichloromethane solvate was disordered over two sites (50:50) both water molecules were disordered over two sites (50:50) solvate atoms were refined only isotropically hydrogen atoms were not generated on the solvate molecules ; _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^)+(0.0847P)^2^+15.7626P] 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 8411 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1621 _refine_ls_wR_factor_gt 0.1523 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.18079(2) 0.57970(3) 0.43799(2) 0.02234(14) Uani 1 1 d . . . Fe2 Fe 0.16844(2) 0.39335(3) 0.06203(2) 0.01716(13) Uani 1 1 d . . . P1 P 0.19058(4) 0.43810(6) 0.42602(4) 0.02214(19) Uani 1 1 d . . . P2 P 0.11211(4) 0.27575(5) 0.07336(4) 0.01755(18) Uani 1 1 d . . . S1 S 0.18288(6) 0.70190(8) 0.5000 0.0280(3) Uani 1 2 d S . . S2 S 0.09731(6) 0.54520(8) 0.5000 0.0236(2) Uani 1 2 d S . . S3 S 0.08989(5) 0.44486(7) 0.0000 0.0185(2) Uani 1 2 d S . . S4 S 0.22664(5) 0.48404(8) 0.0000 0.0233(2) Uani 1 2 d S . . N1 N 0.2090(2) 0.3906(3) 0.5000 0.0224(8) Uani 1 2 d S . . N2 N 0.10483(18) 0.2209(3) 0.0000 0.0196(8) Uani 1 2 d S . . O1 O 0.31149(16) 0.6083(2) 0.41328(19) 0.0525(9) Uani 1 1 d . . . O2 O 0.13554(19) 0.6340(2) 0.30693(15) 0.0545(9) Uani 1 1 d . . . O3 O 0.28002(12) 0.2937(2) 0.08851(15) 0.0378(7) Uani 1 1 d . . . O4 O 0.15496(14) 0.47273(19) 0.19393(13) 0.0360(6) Uani 1 1 d . . . C1 C 0.2596(2) 0.5960(3) 0.4221(2) 0.0332(8) Uani 1 1 d . . . C2 C 0.1526(2) 0.6115(2) 0.35822(19) 0.0332(8) Uani 1 1 d . . . C3 C 0.1084(3) 0.7577(4) 0.5000 0.0518(18) Uani 1 2 d S . . C4 C 0.0572(4) 0.7156(5) 0.4702(4) 0.0326(16) Uani 0.50 1 d P . . C5 C 0.0367(3) 0.6278(4) 0.5000 0.0338(12) Uani 1 2 d S . . C6 C 0.12431(17) 0.3774(2) 0.39377(19) 0.0297(8) Uani 1 1 d . . . C7 C 0.08061(19) 0.4183(3) 0.3536(2) 0.0357(9) Uani 1 1 d . . . H7A H 0.0832 0.4791 0.3459 0.043 Uiso 1 1 calc R . . C8 C 0.0333(2) 0.3705(3) 0.3249(2) 0.0446(11) Uani 1 1 d . . . H8A H 0.0039 0.3987 0.2972 0.054 Uiso 1 1 calc R . . C9 C 0.0288(2) 0.2831(4) 0.3363(3) 0.0558(14) Uani 1 1 d . . . H9A H -0.0034 0.2505 0.3163 0.067 Uiso 1 1 calc R . . C10 C 0.0708(3) 0.2426(3) 0.3765(4) 0.0699(18) Uani 1 1 d . . . H10A H 0.0674 0.1819 0.3845 0.084 Uiso 1 1 calc R . . C11 C 0.1185(2) 0.2896(3) 0.4060(3) 0.0539(13) Uani 1 1 d . . . H11A H 0.1471 0.2611 0.4344 0.065 Uiso 1 1 calc R . . C12 C 0.25233(18) 0.3980(2) 0.37298(17) 0.0275(7) Uani 1 1 d . . . C13 C 0.2411(2) 0.3644(3) 0.30943(19) 0.0395(10) Uani 1 1 d . . . H13A H 0.2000 0.3584 0.2940 0.047 Uiso 1 1 calc R . . C14 C 0.2899(3) 0.3396(3) 0.2687(2) 0.0511(12) Uani 1 1 d . . . H14A H 0.2820 0.3158 0.2258 0.061 Uiso 1 1 calc R . . C15 C 0.3492(2) 0.3495(3) 0.2901(2) 0.0500(12) Uani 1 1 d . . . H15A H 0.3824 0.3327 0.2620 0.060 Uiso 1 1 calc R . . C16 C 0.3613(2) 0.3835(3) 0.3519(2) 0.0472(11) Uani 1 1 d . . . H16A H 0.4027 0.3908 0.3661 0.057 Uiso 1 1 calc R . . C17 C 0.31356(19) 0.4073(3) 0.3937(2) 0.0365(9) Uani 1 1 d . . . H17A H 0.3224 0.4300 0.4367 0.044 Uiso 1 1 calc R . . C18 C 0.23568(16) 0.3323(2) 0.07844(17) 0.0239(7) Uani 1 1 d . . . C19 C 0.15935(15) 0.4418(2) 0.14203(17) 0.0228(7) Uani 1 1 d . . . C20 C 0.0836(2) 0.5636(3) 0.0000 0.0255(10) Uani 1 2 d S . . C21 C 0.1382(3) 0.6119(5) 0.0272(4) 0.0291(15) Uani 0.50 1 d P . . C22 C 0.1976(3) 0.5954(4) 0.0000 0.0483(18) Uani 1 2 d S . . C23 C 0.03334(15) 0.2864(2) 0.10574(16) 0.0232(7) Uani 1 1 d . . . C24 C -0.0081(2) 0.2182(3) 0.0988(3) 0.0608(16) Uani 1 1 d . . . H24A H 0.0037 0.1674 0.0751 0.073 Uiso 1 1 calc R . . C25 C -0.0667(2) 0.2242(4) 0.1263(4) 0.078(2) Uani 1 1 d . . . H25A H -0.0944 0.1768 0.1218 0.093 Uiso 1 1 calc R . . C26 C -0.08496(19) 0.2969(3) 0.1599(2) 0.0423(10) Uani 1 1 d . . . H26A H -0.1255 0.3009 0.1776 0.051 Uiso 1 1 calc R . . C27 C -0.04452(17) 0.3637(3) 0.16770(17) 0.0299(8) Uani 1 1 d . . . H27A H -0.0565 0.4139 0.1920 0.036 Uiso 1 1 calc R . . C28 C 0.01449(16) 0.3589(2) 0.14021(17) 0.0269(7) Uani 1 1 d . . . H28A H 0.0420 0.4064 0.1454 0.032 Uiso 1 1 calc R . . C29 C 0.14231(16) 0.1942(2) 0.13015(17) 0.0237(7) Uani 1 1 d . . . C30 C 0.16985(18) 0.1180(3) 0.10918(19) 0.0318(8) Uani 1 1 d . . . H30A H 0.1712 0.1046 0.0629 0.038 Uiso 1 1 calc R . . C31 C 0.1957(2) 0.0603(3) 0.1550(2) 0.0414(10) Uani 1 1 d . . . H31A H 0.2137 0.0076 0.1399 0.050 Uiso 1 1 calc R . . C32 C 0.1953(2) 0.0795(3) 0.2216(2) 0.0460(11) Uani 1 1 d . . . H32A H 0.2139 0.0410 0.2527 0.055 Uiso 1 1 calc R . . C33 C 0.1675(3) 0.1555(3) 0.2432(2) 0.0614(16) Uani 1 1 d . . . H33A H 0.1667 0.1688 0.2894 0.074 Uiso 1 1 calc R . . C34 C 0.1409(3) 0.2121(3) 0.1979(2) 0.0487(13) Uani 1 1 d . . . H34A H 0.1215 0.2636 0.2134 0.058 Uiso 1 1 calc R . . C40 C 0.5000 0.5000 0.447(2) 0.165(14) Uiso 0.50 2 d SP . . Cl1 Cl 0.4380(3) 0.5270(4) 0.5000 0.188(2) Uiso 1 2 d S . . C41 C 0.0987(4) -0.0410(6) 0.0000 0.069(2) Uiso 1 2 d S . . O10 O 0.0567(3) 0.0332(5) 0.0000 0.090(2) Uiso 1 2 d S . . O11 O 0.5137(4) 0.4665(6) 0.3007(4) 0.074(2) Uiso 0.50 1 d P . . O12 O -0.0321(5) -0.0073(7) 0.1708(6) 0.098(3) Uiso 0.50 1 d P . . 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 0.0298(3) 0.0215(3) 0.0157(2) 0.00137(17) 0.00068(18) 0.00027(19) Fe2 0.0162(2) 0.0196(2) 0.0157(2) -0.00070(16) -0.00119(16) 0.00008(16) P1 0.0275(4) 0.0230(4) 0.0159(4) -0.0015(3) -0.0010(3) 0.0018(3) P2 0.0185(4) 0.0204(4) 0.0137(4) 0.0003(3) -0.0003(3) 0.0001(3) S1 0.0346(7) 0.0206(6) 0.0288(6) 0.000 0.000 -0.0016(5) S2 0.0290(6) 0.0214(6) 0.0203(5) 0.000 0.000 0.0003(5) S3 0.0159(5) 0.0222(5) 0.0174(5) 0.000 0.000 0.0012(4) S4 0.0192(5) 0.0223(6) 0.0282(6) 0.000 0.000 -0.0033(4) N1 0.032(2) 0.0208(19) 0.0150(18) 0.000 0.000 0.0027(16) N2 0.0203(19) 0.025(2) 0.0138(17) 0.000 0.000 -0.0023(15) O1 0.0429(19) 0.0470(19) 0.068(2) -0.0013(17) 0.0171(17) -0.0127(15) O2 0.090(3) 0.0457(18) 0.0280(16) 0.0088(14) -0.0163(16) 0.0004(18) O3 0.0255(14) 0.0443(16) 0.0438(16) 0.0008(13) -0.0061(12) 0.0104(12) O4 0.0432(16) 0.0426(16) 0.0223(13) -0.0086(12) -0.0007(11) 0.0030(13) C1 0.040(2) 0.0293(19) 0.0306(19) 0.0015(15) 0.0077(16) -0.0046(16) C2 0.048(2) 0.0255(19) 0.0262(19) 0.0020(14) -0.0036(17) 0.0015(16) C3 0.036(3) 0.023(3) 0.096(6) 0.000 0.000 0.007(2) C4 0.032(4) 0.031(4) 0.035(4) 0.000(3) 0.000(3) 0.008(3) C5 0.033(3) 0.026(3) 0.043(3) 0.000 0.000 0.007(2) C6 0.0297(18) 0.0323(19) 0.0270(18) -0.0106(15) -0.0033(14) 0.0003(15) C7 0.038(2) 0.042(2) 0.0273(19) -0.0005(16) -0.0076(16) 0.0008(17) C8 0.039(2) 0.063(3) 0.032(2) -0.011(2) -0.0115(18) 0.003(2) C9 0.046(3) 0.054(3) 0.067(3) -0.029(3) -0.019(2) -0.002(2) C10 0.062(3) 0.033(3) 0.115(5) -0.015(3) -0.034(3) -0.008(2) C11 0.050(3) 0.032(2) 0.080(4) -0.008(2) -0.027(3) 0.001(2) C12 0.0363(19) 0.0261(18) 0.0202(16) 0.0000(13) 0.0025(14) 0.0076(15) C13 0.051(3) 0.046(2) 0.0218(18) -0.0038(17) 0.0007(17) 0.010(2) C14 0.072(3) 0.056(3) 0.025(2) -0.0077(19) 0.010(2) 0.013(3) C15 0.058(3) 0.051(3) 0.041(3) 0.004(2) 0.023(2) 0.019(2) C16 0.037(2) 0.059(3) 0.046(3) 0.004(2) 0.012(2) 0.014(2) C17 0.036(2) 0.043(2) 0.030(2) -0.0023(17) 0.0024(16) 0.0065(17) C18 0.0234(17) 0.0279(17) 0.0205(16) -0.0024(13) -0.0022(12) -0.0005(13) C19 0.0212(16) 0.0240(17) 0.0232(17) 0.0032(13) -0.0016(13) 0.0002(12) C20 0.028(2) 0.020(2) 0.029(3) 0.000 0.000 0.0039(19) C21 0.032(4) 0.020(3) 0.034(3) -0.002(3) -0.002(3) 0.005(3) C22 0.035(3) 0.014(2) 0.096(6) 0.000 0.000 -0.003(2) C23 0.0195(15) 0.0308(17) 0.0193(15) 0.0003(13) 0.0048(12) -0.0016(13) C24 0.044(3) 0.050(3) 0.089(4) -0.034(3) 0.038(3) -0.022(2) C25 0.048(3) 0.067(4) 0.117(5) -0.042(4) 0.050(3) -0.034(3) C26 0.028(2) 0.061(3) 0.039(2) -0.002(2) 0.0156(17) -0.0043(19) C27 0.0280(18) 0.043(2) 0.0187(16) 0.0004(15) 0.0030(13) 0.0104(16) C28 0.0210(16) 0.0348(19) 0.0250(17) -0.0025(14) 0.0003(13) 0.0003(14) C29 0.0271(17) 0.0250(17) 0.0190(16) 0.0033(13) -0.0030(13) -0.0008(13) C30 0.0337(19) 0.039(2) 0.0231(18) 0.0014(15) 0.0029(15) 0.0134(16) C31 0.049(3) 0.040(2) 0.035(2) 0.0048(18) 0.0017(19) 0.021(2) C32 0.066(3) 0.039(2) 0.033(2) 0.0124(18) -0.012(2) 0.009(2) C33 0.121(5) 0.043(3) 0.021(2) 0.0004(18) -0.020(3) 0.021(3) C34 0.095(4) 0.030(2) 0.0209(19) -0.0027(16) -0.011(2) 0.019(2) _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 C1 1.758(4) . ? Fe1 C2 1.781(4) . ? Fe1 P1 2.2020(10) . ? Fe1 S1 2.2544(11) . ? Fe1 S2 2.2603(11) . ? Fe1 Fe1 2.4866(9) 6_556 ? Fe2 C18 1.766(4) . ? Fe2 C19 1.780(4) . ? Fe2 P2 2.1954(9) . ? Fe2 S3 2.2540(10) . ? Fe2 S4 2.2556(11) . ? Fe2 Fe2 2.4871(9) 6 ? P1 N1 1.701(2) . ? P1 C12 1.818(4) . ? P1 C6 1.832(4) . ? P2 N2 1.703(2) . ? P2 C29 1.817(3) . ? P2 C23 1.836(3) . ? S1 C3 1.830(6) . ? S1 Fe1 2.2544(11) 6_556 ? S2 C5 1.829(5) . ? S2 Fe1 2.2603(11) 6_556 ? S3 C20 1.832(5) . ? S3 Fe2 2.2540(10) 6 ? S4 C22 1.825(6) . ? S4 Fe2 2.2556(11) 6 ? N1 P1 1.701(2) 6_556 ? N2 P2 1.703(2) 6 ? O1 C1 1.155(5) . ? O2 C2 1.146(5) . ? O3 C18 1.149(4) . ? O4 C19 1.148(4) . ? C3 C4 1.417(10) 6_556 ? C3 C4 1.417(10) . ? C4 C4 1.193(16) 6_556 ? C4 C5 1.542(9) . ? C5 C4 1.542(9) 6_556 ? C6 C11 1.378(6) . ? C6 C7 1.393(5) . ? C7 C8 1.387(6) . ? C8 C9 1.368(7) . ? C9 C10 1.366(8) . ? C10 C11 1.395(7) . ? C12 C13 1.397(5) . ? C12 C17 1.399(6) . ? C13 C14 1.391(6) . ? C14 C15 1.364(8) . ? C15 C16 1.370(7) . ? C16 C17 1.381(6) . ? C20 C21 1.500(9) . ? C20 C21 1.500(9) 6 ? C21 C21 1.093(15) 6 ? C21 C22 1.424(9) . ? C22 C21 1.424(9) 6 ? C23 C28 1.374(5) . ? C23 C24 1.388(6) . ? C24 C25 1.389(6) . ? C25 C26 1.365(7) . ? C26 C27 1.360(6) . ? C27 C28 1.396(5) . ? C29 C30 1.382(5) . ? C29 C34 1.387(5) . ? C30 C31 1.395(5) . ? C31 C32 1.366(6) . ? C32 C33 1.385(7) . ? C33 C34 1.384(6) . ? C40 Cl1 1.77(2) 5_666 ? C40 Cl1 1.77(2) . ? Cl1 C40 1.77(2) 5_666 ? C41 O10 1.460(11) . ? O11 O11 1.191(16) 2_665 ? O12 O12 1.41(2) 2 ? 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 C1 Fe1 C2 97.63(19) . . ? C1 Fe1 P1 91.57(13) . . ? C2 Fe1 P1 101.96(13) . . ? C1 Fe1 S1 87.79(14) . . ? C2 Fe1 S1 105.84(13) . . ? P1 Fe1 S1 152.03(4) . . ? C1 Fe1 S2 155.92(14) . . ? C2 Fe1 S2 106.43(14) . . ? P1 Fe1 S2 84.54(4) . . ? S1 Fe1 S2 84.76(4) . . ? C1 Fe1 Fe1 100.43(13) . 6_556 ? C2 Fe1 Fe1 153.89(13) . 6_556 ? P1 Fe1 Fe1 96.25(3) . 6_556 ? S1 Fe1 Fe1 56.53(2) . 6_556 ? S2 Fe1 Fe1 56.63(2) . 6_556 ? C18 Fe2 C19 98.42(15) . . ? C18 Fe2 P2 90.15(12) . . ? C19 Fe2 P2 100.96(11) . . ? C18 Fe2 S3 156.14(11) . . ? C19 Fe2 S3 105.44(11) . . ? P2 Fe2 S3 85.74(4) . . ? C18 Fe2 S4 88.22(12) . . ? C19 Fe2 S4 107.45(11) . . ? P2 Fe2 S4 151.47(4) . . ? S3 Fe2 S4 84.36(4) . . ? C18 Fe2 Fe2 100.74(11) . 6 ? C19 Fe2 Fe2 154.33(11) . 6 ? P2 Fe2 Fe2 95.94(2) . 6 ? S3 Fe2 Fe2 56.515(19) . 6 ? S4 Fe2 Fe2 56.54(2) . 6 ? N1 P1 C12 101.02(17) . . ? N1 P1 C6 105.9(2) . . ? C12 P1 C6 101.50(17) . . ? N1 P1 Fe1 110.64(13) . . ? C12 P1 Fe1 118.04(13) . . ? C6 P1 Fe1 117.82(13) . . ? N2 P2 C29 103.46(17) . . ? N2 P2 C23 105.27(17) . . ? C29 P2 C23 100.13(16) . . ? N2 P2 Fe2 111.75(12) . . ? C29 P2 Fe2 115.67(11) . . ? C23 P2 Fe2 118.79(12) . . ? C3 S1 Fe1 111.92(17) . . ? C3 S1 Fe1 111.92(17) . 6_556 ? Fe1 S1 Fe1 66.94(4) . 6_556 ? C5 S2 Fe1 114.40(16) . 6_556 ? C5 S2 Fe1 114.40(16) . . ? Fe1 S2 Fe1 66.74(4) 6_556 . ? C20 S3 Fe2 113.99(14) . . ? C20 S3 Fe2 113.99(14) . 6 ? Fe2 S3 Fe2 66.97(4) . 6 ? C22 S4 Fe2 112.81(16) . 6 ? C22 S4 Fe2 112.81(16) . . ? Fe2 S4 Fe2 66.92(4) 6 . ? P1 N1 P1 121.4(2) 6_556 . ? P2 N2 P2 119.5(2) . 6 ? O1 C1 Fe1 178.0(4) . . ? O2 C2 Fe1 178.0(4) . . ? C4 C3 C4 49.8(7) 6_556 . ? C4 C3 S1 118.5(5) 6_556 . ? C4 C3 S1 118.5(5) . . ? C4 C4 C3 65.1(3) 6_556 . ? C4 C4 C5 67.2(3) 6_556 . ? C3 C4 C5 117.6(6) . . ? C4 C5 C4 45.5(6) 6_556 . ? C4 C5 S2 113.7(4) 6_556 . ? C4 C5 S2 113.7(4) . . ? C11 C6 C7 118.8(4) . . ? C11 C6 P1 120.5(3) . . ? C7 C6 P1 120.6(3) . . ? C8 C7 C6 120.3(4) . . ? C9 C8 C7 120.3(4) . . ? C10 C9 C8 119.9(4) . . ? C9 C10 C11 120.6(5) . . ? C6 C11 C10 120.1(5) . . ? C13 C12 C17 118.2(4) . . ? C13 C12 P1 122.1(3) . . ? C17 C12 P1 119.5(3) . . ? C14 C13 C12 120.3(4) . . ? C15 C14 C13 120.2(4) . . ? C14 C15 C16 120.4(4) . . ? C15 C16 C17 120.4(5) . . ? C16 C17 C12 120.4(4) . . ? O3 C18 Fe2 178.8(4) . . ? O4 C19 Fe2 178.4(3) . . ? C21 C20 C21 42.7(6) . 6 ? C21 C20 S3 115.8(4) . . ? C21 C20 S3 115.8(4) 6 . ? C21 C21 C22 67.4(3) 6 . ? C21 C21 C20 68.6(3) 6 . ? C22 C21 C20 119.1(5) . . ? C21 C22 C21 45.1(6) 6 . ? C21 C22 S4 118.7(4) 6 . ? C21 C22 S4 118.7(4) . . ? C28 C23 C24 118.1(3) . . ? C28 C23 P2 121.8(3) . . ? C24 C23 P2 120.0(3) . . ? C23 C24 C25 120.2(4) . . ? C26 C25 C24 121.1(4) . . ? C27 C26 C25 119.2(4) . . ? C26 C27 C28 120.4(4) . . ? C23 C28 C27 121.0(3) . . ? C30 C29 C34 118.4(3) . . ? C30 C29 P2 123.5(3) . . ? C34 C29 P2 118.0(3) . . ? C29 C30 C31 120.9(4) . . ? C32 C31 C30 120.3(4) . . ? C31 C32 C33 119.4(4) . . ? C34 C33 C32 120.5(4) . . ? C33 C34 C29 120.6(4) . . ? Cl1 C40 Cl1 105(2) 5_666 . ? C40 Cl1 C40 75(2) 5_666 . ? 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 C1 Fe1 P1 N1 88.8(2) . . . . ? C2 Fe1 P1 N1 -173.0(2) . . . . ? S1 Fe1 P1 N1 0.6(2) . . . . ? S2 Fe1 P1 N1 -67.36(16) . . . . ? Fe1 Fe1 P1 N1 -11.86(16) 6_556 . . . ? C1 Fe1 P1 C12 -26.78(19) . . . . ? C2 Fe1 P1 C12 71.4(2) . . . . ? S1 Fe1 P1 C12 -115.02(16) . . . . ? S2 Fe1 P1 C12 177.04(14) . . . . ? Fe1 Fe1 P1 C12 -127.45(14) 6_556 . . . ? C1 Fe1 P1 C6 -149.23(19) . . . . ? C2 Fe1 P1 C6 -51.1(2) . . . . ? S1 Fe1 P1 C6 122.53(17) . . . . ? S2 Fe1 P1 C6 54.59(14) . . . . ? Fe1 Fe1 P1 C6 110.10(14) 6_556 . . . ? C18 Fe2 P2 N2 -88.35(18) . . . . ? C19 Fe2 P2 N2 173.05(18) . . . . ? S3 Fe2 P2 N2 68.13(14) . . . . ? S4 Fe2 P2 N2 -1.79(18) . . . . ? Fe2 Fe2 P2 N2 12.46(14) 6 . . . ? C18 Fe2 P2 C29 29.67(17) . . . . ? C19 Fe2 P2 C29 -68.94(17) . . . . ? S3 Fe2 P2 C29 -173.85(13) . . . . ? S4 Fe2 P2 C29 116.23(15) . . . . ? Fe2 Fe2 P2 C29 130.48(13) 6 . . . ? C18 Fe2 P2 C23 148.79(17) . . . . ? C19 Fe2 P2 C23 50.19(17) . . . . ? S3 Fe2 P2 C23 -54.73(13) . . . . ? S4 Fe2 P2 C23 -124.65(15) . . . . ? Fe2 Fe2 P2 C23 -110.40(13) 6 . . . ? C1 Fe1 S1 C3 150.52(19) . . . . ? C2 Fe1 S1 C3 53.2(2) . . . . ? P1 Fe1 S1 C3 -120.29(16) . . . . ? S2 Fe1 S1 C3 -52.41(14) . . . . ? Fe1 Fe1 S1 C3 -105.43(14) 6_556 . . . ? C1 Fe1 S1 Fe1 -104.05(13) . . . 6_556 ? C2 Fe1 S1 Fe1 158.64(15) . . . 6_556 ? P1 Fe1 S1 Fe1 -14.86(12) . . . 6_556 ? S2 Fe1 S1 Fe1 53.02(4) . . . 6_556 ? C1 Fe1 S2 C5 127.0(4) . . . . ? C2 Fe1 S2 C5 -50.55(18) . . . . ? P1 Fe1 S2 C5 -151.43(13) . . . . ? S1 Fe1 S2 C5 54.45(13) . . . . ? Fe1 Fe1 S2 C5 107.38(13) 6_556 . . . ? C1 Fe1 S2 Fe1 19.6(3) . . . 6_556 ? C2 Fe1 S2 Fe1 -157.93(13) . . . 6_556 ? P1 Fe1 S2 Fe1 101.18(3) . . . 6_556 ? S1 Fe1 S2 Fe1 -52.94(4) . . . 6_556 ? C18 Fe2 S3 C20 -126.4(3) . . . . ? C19 Fe2 S3 C20 52.67(16) . . . . ? P2 Fe2 S3 C20 152.88(11) . . . . ? S4 Fe2 S3 C20 -53.92(11) . . . . ? Fe2 Fe2 S3 C20 -107.12(11) 6 . . . ? C18 Fe2 S3 Fe2 -19.3(3) . . . 6 ? C19 Fe2 S3 Fe2 159.79(11) . . . 6 ? P2 Fe2 S3 Fe2 -100.00(3) . . . 6 ? S4 Fe2 S3 Fe2 53.21(3) . . . 6 ? C18 Fe2 S4 C22 -149.75(17) . . . . ? C19 Fe2 S4 C22 -51.48(18) . . . . ? P2 Fe2 S4 C22 123.20(15) . . . . ? S3 Fe2 S4 C22 52.95(13) . . . . ? Fe2 Fe2 S4 C22 106.13(13) 6 . . . ? C18 Fe2 S4 Fe2 104.12(11) . . . 6 ? C19 Fe2 S4 Fe2 -157.62(11) . . . 6 ? P2 Fe2 S4 Fe2 17.07(10) . . . 6 ? S3 Fe2 S4 Fe2 -53.18(3) . . . 6 ? C12 P1 N1 P1 150.5(3) . . . 6_556 ? C6 P1 N1 P1 -104.1(3) . . . 6_556 ? Fe1 P1 N1 P1 24.7(3) . . . 6_556 ? C29 P2 N2 P2 -150.3(2) . . . 6 ? C23 P2 N2 P2 105.1(2) . . . 6 ? Fe2 P2 N2 P2 -25.2(3) . . . 6 ? C2 Fe1 C1 O1 124(12) . . . . ? P1 Fe1 C1 O1 -134(12) . . . . ? S1 Fe1 C1 O1 18(12) . . . . ? S2 Fe1 C1 O1 -54(12) . . . . ? Fe1 Fe1 C1 O1 -37(12) 6_556 . . . ? C1 Fe1 C2 O2 -44(13) . . . . ? P1 Fe1 C2 O2 -137(13) . . . . ? S1 Fe1 C2 O2 46(13) . . . . ? S2 Fe1 C2 O2 135(13) . . . . ? Fe1 Fe1 C2 O2 90(13) 6_556 . . . ? Fe1 S1 C3 C4 65.1(4) . . . 6_556 ? Fe1 S1 C3 C4 -7.8(5) 6_556 . . 6_556 ? Fe1 S1 C3 C4 7.8(5) . . . . ? Fe1 S1 C3 C4 -65.1(4) 6_556 . . . ? S1 C3 C4 C4 104.6(4) . . . 6_556 ? C4 C3 C4 C5 -43.6(6) 6_556 . . . ? S1 C3 C4 C5 61.0(7) . . . . ? C3 C4 C5 C4 42.7(6) . . . 6_556 ? C4 C4 C5 S2 -100.6(3) 6_556 . . . ? C3 C4 C5 S2 -57.9(6) . . . . ? Fe1 S2 C5 C4 12.2(4) 6_556 . . 6_556 ? Fe1 S2 C5 C4 -62.1(3) . . . 6_556 ? Fe1 S2 C5 C4 62.1(3) 6_556 . . . ? Fe1 S2 C5 C4 -12.2(4) . . . . ? N1 P1 C6 C11 -33.2(4) . . . . ? C12 P1 C6 C11 71.9(4) . . . . ? Fe1 P1 C6 C11 -157.6(4) . . . . ? N1 P1 C6 C7 150.1(3) . . . . ? C12 P1 C6 C7 -104.8(3) . . . . ? Fe1 P1 C6 C7 25.8(4) . . . . ? C11 C6 C7 C8 -1.9(6) . . . . ? P1 C6 C7 C8 174.8(3) . . . . ? C6 C7 C8 C9 0.6(7) . . . . ? C7 C8 C9 C10 0.5(8) . . . . ? C8 C9 C10 C11 -0.3(10) . . . . ? C7 C6 C11 C10 2.1(8) . . . . ? P1 C6 C11 C10 -174.6(5) . . . . ? C9 C10 C11 C6 -1.0(10) . . . . ? N1 P1 C12 C13 133.8(3) . . . . ? C6 P1 C12 C13 24.9(4) . . . . ? Fe1 P1 C12 C13 -105.5(3) . . . . ? N1 P1 C12 C17 -51.5(4) . . . . ? C6 P1 C12 C17 -160.4(3) . . . . ? Fe1 P1 C12 C17 69.2(3) . . . . ? C17 C12 C13 C14 1.0(6) . . . . ? P1 C12 C13 C14 175.8(4) . . . . ? C12 C13 C14 C15 -1.2(7) . . . . ? C13 C14 C15 C16 0.2(8) . . . . ? C14 C15 C16 C17 0.8(8) . . . . ? C15 C16 C17 C12 -0.9(7) . . . . ? C13 C12 C17 C16 0.0(6) . . . . ? P1 C12 C17 C16 -174.9(3) . . . . ? C19 Fe2 C18 O3 -103(17) . . . . ? P2 Fe2 C18 O3 156(17) . . . . ? S3 Fe2 C18 O3 76(17) . . . . ? S4 Fe2 C18 O3 5(17) . . . . ? Fe2 Fe2 C18 O3 60(17) 6 . . . ? C18 Fe2 C19 O4 23(11) . . . . ? P2 Fe2 C19 O4 114(11) . . . . ? S3 Fe2 C19 O4 -157(11) . . . . ? S4 Fe2 C19 O4 -68(11) . . . . ? Fe2 Fe2 C19 O4 -115(11) 6 . . . ? Fe2 S3 C20 C21 13.3(4) . . . . ? Fe2 S3 C20 C21 -61.0(3) 6 . . . ? Fe2 S3 C20 C21 61.0(3) . . . 6 ? Fe2 S3 C20 C21 -13.3(4) 6 . . 6 ? S3 C20 C21 C21 100.9(2) . . . 6 ? C21 C20 C21 C22 -46.4(6) 6 . . . ? S3 C20 C21 C22 54.5(6) . . . . ? C20 C21 C22 C21 46.9(6) . . . 6 ? C21 C21 C22 S4 -103.1(3) 6 . . . ? C20 C21 C22 S4 -56.2(6) . . . . ? Fe2 S4 C22 C21 10.8(4) 6 . . 6 ? Fe2 S4 C22 C21 -62.6(4) . . . 6 ? Fe2 S4 C22 C21 62.6(4) 6 . . . ? Fe2 S4 C22 C21 -10.8(4) . . . . ? N2 P2 C23 C28 -144.8(3) . . . . ? C29 P2 C23 C28 108.1(3) . . . . ? Fe2 P2 C23 C28 -18.8(3) . . . . ? N2 P2 C23 C24 38.6(4) . . . . ? C29 P2 C23 C24 -68.5(4) . . . . ? Fe2 P2 C23 C24 164.6(4) . . . . ? C28 C23 C24 C25 -0.2(9) . . . . ? P2 C23 C24 C25 176.5(5) . . . . ? C23 C24 C25 C26 0.8(11) . . . . ? C24 C25 C26 C27 -1.6(10) . . . . ? C25 C26 C27 C28 1.7(7) . . . . ? C24 C23 C28 C27 0.3(6) . . . . ? P2 C23 C28 C27 -176.3(3) . . . . ? C26 C27 C28 C23 -1.1(6) . . . . ? N2 P2 C29 C30 18.0(4) . . . . ? C23 P2 C29 C30 126.6(3) . . . . ? Fe2 P2 C29 C30 -104.5(3) . . . . ? N2 P2 C29 C34 -166.0(4) . . . . ? C23 P2 C29 C34 -57.5(4) . . . . ? Fe2 P2 C29 C34 71.5(4) . . . . ? C34 C29 C30 C31 -0.1(6) . . . . ? P2 C29 C30 C31 175.9(3) . . . . ? C29 C30 C31 C32 -1.4(7) . . . . ? C30 C31 C32 C33 1.7(8) . . . . ? C31 C32 C33 C34 -0.6(9) . . . . ? C32 C33 C34 C29 -0.9(9) . . . . ? C30 C29 C34 C33 1.2(7) . . . . ? P2 C29 C34 C33 -175.0(4) . . . . ? Cl1 C40 Cl1 C40 0.000(7) 5_666 . . 5_666 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.832 _refine_diff_density_min -2.255 _refine_diff_density_rms 0.135 data_str0463 _database_code_depnum_ccdc_archive 'CCDC 919234' #TrackingRef 'STR0463.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H31 Fe2 N O4 P2 S2' _chemical_formula_weight 755.36 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1bar loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8977(5) _cell_length_b 10.2309(6) _cell_length_c 19.2787(11) _cell_angle_alpha 89.0140(10) _cell_angle_beta 79.5570(10) _cell_angle_gamma 75.4280(10) _cell_volume 1669.64(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 1.129 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7734 _exptl_absorpt_correction_T_max 0.8580 _exptl_absorpt_process_details ? _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 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14741 _diffrn_reflns_av_R_equivalents 0.0127 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 28.25 _reflns_number_total 7671 _reflns_number_gt 7151 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0380P)^2^+0.8205P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 7671 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0701 _refine_ls_wR_factor_gt 0.0689 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.98468(2) 0.59488(2) 0.208605(10) 0.01725(6) Uani 1 1 d . . . Fe2 Fe 0.87880(2) 0.68785(2) 0.330736(10) 0.01638(6) Uani 1 1 d . . . P1 P 0.76343(4) 0.68615(4) 0.169791(18) 0.01594(8) Uani 1 1 d . . . P2 P 0.64051(4) 0.79684(4) 0.315263(18) 0.01473(8) Uani 1 1 d . . . S1 S 0.83299(4) 0.49817(4) 0.289308(18) 0.01810(8) Uani 1 1 d . . . S2 S 1.13583(4) 0.58508(4) 0.29153(2) 0.02214(8) Uani 1 1 d . . . N1 N 0.60977(14) 0.77575(12) 0.23172(6) 0.0161(2) Uani 1 1 d . . . O1 O 1.17996(15) 0.76043(14) 0.13304(7) 0.0357(3) Uani 1 1 d . . . O2 O 1.12334(19) 0.36209(15) 0.11194(8) 0.0478(4) Uani 1 1 d . . . O3 O 0.98132(16) 0.93806(14) 0.31716(8) 0.0407(3) Uani 1 1 d . . . O4 O 0.80975(16) 0.67651(16) 0.48436(6) 0.0408(3) Uani 1 1 d . . . C1 C 1.09759(18) 0.69959(17) 0.16260(8) 0.0241(3) Uani 1 1 d . . . C2 C 1.0679(2) 0.45373(17) 0.14935(9) 0.0273(3) Uani 1 1 d . . . C3 C 0.93887(18) 0.84070(17) 0.32277(9) 0.0250(3) Uani 1 1 d . . . C4 C 0.83730(18) 0.68002(17) 0.42409(8) 0.0239(3) Uani 1 1 d . . . C5 C 0.9491(2) 0.34171(16) 0.32073(9) 0.0283(3) Uani 1 1 d . . . H5A H 0.8767 0.2958 0.3485 0.034 Uiso 1 1 calc R . . H5B H 1.0047 0.2836 0.2801 0.034 Uiso 1 1 calc R . . C6 C 1.0676(2) 0.35745(18) 0.36434(10) 0.0321(4) Uani 1 1 d . . . H6A H 1.1146 0.2697 0.3814 0.039 Uiso 1 1 calc R . . H6B H 1.0128 0.4157 0.4051 0.039 Uiso 1 1 calc R . . C7 C 1.19772(19) 0.41568(18) 0.32513(9) 0.0299(4) Uani 1 1 d . . . H7A H 1.2547 0.3550 0.2856 0.036 Uiso 1 1 calc R . . H7B H 1.2712 0.4175 0.3564 0.036 Uiso 1 1 calc R . . C8 C 0.45228(17) 0.82835(15) 0.21080(8) 0.0198(3) Uani 1 1 d . . . H8A H 0.3715 0.8172 0.2500 0.024 Uiso 1 1 calc R . . H8B H 0.4469 0.7726 0.1716 0.024 Uiso 1 1 calc R . . C9 C 0.41278(19) 0.97313(16) 0.18990(8) 0.0248(3) Uani 1 1 d . . . H9A H 0.4906 1.0042 0.1605 0.030 Uiso 1 1 calc R . . C10 C 0.2749(2) 1.05868(19) 0.21066(10) 0.0353(4) Uani 1 1 d . . . H10A H 0.1947 1.0306 0.2401 0.042 Uiso 1 1 calc R . . H10B H 0.2574 1.1474 0.1959 0.042 Uiso 1 1 calc R . . C11 C 0.68309(18) 0.55811(15) 0.13511(8) 0.0204(3) Uani 1 1 d . . . C12 C 0.55574(19) 0.51598(16) 0.17311(9) 0.0237(3) Uani 1 1 d . . . H12A H 0.5070 0.5547 0.2174 0.028 Uiso 1 1 calc R . . C13 C 0.5011(2) 0.41590(18) 0.14489(10) 0.0330(4) Uani 1 1 d . . . H13A H 0.4149 0.3892 0.1701 0.040 Uiso 1 1 calc R . . C14 C 0.5741(3) 0.35671(19) 0.07998(11) 0.0396(4) Uani 1 1 d . . . H14A H 0.5364 0.2908 0.0611 0.048 Uiso 1 1 calc R . . C15 C 0.7034(3) 0.3948(2) 0.04265(10) 0.0390(4) Uani 1 1 d . . . H15A H 0.7537 0.3534 -0.0009 0.047 Uiso 1 1 calc R . . C16 C 0.7584(2) 0.49460(17) 0.07002(9) 0.0290(3) Uani 1 1 d . . . H16A H 0.8460 0.5194 0.0449 0.035 Uiso 1 1 calc R . . C17 C 0.76663(18) 0.80778(15) 0.09921(8) 0.0216(3) Uani 1 1 d . . . C18 C 0.6942(2) 0.80627(18) 0.04112(9) 0.0308(4) Uani 1 1 d . . . H18A H 0.6464 0.7373 0.0350 0.037 Uiso 1 1 calc R . . C19 C 0.6934(3) 0.9081(2) -0.00785(10) 0.0426(5) Uani 1 1 d . . . H19A H 0.6475 0.9053 -0.0473 0.051 Uiso 1 1 calc R . . C20 C 0.7597(3) 1.0125(2) 0.00159(11) 0.0457(5) Uani 1 1 d . . . H20A H 0.7574 1.0806 -0.0311 0.055 Uiso 1 1 calc R . . C21 C 0.8298(2) 1.01650(19) 0.05961(11) 0.0399(5) Uani 1 1 d . . . H21A H 0.8737 1.0877 0.0663 0.048 Uiso 1 1 calc R . . C22 C 0.83467(19) 0.91424(17) 0.10787(9) 0.0286(3) Uani 1 1 d . . . H22A H 0.8837 0.9164 0.1464 0.034 Uiso 1 1 calc R . . C23 C 0.46876(17) 0.76115(15) 0.37343(7) 0.0181(3) Uani 1 1 d . . . C24 C 0.32361(18) 0.85797(17) 0.38851(8) 0.0248(3) Uani 1 1 d . . . H24A H 0.3119 0.9417 0.3677 0.030 Uiso 1 1 calc R . . C25 C 0.19698(19) 0.8295(2) 0.43441(9) 0.0306(4) Uani 1 1 d . . . H25A H 0.1014 0.8947 0.4446 0.037 Uiso 1 1 calc R . . C26 C 0.2123(2) 0.7048(2) 0.46504(9) 0.0316(4) Uani 1 1 d . . . H26A H 0.1268 0.6861 0.4954 0.038 Uiso 1 1 calc R . . C27 C 0.3540(2) 0.60814(18) 0.45062(9) 0.0278(3) Uani 1 1 d . . . H27A H 0.3642 0.5241 0.4711 0.033 Uiso 1 1 calc R . . C28 C 0.48211(18) 0.63647(16) 0.40533(8) 0.0220(3) Uani 1 1 d . . . H28A H 0.5778 0.5713 0.3963 0.026 Uiso 1 1 calc R . . C29 C 0.60538(17) 0.97824(14) 0.33229(8) 0.0189(3) Uani 1 1 d . . . C30 C 0.5716(2) 1.02540(17) 0.40214(9) 0.0279(3) Uani 1 1 d . . . H30A H 0.5559 0.9664 0.4384 0.033 Uiso 1 1 calc R . . C31 C 0.5610(2) 1.15934(18) 0.41829(10) 0.0346(4) Uani 1 1 d . . . H31A H 0.5381 1.1900 0.4651 0.042 Uiso 1 1 calc R . . C32 C 0.5847(2) 1.24686(17) 0.36459(11) 0.0341(4) Uani 1 1 d . . . H32A H 0.5753 1.3372 0.3752 0.041 Uiso 1 1 calc R . . C33 C 0.6221(2) 1.20131(17) 0.29537(10) 0.0323(4) Uani 1 1 d . . . H33A H 0.6403 1.2603 0.2594 0.039 Uiso 1 1 calc R . . C34 C 0.63283(19) 1.06665(16) 0.27908(9) 0.0250(3) Uani 1 1 d . . . H34A H 0.6585 1.0360 0.2322 0.030 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 0.01578(10) 0.02042(11) 0.01408(10) 0.00037(8) -0.00139(7) -0.00282(8) Fe2 0.01558(10) 0.01987(11) 0.01390(10) 0.00037(8) -0.00293(7) -0.00468(8) P1 0.01746(17) 0.01706(17) 0.01274(16) 0.00016(13) -0.00224(13) -0.00368(13) P2 0.01596(17) 0.01512(16) 0.01295(16) -0.00035(12) -0.00187(12) -0.00411(13) S1 0.01838(16) 0.01757(16) 0.01755(16) 0.00147(13) -0.00303(13) -0.00330(13) S2 0.01596(17) 0.0300(2) 0.01986(17) 0.00189(14) -0.00394(13) -0.00438(14) N1 0.0157(5) 0.0190(6) 0.0127(5) -0.0016(4) -0.0031(4) -0.0023(4) O1 0.0294(6) 0.0486(8) 0.0338(7) 0.0150(6) -0.0065(5) -0.0189(6) O2 0.0534(9) 0.0382(8) 0.0398(8) -0.0151(6) -0.0049(7) 0.0090(7) O3 0.0327(7) 0.0332(7) 0.0641(10) 0.0103(6) -0.0161(6) -0.0182(6) O4 0.0384(7) 0.0656(10) 0.0182(6) 0.0032(6) -0.0050(5) -0.0127(7) C1 0.0208(7) 0.0324(8) 0.0185(7) 0.0032(6) -0.0049(6) -0.0052(6) C2 0.0259(8) 0.0295(8) 0.0227(8) -0.0006(6) -0.0038(6) -0.0006(6) C3 0.0185(7) 0.0292(8) 0.0281(8) 0.0032(6) -0.0067(6) -0.0063(6) C4 0.0198(7) 0.0311(8) 0.0212(7) -0.0002(6) -0.0057(6) -0.0060(6) C5 0.0287(8) 0.0201(7) 0.0341(9) 0.0082(6) -0.0069(7) -0.0022(6) C6 0.0314(9) 0.0307(9) 0.0311(9) 0.0075(7) -0.0090(7) 0.0002(7) C7 0.0211(8) 0.0337(9) 0.0315(9) 0.0049(7) -0.0090(6) 0.0023(7) C8 0.0173(7) 0.0233(7) 0.0185(7) -0.0004(5) -0.0054(5) -0.0031(5) C9 0.0255(8) 0.0262(8) 0.0227(7) 0.0027(6) -0.0080(6) -0.0040(6) C10 0.0317(9) 0.0286(9) 0.0391(10) 0.0034(7) -0.0028(7) 0.0012(7) C11 0.0239(7) 0.0194(7) 0.0180(7) -0.0011(5) -0.0073(6) -0.0033(6) C12 0.0258(8) 0.0216(7) 0.0246(8) 0.0008(6) -0.0071(6) -0.0062(6) C13 0.0340(9) 0.0281(8) 0.0422(10) 0.0021(7) -0.0135(8) -0.0134(7) C14 0.0504(12) 0.0297(9) 0.0459(11) -0.0078(8) -0.0217(9) -0.0135(8) C15 0.0530(12) 0.0337(10) 0.0298(9) -0.0128(8) -0.0093(8) -0.0079(9) C16 0.0335(9) 0.0290(8) 0.0223(8) -0.0055(6) -0.0031(6) -0.0052(7) C17 0.0213(7) 0.0220(7) 0.0165(7) 0.0039(5) 0.0018(5) -0.0002(6) C18 0.0367(9) 0.0311(9) 0.0193(7) 0.0025(6) -0.0040(7) 0.0003(7) C19 0.0535(12) 0.0421(11) 0.0203(8) 0.0089(8) -0.0040(8) 0.0073(9) C20 0.0480(12) 0.0385(11) 0.0346(10) 0.0214(8) 0.0090(9) 0.0053(9) C21 0.0326(9) 0.0278(9) 0.0509(12) 0.0133(8) 0.0079(8) -0.0043(7) C22 0.0226(8) 0.0265(8) 0.0325(9) 0.0061(7) 0.0016(6) -0.0037(6) C23 0.0188(7) 0.0227(7) 0.0137(6) -0.0021(5) -0.0016(5) -0.0079(6) C24 0.0208(7) 0.0299(8) 0.0219(7) 0.0017(6) -0.0030(6) -0.0037(6) C25 0.0186(7) 0.0441(10) 0.0261(8) -0.0015(7) -0.0009(6) -0.0046(7) C26 0.0232(8) 0.0531(11) 0.0220(8) 0.0017(7) -0.0003(6) -0.0185(8) C27 0.0330(9) 0.0323(9) 0.0226(8) 0.0047(6) -0.0037(6) -0.0175(7) C28 0.0233(7) 0.0233(7) 0.0202(7) -0.0003(6) -0.0020(6) -0.0084(6) C29 0.0181(7) 0.0169(6) 0.0215(7) -0.0020(5) -0.0039(5) -0.0039(5) C30 0.0349(9) 0.0261(8) 0.0227(8) -0.0047(6) -0.0001(6) -0.0109(7) C31 0.0372(10) 0.0296(9) 0.0359(10) -0.0150(7) 0.0008(8) -0.0105(7) C32 0.0300(9) 0.0185(7) 0.0544(12) -0.0083(7) -0.0098(8) -0.0053(7) C33 0.0361(9) 0.0211(8) 0.0450(10) 0.0091(7) -0.0160(8) -0.0110(7) C34 0.0288(8) 0.0221(7) 0.0261(8) 0.0024(6) -0.0086(6) -0.0079(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 1.7689(16) . ? Fe1 C2 1.7751(17) . ? Fe1 P1 2.2119(4) . ? Fe1 S1 2.2537(4) . ? Fe1 S2 2.2540(4) . ? Fe1 Fe2 2.4816(3) . ? Fe2 C3 1.7712(17) . ? Fe2 C4 1.7750(16) . ? Fe2 P2 2.2036(4) . ? Fe2 S2 2.2579(4) . ? Fe2 S1 2.2671(4) . ? P1 N1 1.7177(12) . ? P1 C17 1.8293(15) . ? P1 C11 1.8300(15) . ? P2 N1 1.7078(12) . ? P2 C29 1.8280(15) . ? P2 C23 1.8362(15) . ? S1 C5 1.8326(16) . ? S2 C7 1.8267(18) . ? N1 C8 1.4946(18) . ? O1 C1 1.147(2) . ? O2 C2 1.142(2) . ? O3 C3 1.148(2) . ? O4 C4 1.145(2) . ? C5 C6 1.501(2) . ? C6 C7 1.511(3) . ? C8 C9 1.500(2) . ? C9 C10 1.313(2) . ? C11 C12 1.393(2) . ? C11 C16 1.396(2) . ? C12 C13 1.395(2) . ? C13 C14 1.374(3) . ? C14 C15 1.382(3) . ? C15 C16 1.387(2) . ? C17 C18 1.392(2) . ? C17 C22 1.398(2) . ? C18 C19 1.393(2) . ? C19 C20 1.373(3) . ? C20 C21 1.382(3) . ? C21 C22 1.386(2) . ? C23 C28 1.394(2) . ? C23 C24 1.401(2) . ? C24 C25 1.390(2) . ? C25 C26 1.382(3) . ? C26 C27 1.379(3) . ? C27 C28 1.393(2) . ? C29 C34 1.385(2) . ? C29 C30 1.393(2) . ? C30 C31 1.387(2) . ? C31 C32 1.379(3) . ? C32 C33 1.375(3) . ? C33 C34 1.394(2) . ? 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 C1 Fe1 C2 95.14(8) . . ? C1 Fe1 P1 96.70(5) . . ? C2 Fe1 P1 101.09(6) . . ? C1 Fe1 S1 165.84(5) . . ? C2 Fe1 S1 98.23(6) . . ? P1 Fe1 S1 85.310(15) . . ? C1 Fe1 S2 86.13(5) . . ? C2 Fe1 S2 108.88(6) . . ? P1 Fe1 S2 149.547(17) . . ? S1 Fe1 S2 85.159(15) . . ? C1 Fe1 Fe2 108.87(5) . . ? C2 Fe1 Fe2 149.81(6) . . ? P1 Fe1 Fe2 94.161(13) . . ? S1 Fe1 Fe2 56.965(11) . . ? S2 Fe1 Fe2 56.707(12) . . ? C3 Fe2 C4 99.56(8) . . ? C3 Fe2 P2 90.13(5) . . ? C4 Fe2 P2 97.95(5) . . ? C3 Fe2 S2 85.72(5) . . ? C4 Fe2 S2 108.99(5) . . ? P2 Fe2 S2 153.064(17) . . ? C3 Fe2 S1 154.81(6) . . ? C4 Fe2 S1 105.59(5) . . ? P2 Fe2 S1 87.899(15) . . ? S2 Fe2 S1 84.759(15) . . ? C3 Fe2 Fe1 99.09(5) . . ? C4 Fe2 Fe1 155.28(5) . . ? P2 Fe2 Fe1 98.098(13) . . ? S2 Fe2 Fe1 56.558(11) . . ? S1 Fe2 Fe1 56.450(11) . . ? N1 P1 C17 100.95(6) . . ? N1 P1 C11 104.04(7) . . ? C17 P1 C11 103.56(7) . . ? N1 P1 Fe1 115.67(4) . . ? C17 P1 Fe1 118.94(5) . . ? C11 P1 Fe1 111.86(5) . . ? N1 P2 C29 107.37(6) . . ? N1 P2 C23 104.87(6) . . ? C29 P2 C23 100.95(7) . . ? N1 P2 Fe2 112.86(4) . . ? C29 P2 Fe2 111.01(5) . . ? C23 P2 Fe2 118.64(5) . . ? C5 S1 Fe1 111.42(6) . . ? C5 S1 Fe2 113.67(6) . . ? Fe1 S1 Fe2 66.585(13) . . ? C7 S2 Fe1 113.14(6) . . ? C7 S2 Fe2 113.63(6) . . ? Fe1 S2 Fe2 66.735(13) . . ? C8 N1 P2 122.50(9) . . ? C8 N1 P1 118.39(9) . . ? P2 N1 P1 119.07(7) . . ? O1 C1 Fe1 175.24(15) . . ? O2 C2 Fe1 178.82(16) . . ? O3 C3 Fe2 178.43(15) . . ? O4 C4 Fe2 179.23(17) . . ? C6 C5 S1 116.08(12) . . ? C5 C6 C7 114.05(15) . . ? C6 C7 S2 116.17(11) . . ? N1 C8 C9 116.40(12) . . ? C10 C9 C8 123.95(16) . . ? C12 C11 C16 118.84(15) . . ? C12 C11 P1 122.41(11) . . ? C16 C11 P1 118.62(13) . . ? C11 C12 C13 120.16(15) . . ? C14 C13 C12 120.24(18) . . ? C13 C14 C15 120.17(16) . . ? C14 C15 C16 120.12(17) . . ? C15 C16 C11 120.41(17) . . ? C18 C17 C22 118.75(15) . . ? C18 C17 P1 123.74(13) . . ? C22 C17 P1 117.28(12) . . ? C17 C18 C19 119.99(18) . . ? C20 C19 C18 120.61(19) . . ? C19 C20 C21 120.05(17) . . ? C20 C21 C22 119.91(19) . . ? C21 C22 C17 120.66(18) . . ? C28 C23 C24 118.35(14) . . ? C28 C23 P2 119.98(11) . . ? C24 C23 P2 121.65(12) . . ? C25 C24 C23 120.37(16) . . ? C26 C25 C24 120.37(16) . . ? C27 C26 C25 120.05(15) . . ? C26 C27 C28 119.92(16) . . ? C27 C28 C23 120.92(15) . . ? C34 C29 C30 118.80(14) . . ? C34 C29 P2 122.31(12) . . ? C30 C29 P2 118.25(12) . . ? C31 C30 C29 120.77(16) . . ? C32 C31 C30 119.66(17) . . ? C33 C32 C31 120.38(15) . . ? C32 C33 C34 119.99(17) . . ? C29 C34 C33 120.35(16) . . ? 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 C1 Fe1 Fe2 C3 6.73(7) . . . . ? C2 Fe1 Fe2 C3 147.64(12) . . . . ? P1 Fe1 Fe2 C3 -91.80(5) . . . . ? S1 Fe1 Fe2 C3 -173.46(5) . . . . ? S2 Fe1 Fe2 C3 78.69(5) . . . . ? C1 Fe1 Fe2 C4 -131.82(13) . . . . ? C2 Fe1 Fe2 C4 9.08(17) . . . . ? P1 Fe1 Fe2 C4 129.65(12) . . . . ? S1 Fe1 Fe2 C4 47.99(12) . . . . ? S2 Fe1 Fe2 C4 -59.87(12) . . . . ? C1 Fe1 Fe2 P2 98.17(5) . . . . ? C2 Fe1 Fe2 P2 -120.93(11) . . . . ? P1 Fe1 Fe2 P2 -0.365(16) . . . . ? S1 Fe1 Fe2 P2 -82.022(16) . . . . ? S2 Fe1 Fe2 P2 170.124(18) . . . . ? C1 Fe1 Fe2 S2 -71.95(5) . . . . ? C2 Fe1 Fe2 S2 68.95(11) . . . . ? P1 Fe1 Fe2 S2 -170.489(18) . . . . ? S1 Fe1 Fe2 S2 107.854(18) . . . . ? C1 Fe1 Fe2 S1 -179.81(5) . . . . ? C2 Fe1 Fe2 S1 -38.90(11) . . . . ? P1 Fe1 Fe2 S1 81.656(16) . . . . ? S2 Fe1 Fe2 S1 -107.854(18) . . . . ? C1 Fe1 P1 N1 -111.31(7) . . . . ? C2 Fe1 P1 N1 152.08(8) . . . . ? S1 Fe1 P1 N1 54.60(5) . . . . ? S2 Fe1 P1 N1 -17.55(6) . . . . ? Fe2 Fe1 P1 N1 -1.73(5) . . . . ? C1 Fe1 P1 C17 9.13(8) . . . . ? C2 Fe1 P1 C17 -87.47(8) . . . . ? S1 Fe1 P1 C17 175.04(6) . . . . ? S2 Fe1 P1 C17 102.89(6) . . . . ? Fe2 Fe1 P1 C17 118.71(6) . . . . ? C1 Fe1 P1 C11 129.82(8) . . . . ? C2 Fe1 P1 C11 33.22(8) . . . . ? S1 Fe1 P1 C11 -64.27(5) . . . . ? S2 Fe1 P1 C11 -136.41(6) . . . . ? Fe2 Fe1 P1 C11 -120.60(5) . . . . ? C3 Fe2 P2 N1 101.62(7) . . . . ? C4 Fe2 P2 N1 -158.71(7) . . . . ? S2 Fe2 P2 N1 20.84(6) . . . . ? S1 Fe2 P2 N1 -53.26(5) . . . . ? Fe1 Fe2 P2 N1 2.42(5) . . . . ? C3 Fe2 P2 C29 -18.98(8) . . . . ? C4 Fe2 P2 C29 80.69(8) . . . . ? S2 Fe2 P2 C29 -99.76(6) . . . . ? S1 Fe2 P2 C29 -173.86(5) . . . . ? Fe1 Fe2 P2 C29 -118.18(5) . . . . ? C3 Fe2 P2 C23 -135.18(7) . . . . ? C4 Fe2 P2 C23 -35.51(8) . . . . ? S2 Fe2 P2 C23 144.04(6) . . . . ? S1 Fe2 P2 C23 69.94(5) . . . . ? Fe1 Fe2 P2 C23 125.62(5) . . . . ? C1 Fe1 S1 C5 -106.7(2) . . . . ? C2 Fe1 S1 C5 53.92(8) . . . . ? P1 Fe1 S1 C5 154.47(6) . . . . ? S2 Fe1 S1 C5 -54.48(6) . . . . ? Fe2 Fe1 S1 C5 -107.47(6) . . . . ? C1 Fe1 S1 Fe2 0.7(2) . . . . ? C2 Fe1 S1 Fe2 161.39(6) . . . . ? P1 Fe1 S1 Fe2 -98.059(14) . . . . ? S2 Fe1 S1 Fe2 52.984(13) . . . . ? C3 Fe2 S1 C5 119.48(14) . . . . ? C4 Fe2 S1 C5 -57.02(8) . . . . ? P2 Fe2 S1 C5 -154.69(6) . . . . ? S2 Fe2 S1 C5 51.26(6) . . . . ? Fe1 Fe2 S1 C5 104.16(6) . . . . ? C3 Fe2 S1 Fe1 15.32(12) . . . . ? C4 Fe2 S1 Fe1 -161.18(5) . . . . ? P2 Fe2 S1 Fe1 101.156(14) . . . . ? S2 Fe2 S1 Fe1 -52.901(13) . . . . ? C1 Fe1 S2 C7 -137.49(8) . . . . ? C2 Fe1 S2 C7 -43.37(9) . . . . ? P1 Fe1 S2 C7 125.87(7) . . . . ? S1 Fe1 S2 C7 53.69(6) . . . . ? Fe2 Fe1 S2 C7 106.90(6) . . . . ? C1 Fe1 S2 Fe2 115.61(5) . . . . ? C2 Fe1 S2 Fe2 -150.27(6) . . . . ? P1 Fe1 S2 Fe2 18.97(3) . . . . ? S1 Fe1 S2 Fe2 -53.208(13) . . . . ? C3 Fe2 S2 C7 149.96(8) . . . . ? C4 Fe2 S2 C7 51.31(9) . . . . ? P2 Fe2 S2 C7 -128.21(7) . . . . ? S1 Fe2 S2 C7 -53.39(7) . . . . ? Fe1 Fe2 S2 C7 -106.20(7) . . . . ? C3 Fe2 S2 Fe1 -103.85(5) . . . . ? C4 Fe2 S2 Fe1 157.51(6) . . . . ? P2 Fe2 S2 Fe1 -22.02(4) . . . . ? S1 Fe2 S2 Fe1 52.806(13) . . . . ? C29 P2 N1 C8 -63.66(12) . . . . ? C23 P2 N1 C8 43.13(12) . . . . ? Fe2 P2 N1 C8 173.69(10) . . . . ? C29 P2 N1 P1 118.47(8) . . . . ? C23 P2 N1 P1 -134.73(8) . . . . ? Fe2 P2 N1 P1 -4.18(9) . . . . ? C17 P1 N1 C8 56.22(12) . . . . ? C11 P1 N1 C8 -50.91(12) . . . . ? Fe1 P1 N1 C8 -174.00(9) . . . . ? C17 P1 N1 P2 -125.83(9) . . . . ? C11 P1 N1 P2 127.04(8) . . . . ? Fe1 P1 N1 P2 3.96(9) . . . . ? C2 Fe1 C1 O1 -53.4(18) . . . . ? P1 Fe1 C1 O1 -155.3(18) . . . . ? S1 Fe1 C1 O1 107.3(18) . . . . ? S2 Fe1 C1 O1 55.2(18) . . . . ? Fe2 Fe1 C1 O1 108.0(18) . . . . ? C1 Fe1 C2 O2 93(9) . . . . ? P1 Fe1 C2 O2 -169(9) . . . . ? S1 Fe1 C2 O2 -83(9) . . . . ? S2 Fe1 C2 O2 5(9) . . . . ? Fe2 Fe1 C2 O2 -50(9) . . . . ? C4 Fe2 C3 O3 105(6) . . . . ? P2 Fe2 C3 O3 -156(6) . . . . ? S2 Fe2 C3 O3 -3(6) . . . . ? S1 Fe2 C3 O3 -71(6) . . . . ? Fe1 Fe2 C3 O3 -58(6) . . . . ? C3 Fe2 C4 O4 41(11) . . . . ? P2 Fe2 C4 O4 -51(11) . . . . ? S2 Fe2 C4 O4 129(11) . . . . ? S1 Fe2 C4 O4 -141(11) . . . . ? Fe1 Fe2 C4 O4 179(100) . . . . ? Fe1 S1 C5 C6 68.17(14) . . . . ? Fe2 S1 C5 C6 -4.73(15) . . . . ? S1 C5 C6 C7 -63.60(18) . . . . ? C5 C6 C7 S2 61.11(19) . . . . ? Fe1 S2 C7 C6 -64.24(14) . . . . ? Fe2 S2 C7 C6 9.38(16) . . . . ? P2 N1 C8 C9 84.48(15) . . . . ? P1 N1 C8 C9 -97.64(14) . . . . ? N1 C8 C9 C10 -136.17(17) . . . . ? N1 P1 C11 C12 -23.06(14) . . . . ? C17 P1 C11 C12 -128.24(13) . . . . ? Fe1 P1 C11 C12 102.49(13) . . . . ? N1 P1 C11 C16 160.93(13) . . . . ? C17 P1 C11 C16 55.76(14) . . . . ? Fe1 P1 C11 C16 -73.52(13) . . . . ? C16 C11 C12 C13 -2.6(2) . . . . ? P1 C11 C12 C13 -178.64(13) . . . . ? C11 C12 C13 C14 1.1(3) . . . . ? C12 C13 C14 C15 0.8(3) . . . . ? C13 C14 C15 C16 -1.1(3) . . . . ? C14 C15 C16 C11 -0.5(3) . . . . ? C12 C11 C16 C15 2.4(2) . . . . ? P1 C11 C16 C15 178.51(14) . . . . ? N1 P1 C17 C18 -97.11(14) . . . . ? C11 P1 C17 C18 10.40(15) . . . . ? Fe1 P1 C17 C18 135.22(12) . . . . ? N1 P1 C17 C22 77.36(13) . . . . ? C11 P1 C17 C22 -175.14(12) . . . . ? Fe1 P1 C17 C22 -50.32(13) . . . . ? C22 C17 C18 C19 1.3(2) . . . . ? P1 C17 C18 C19 175.72(14) . . . . ? C17 C18 C19 C20 -1.8(3) . . . . ? C18 C19 C20 C21 0.8(3) . . . . ? C19 C20 C21 C22 0.7(3) . . . . ? C20 C21 C22 C17 -1.2(3) . . . . ? C18 C17 C22 C21 0.1(2) . . . . ? P1 C17 C22 C21 -174.61(13) . . . . ? N1 P2 C23 C28 101.38(12) . . . . ? C29 P2 C23 C28 -147.15(12) . . . . ? Fe2 P2 C23 C28 -25.70(13) . . . . ? N1 P2 C23 C24 -80.37(13) . . . . ? C29 P2 C23 C24 31.10(14) . . . . ? Fe2 P2 C23 C24 152.55(11) . . . . ? C28 C23 C24 C25 0.2(2) . . . . ? P2 C23 C24 C25 -178.06(13) . . . . ? C23 C24 C25 C26 -0.8(3) . . . . ? C24 C25 C26 C27 0.5(3) . . . . ? C25 C26 C27 C28 0.2(3) . . . . ? C26 C27 C28 C23 -0.8(2) . . . . ? C24 C23 C28 C27 0.6(2) . . . . ? P2 C23 C28 C27 178.87(12) . . . . ? N1 P2 C29 C34 -30.11(15) . . . . ? C23 P2 C29 C34 -139.65(13) . . . . ? Fe2 P2 C29 C34 93.68(13) . . . . ? N1 P2 C29 C30 159.17(12) . . . . ? C23 P2 C29 C30 49.64(14) . . . . ? Fe2 P2 C29 C30 -77.03(13) . . . . ? C34 C29 C30 C31 1.8(3) . . . . ? P2 C29 C30 C31 172.87(14) . . . . ? C29 C30 C31 C32 -0.2(3) . . . . ? C30 C31 C32 C33 -1.5(3) . . . . ? C31 C32 C33 C34 1.5(3) . . . . ? C30 C29 C34 C33 -1.8(2) . . . . ? P2 C29 C34 C33 -172.51(13) . . . . ? C32 C33 C34 C29 0.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.539 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.058 data_str0541 _database_code_depnum_ccdc_archive 'CCDC 919235' #TrackingRef 'STR0541.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H33 Fe2 N O4 P2 S2' _chemical_formula_weight 757.37 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' Fe Fe 0.3463 0.8444 '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 10.4283(11) _cell_length_b 11.7343(13) _cell_length_c 14.6476(16) _cell_angle_alpha 84.906(2) _cell_angle_beta 73.720(2) _cell_angle_gamma 74.371(2) _cell_volume 1656.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 1.138 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8755 _exptl_absorpt_correction_T_max 0.9349 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14313 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 28.25 _reflns_number_total 7555 _reflns_number_gt 6538 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0610P)^2^+0.9132P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 7555 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.55757(3) 0.27560(3) 0.26357(2) 0.01304(9) Uani 1 1 d . . . Fe2 Fe 0.69934(3) 0.14796(3) 0.36097(2) 0.01195(9) Uani 1 1 d . . . P1 P 0.70498(6) 0.38115(5) 0.19101(4) 0.01314(12) Uani 1 1 d . . . P2 P 0.87564(6) 0.22797(5) 0.30454(4) 0.01147(12) Uani 1 1 d . . . S1 S 0.49780(6) 0.12122(5) 0.35217(4) 0.01621(13) Uani 1 1 d . . . S2 S 0.57836(6) 0.33599(5) 0.39975(4) 0.01320(12) Uani 1 1 d . . . N1 N 0.84207(19) 0.35785(16) 0.24007(13) 0.0130(4) Uani 1 1 d . . . O1 O 0.6461(2) 0.11117(18) 0.10654(13) 0.0298(4) Uani 1 1 d . . . O2 O 0.2996(2) 0.42513(19) 0.23278(16) 0.0363(5) Uani 1 1 d . . . O3 O 0.82935(19) -0.08447(15) 0.27402(13) 0.0245(4) Uani 1 1 d . . . O4 O 0.72433(19) 0.08203(16) 0.55371(12) 0.0228(4) Uani 1 1 d . . . C1 C 0.6118(3) 0.1783(2) 0.16648(17) 0.0191(5) Uani 1 1 d . . . C2 C 0.4018(3) 0.3686(2) 0.24438(18) 0.0211(5) Uani 1 1 d . . . C3 C 0.7808(2) 0.0083(2) 0.30603(17) 0.0165(5) Uani 1 1 d . . . C4 C 0.7167(2) 0.1051(2) 0.47730(16) 0.0154(4) Uani 1 1 d . . . C5 C 0.3588(3) 0.1658(2) 0.46008(19) 0.0246(5) Uani 1 1 d . . . H5A H 0.2764 0.1439 0.4538 0.030 Uiso 1 1 calc R . . H5B H 0.3870 0.1191 0.5141 0.030 Uiso 1 1 calc R . . C6 C 0.3172(3) 0.2936(3) 0.4847(2) 0.0345(7) Uani 1 1 d . . . H6A H 0.2391 0.3060 0.5429 0.041 Uiso 1 1 calc R . . H6B H 0.2830 0.3402 0.4327 0.041 Uiso 1 1 calc R . . C7 C 0.4276(2) 0.3420(2) 0.50109(17) 0.0199(5) Uani 1 1 d . . . H7A H 0.4592 0.2977 0.5549 0.024 Uiso 1 1 calc R . . H7B H 0.3865 0.4256 0.5204 0.024 Uiso 1 1 calc R . . C8 C 0.9444(3) 0.4324(2) 0.22623(17) 0.0182(5) Uani 1 1 d . . . H8A H 1.0068 0.3945 0.2674 0.022 Uiso 1 1 calc R . . C9 C 1.0386(3) 0.4319(2) 0.12585(18) 0.0239(5) Uani 1 1 d . . . H9A H 1.0799 0.3501 0.1044 0.036 Uiso 1 1 calc R . . H9B H 1.1119 0.4696 0.1255 0.036 Uiso 1 1 calc R . . H9C H 0.9846 0.4757 0.0830 0.036 Uiso 1 1 calc R . . C10 C 0.8792(3) 0.5594(2) 0.26174(19) 0.0230(5) Uani 1 1 d . . . H10A H 0.8193 0.5581 0.3265 0.034 Uiso 1 1 calc R . . H10B H 0.8243 0.6041 0.2197 0.034 Uiso 1 1 calc R . . H10C H 0.9522 0.5973 0.2617 0.034 Uiso 1 1 calc R . . C11 C 0.7676(3) 0.3485(2) 0.06383(16) 0.0167(5) Uani 1 1 d . . . C12 C 0.8992(3) 0.2821(2) 0.01919(17) 0.0191(5) Uani 1 1 d . . . H12A H 0.9679 0.2601 0.0530 0.023 Uiso 1 1 calc R . . C13 C 0.9313(3) 0.2472(2) -0.07494(18) 0.0261(6) Uani 1 1 d . . . H13A H 1.0217 0.2023 -0.1051 0.031 Uiso 1 1 calc R . . C14 C 0.8313(3) 0.2779(3) -0.12412(18) 0.0311(7) Uani 1 1 d . . . H14A H 0.8531 0.2539 -0.1881 0.037 Uiso 1 1 calc R . . C15 C 0.6993(3) 0.3439(3) -0.08048(19) 0.0288(6) Uani 1 1 d . . . H15A H 0.6307 0.3649 -0.1144 0.035 Uiso 1 1 calc R . . C16 C 0.6678(3) 0.3790(2) 0.01273(18) 0.0233(5) Uani 1 1 d . . . H16A H 0.5773 0.4243 0.0424 0.028 Uiso 1 1 calc R . . C17 C 0.6354(3) 0.5422(2) 0.18726(18) 0.0197(5) Uani 1 1 d . . . C18 C 0.5299(3) 0.5986(2) 0.26294(19) 0.0241(5) Uani 1 1 d . . . H18A H 0.4921 0.5531 0.3155 0.029 Uiso 1 1 calc R . . C19 C 0.4794(4) 0.7209(3) 0.2623(2) 0.0365(7) Uani 1 1 d . . . H19A H 0.4075 0.7590 0.3144 0.044 Uiso 1 1 calc R . . C20 C 0.5341(4) 0.7872(3) 0.1856(2) 0.0442(9) Uani 1 1 d . . . H20A H 0.5013 0.8710 0.1860 0.053 Uiso 1 1 calc R . . C21 C 0.6350(4) 0.7328(3) 0.1090(2) 0.0382(7) Uani 1 1 d . . . H21A H 0.6703 0.7789 0.0560 0.046 Uiso 1 1 calc R . . C22 C 0.6862(3) 0.6100(2) 0.1086(2) 0.0274(6) Uani 1 1 d . . . H22A H 0.7554 0.5724 0.0551 0.033 Uiso 1 1 calc R . . C23 C 0.9233(2) 0.2612(2) 0.40848(16) 0.0142(4) Uani 1 1 d . . . C24 C 0.9963(2) 0.1648(2) 0.45257(17) 0.0183(5) Uani 1 1 d . . . H24A H 1.0364 0.0914 0.4207 0.022 Uiso 1 1 calc R . . C25 C 1.0104(3) 0.1759(2) 0.54254(18) 0.0211(5) Uani 1 1 d . . . H25A H 1.0588 0.1097 0.5724 0.025 Uiso 1 1 calc R . . C26 C 0.9544(3) 0.2829(2) 0.58889(18) 0.0243(5) Uani 1 1 d . . . H26A H 0.9644 0.2902 0.6504 0.029 Uiso 1 1 calc R . . C27 C 0.8841(3) 0.3789(2) 0.54563(18) 0.0260(6) Uani 1 1 d . . . H27A H 0.8467 0.4526 0.5771 0.031 Uiso 1 1 calc R . . C28 C 0.8673(3) 0.3683(2) 0.45580(17) 0.0192(5) Uani 1 1 d . . . H28A H 0.8175 0.4346 0.4268 0.023 Uiso 1 1 calc R . . C29 C 1.0398(2) 0.1438(2) 0.22955(16) 0.0146(4) Uani 1 1 d . . . C30 C 1.0362(2) 0.0759(2) 0.15675(17) 0.0172(5) Uani 1 1 d . . . H30A H 0.9500 0.0675 0.1523 0.021 Uiso 1 1 calc R . . C31 C 1.1575(3) 0.0208(2) 0.09091(17) 0.0205(5) Uani 1 1 d . . . H31A H 1.1538 -0.0244 0.0414 0.025 Uiso 1 1 calc R . . C32 C 1.2833(3) 0.0316(2) 0.09737(18) 0.0230(5) Uani 1 1 d . . . H32A H 1.3661 -0.0059 0.0522 0.028 Uiso 1 1 calc R . . C33 C 1.2886(3) 0.0970(2) 0.16963(19) 0.0240(5) Uani 1 1 d . . . H33A H 1.3753 0.1033 0.1746 0.029 Uiso 1 1 calc R . . C34 C 1.1678(2) 0.1534(2) 0.23488(17) 0.0191(5) Uani 1 1 d . . . H34A H 1.1725 0.1990 0.2837 0.023 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 0.01164(16) 0.01492(17) 0.01291(17) -0.00198(12) -0.00401(12) -0.00265(12) Fe2 0.01119(16) 0.01154(16) 0.01301(16) -0.00027(12) -0.00307(12) -0.00290(12) P1 0.0149(3) 0.0125(3) 0.0117(3) -0.0002(2) -0.0048(2) -0.0018(2) P2 0.0108(3) 0.0123(3) 0.0117(3) -0.0011(2) -0.0040(2) -0.0024(2) S1 0.0135(3) 0.0171(3) 0.0189(3) -0.0027(2) -0.0027(2) -0.0062(2) S2 0.0123(3) 0.0138(3) 0.0128(3) -0.00203(19) -0.0025(2) -0.0025(2) N1 0.0139(9) 0.0133(9) 0.0136(9) 0.0014(7) -0.0055(7) -0.0054(7) O1 0.0340(11) 0.0324(11) 0.0239(10) -0.0123(8) 0.0013(8) -0.0157(9) O2 0.0240(10) 0.0387(12) 0.0461(13) 0.0061(10) -0.0181(10) -0.0007(9) O3 0.0286(10) 0.0157(9) 0.0268(10) -0.0048(7) -0.0046(8) -0.0033(7) O4 0.0276(10) 0.0234(9) 0.0172(9) 0.0014(7) -0.0058(7) -0.0070(8) C1 0.0172(11) 0.0233(12) 0.0176(11) -0.0017(9) -0.0011(9) -0.0099(10) C2 0.0210(12) 0.0222(12) 0.0205(12) -0.0001(9) -0.0069(10) -0.0047(10) C3 0.0144(11) 0.0188(12) 0.0174(11) 0.0023(9) -0.0039(9) -0.0071(9) C4 0.0138(10) 0.0132(11) 0.0185(12) -0.0019(8) -0.0037(9) -0.0022(8) C5 0.0163(12) 0.0294(14) 0.0248(13) -0.0038(10) 0.0039(10) -0.0090(10) C6 0.0291(15) 0.0363(17) 0.0340(16) -0.0041(13) -0.0005(13) -0.0090(13) C7 0.0155(11) 0.0247(13) 0.0159(11) -0.0061(9) 0.0023(9) -0.0042(10) C8 0.0193(11) 0.0201(12) 0.0187(11) 0.0002(9) -0.0053(9) -0.0105(9) C9 0.0224(13) 0.0273(14) 0.0248(13) 0.0039(10) -0.0049(11) -0.0138(11) C10 0.0311(14) 0.0180(12) 0.0248(13) -0.0014(10) -0.0093(11) -0.0121(10) C11 0.0250(12) 0.0151(11) 0.0118(10) 0.0011(8) -0.0052(9) -0.0082(9) C12 0.0233(12) 0.0170(12) 0.0167(11) -0.0001(9) -0.0021(10) -0.0081(10) C13 0.0352(15) 0.0216(13) 0.0191(12) -0.0037(10) 0.0029(11) -0.0129(11) C14 0.057(2) 0.0304(15) 0.0120(11) 0.0004(10) -0.0067(12) -0.0238(14) C15 0.0438(17) 0.0325(15) 0.0193(13) 0.0058(11) -0.0164(12) -0.0185(13) C16 0.0274(13) 0.0257(13) 0.0187(12) 0.0026(10) -0.0098(10) -0.0070(11) C17 0.0257(13) 0.0123(11) 0.0229(12) 0.0004(9) -0.0131(10) -0.0011(9) C18 0.0325(14) 0.0186(12) 0.0215(12) -0.0030(9) -0.0145(11) 0.0014(10) C19 0.0505(19) 0.0232(14) 0.0344(16) -0.0100(12) -0.0252(15) 0.0103(13) C20 0.072(2) 0.0141(13) 0.050(2) -0.0008(13) -0.0384(19) 0.0051(14) C21 0.057(2) 0.0181(14) 0.0429(18) 0.0113(12) -0.0232(16) -0.0088(14) C22 0.0358(15) 0.0198(13) 0.0273(14) 0.0046(10) -0.0128(12) -0.0055(11) C23 0.0120(10) 0.0194(11) 0.0122(10) -0.0019(8) -0.0032(8) -0.0053(9) C24 0.0156(11) 0.0206(12) 0.0202(12) 0.0003(9) -0.0066(9) -0.0054(9) C25 0.0184(12) 0.0286(14) 0.0197(12) 0.0058(10) -0.0101(10) -0.0084(10) C26 0.0253(13) 0.0362(15) 0.0159(12) -0.0012(10) -0.0068(10) -0.0139(11) C27 0.0336(15) 0.0254(14) 0.0202(13) -0.0083(10) -0.0063(11) -0.0079(11) C28 0.0219(12) 0.0182(12) 0.0174(11) -0.0023(9) -0.0052(10) -0.0045(10) C29 0.0123(10) 0.0134(11) 0.0155(11) -0.0002(8) -0.0017(9) -0.0011(8) C30 0.0168(11) 0.0171(11) 0.0170(11) -0.0024(9) -0.0023(9) -0.0046(9) C31 0.0240(13) 0.0175(12) 0.0181(12) -0.0033(9) -0.0020(10) -0.0049(10) C32 0.0174(12) 0.0230(13) 0.0220(13) -0.0026(10) 0.0007(10) 0.0005(10) C33 0.0122(11) 0.0288(14) 0.0286(14) -0.0030(11) -0.0024(10) -0.0034(10) C34 0.0162(11) 0.0212(12) 0.0195(12) -0.0024(9) -0.0037(9) -0.0042(9) _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 C1 1.770(2) . ? Fe1 C2 1.776(3) . ? Fe1 P1 2.2142(7) . ? Fe1 S1 2.2565(7) . ? Fe1 S2 2.2594(6) . ? Fe1 Fe2 2.4646(5) . ? Fe2 C3 1.776(2) . ? Fe2 C4 1.778(2) . ? Fe2 P2 2.2102(7) . ? Fe2 S1 2.2464(7) . ? Fe2 S2 2.2591(7) . ? P1 N1 1.722(2) . ? P1 C11 1.831(2) . ? P1 C17 1.835(2) . ? P2 N1 1.7261(19) . ? P2 C29 1.827(2) . ? P2 C23 1.831(2) . ? S1 C5 1.824(3) . ? S2 C7 1.825(2) . ? N1 C8 1.515(3) . ? O1 C1 1.147(3) . ? O2 C2 1.143(3) . ? O3 C3 1.150(3) . ? O4 C4 1.148(3) . ? C5 C6 1.492(4) . ? C6 C7 1.496(4) . ? C8 C9 1.522(3) . ? C8 C10 1.532(3) . ? C11 C12 1.389(3) . ? C11 C16 1.400(3) . ? C12 C13 1.396(3) . ? C13 C14 1.381(4) . ? C14 C15 1.387(4) . ? C15 C16 1.385(4) . ? C17 C18 1.390(4) . ? C17 C22 1.401(4) . ? C18 C19 1.390(4) . ? C19 C20 1.385(5) . ? C20 C21 1.370(5) . ? C21 C22 1.395(4) . ? C23 C28 1.391(3) . ? C23 C24 1.399(3) . ? C24 C25 1.388(3) . ? C25 C26 1.383(4) . ? C26 C27 1.377(4) . ? C27 C28 1.395(3) . ? C29 C34 1.394(3) . ? C29 C30 1.401(3) . ? C30 C31 1.391(3) . ? C31 C32 1.382(4) . ? C32 C33 1.383(4) . ? C33 C34 1.388(3) . ? 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 C1 Fe1 C2 101.08(12) . . ? C1 Fe1 P1 92.15(8) . . ? C2 Fe1 P1 100.36(8) . . ? C1 Fe1 S1 85.17(8) . . ? C2 Fe1 S1 105.80(8) . . ? P1 Fe1 S1 153.74(3) . . ? C1 Fe1 S2 152.37(9) . . ? C2 Fe1 S2 106.44(8) . . ? P1 Fe1 S2 85.36(2) . . ? S1 Fe1 S2 85.09(2) . . ? C1 Fe1 Fe2 96.39(8) . . ? C2 Fe1 Fe2 154.09(8) . . ? P1 Fe1 Fe2 97.93(2) . . ? S1 Fe1 Fe2 56.619(19) . . ? S2 Fe1 Fe2 56.939(18) . . ? C3 Fe2 C4 97.93(11) . . ? C3 Fe2 P2 96.82(8) . . ? C4 Fe2 P2 100.80(8) . . ? C3 Fe2 S1 87.52(8) . . ? C4 Fe2 S1 107.85(8) . . ? P2 Fe2 S1 150.15(3) . . ? C3 Fe2 S2 166.56(8) . . ? C4 Fe2 S2 95.09(7) . . ? P2 Fe2 S2 83.94(2) . . ? S1 Fe2 S2 85.33(2) . . ? C3 Fe2 Fe1 109.66(8) . . ? C4 Fe2 Fe1 146.79(7) . . ? P2 Fe2 Fe1 94.07(2) . . ? S1 Fe2 Fe1 57.012(19) . . ? S2 Fe2 Fe1 56.950(18) . . ? N1 P1 C11 110.22(10) . . ? N1 P1 C17 105.76(10) . . ? C11 P1 C17 100.80(11) . . ? N1 P1 Fe1 112.31(7) . . ? C11 P1 Fe1 110.25(8) . . ? C17 P1 Fe1 116.82(9) . . ? N1 P2 C29 102.49(10) . . ? N1 P2 C23 107.66(10) . . ? C29 P2 C23 103.01(11) . . ? N1 P2 Fe2 115.43(7) . . ? C29 P2 Fe2 121.15(8) . . ? C23 P2 Fe2 105.90(7) . . ? C5 S1 Fe2 112.64(9) . . ? C5 S1 Fe1 113.32(9) . . ? Fe2 S1 Fe1 66.369(19) . . ? C7 S2 Fe2 111.99(9) . . ? C7 S2 Fe1 114.23(8) . . ? Fe2 S2 Fe1 66.111(19) . . ? C8 N1 P1 127.65(15) . . ? C8 N1 P2 115.92(15) . . ? P1 N1 P2 116.19(11) . . ? O1 C1 Fe1 176.9(2) . . ? O2 C2 Fe1 177.6(2) . . ? O3 C3 Fe2 176.6(2) . . ? O4 C4 Fe2 177.1(2) . . ? C6 C5 S1 116.74(19) . . ? C5 C6 C7 115.9(3) . . ? C6 C7 S2 115.67(18) . . ? N1 C8 C9 114.63(19) . . ? N1 C8 C10 114.1(2) . . ? C9 C8 C10 110.5(2) . . ? C12 C11 C16 118.7(2) . . ? C12 C11 P1 124.73(19) . . ? C16 C11 P1 115.92(19) . . ? C11 C12 C13 120.6(2) . . ? C14 C13 C12 119.9(3) . . ? C13 C14 C15 120.3(2) . . ? C16 C15 C14 119.8(3) . . ? C15 C16 C11 120.8(3) . . ? C18 C17 C22 119.0(2) . . ? C18 C17 P1 119.93(19) . . ? C22 C17 P1 121.1(2) . . ? C17 C18 C19 120.5(3) . . ? C20 C19 C18 119.8(3) . . ? C21 C20 C19 120.5(3) . . ? C20 C21 C22 120.2(3) . . ? C21 C22 C17 119.9(3) . . ? C28 C23 C24 118.8(2) . . ? C28 C23 P2 123.45(18) . . ? C24 C23 P2 116.28(17) . . ? C25 C24 C23 120.3(2) . . ? C26 C25 C24 120.3(2) . . ? C27 C26 C25 119.9(2) . . ? C26 C27 C28 120.4(2) . . ? C23 C28 C27 120.3(2) . . ? C34 C29 C30 118.3(2) . . ? C34 C29 P2 123.19(18) . . ? C30 C29 P2 118.15(17) . . ? C31 C30 C29 120.6(2) . . ? C32 C31 C30 120.1(2) . . ? C31 C32 C33 119.9(2) . . ? C32 C33 C34 120.3(2) . . ? C33 C34 C29 120.7(2) . . ? 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 C1 Fe1 Fe2 C3 -6.56(11) . . . . ? C2 Fe1 Fe2 C3 125.7(2) . . . . ? P1 Fe1 Fe2 C3 -99.64(8) . . . . ? S1 Fe1 Fe2 C3 73.34(8) . . . . ? S2 Fe1 Fe2 C3 -178.80(8) . . . . ? C1 Fe1 Fe2 C4 -150.98(16) . . . . ? C2 Fe1 Fe2 C4 -18.7(2) . . . . ? P1 Fe1 Fe2 C4 115.94(14) . . . . ? S1 Fe1 Fe2 C4 -71.07(14) . . . . ? S2 Fe1 Fe2 C4 36.78(14) . . . . ? C1 Fe1 Fe2 P2 92.17(8) . . . . ? C2 Fe1 Fe2 P2 -135.52(19) . . . . ? P1 Fe1 Fe2 P2 -0.91(2) . . . . ? S1 Fe1 Fe2 P2 172.08(3) . . . . ? S2 Fe1 Fe2 P2 -80.07(2) . . . . ? C1 Fe1 Fe2 S1 -79.90(8) . . . . ? C2 Fe1 Fe2 S1 52.40(19) . . . . ? P1 Fe1 Fe2 S1 -172.98(3) . . . . ? S2 Fe1 Fe2 S1 107.85(3) . . . . ? C1 Fe1 Fe2 S2 172.24(8) . . . . ? C2 Fe1 Fe2 S2 -55.45(19) . . . . ? P1 Fe1 Fe2 S2 79.16(3) . . . . ? S1 Fe1 Fe2 S2 -107.85(3) . . . . ? C1 Fe1 P1 N1 -107.22(11) . . . . ? C2 Fe1 P1 N1 151.11(11) . . . . ? S1 Fe1 P1 N1 -23.78(10) . . . . ? S2 Fe1 P1 N1 45.22(7) . . . . ? Fe2 Fe1 P1 N1 -10.46(7) . . . . ? C1 Fe1 P1 C11 16.13(12) . . . . ? C2 Fe1 P1 C11 -85.55(12) . . . . ? S1 Fe1 P1 C11 99.56(10) . . . . ? S2 Fe1 P1 C11 168.56(9) . . . . ? Fe2 Fe1 P1 C11 112.89(9) . . . . ? C1 Fe1 P1 C17 130.35(12) . . . . ? C2 Fe1 P1 C17 28.67(12) . . . . ? S1 Fe1 P1 C17 -146.22(10) . . . . ? S2 Fe1 P1 C17 -77.22(9) . . . . ? Fe2 Fe1 P1 C17 -132.89(9) . . . . ? C3 Fe2 P2 N1 122.88(11) . . . . ? C4 Fe2 P2 N1 -137.67(10) . . . . ? S1 Fe2 P2 N1 25.93(10) . . . . ? S2 Fe2 P2 N1 -43.62(8) . . . . ? Fe1 Fe2 P2 N1 12.50(8) . . . . ? C3 Fe2 P2 C29 -1.68(12) . . . . ? C4 Fe2 P2 C29 97.78(12) . . . . ? S1 Fe2 P2 C29 -98.62(10) . . . . ? S2 Fe2 P2 C29 -168.17(9) . . . . ? Fe1 Fe2 P2 C29 -112.05(9) . . . . ? C3 Fe2 P2 C23 -118.14(11) . . . . ? C4 Fe2 P2 C23 -18.68(11) . . . . ? S1 Fe2 P2 C23 144.92(9) . . . . ? S2 Fe2 P2 C23 75.36(8) . . . . ? Fe1 Fe2 P2 C23 131.49(8) . . . . ? C3 Fe2 S1 C5 137.96(12) . . . . ? C4 Fe2 S1 C5 40.42(13) . . . . ? P2 Fe2 S1 C5 -122.64(11) . . . . ? S2 Fe2 S1 C5 -53.43(10) . . . . ? Fe1 Fe2 S1 C5 -106.60(10) . . . . ? C3 Fe2 S1 Fe1 -115.44(8) . . . . ? C4 Fe2 S1 Fe1 147.03(8) . . . . ? P2 Fe2 S1 Fe1 -16.03(5) . . . . ? S2 Fe2 S1 Fe1 53.18(2) . . . . ? C1 Fe1 S1 C5 -153.48(13) . . . . ? C2 Fe1 S1 C5 -53.31(13) . . . . ? P1 Fe1 S1 C5 121.47(11) . . . . ? S2 Fe1 S1 C5 52.41(10) . . . . ? Fe2 Fe1 S1 C5 105.60(10) . . . . ? C1 Fe1 S1 Fe2 100.92(8) . . . . ? C2 Fe1 S1 Fe2 -158.91(9) . . . . ? P1 Fe1 S1 Fe2 15.87(6) . . . . ? S2 Fe1 S1 Fe2 -53.194(19) . . . . ? C3 Fe2 S2 C7 112.6(3) . . . . ? C4 Fe2 S2 C7 -53.01(12) . . . . ? P2 Fe2 S2 C7 -153.36(9) . . . . ? S1 Fe2 S2 C7 54.54(9) . . . . ? Fe1 Fe2 S2 C7 107.77(9) . . . . ? C3 Fe2 S2 Fe1 4.9(3) . . . . ? C4 Fe2 S2 Fe1 -160.78(8) . . . . ? P2 Fe2 S2 Fe1 98.87(2) . . . . ? S1 Fe2 S2 Fe1 -53.23(2) . . . . ? C1 Fe1 S2 C7 -121.27(19) . . . . ? C2 Fe1 S2 C7 53.50(13) . . . . ? P1 Fe1 S2 C7 152.95(10) . . . . ? S1 Fe1 S2 C7 -51.54(10) . . . . ? Fe2 Fe1 S2 C7 -104.46(10) . . . . ? C1 Fe1 S2 Fe2 -16.82(17) . . . . ? C2 Fe1 S2 Fe2 157.96(9) . . . . ? P1 Fe1 S2 Fe2 -102.59(2) . . . . ? S1 Fe1 S2 Fe2 52.91(2) . . . . ? C11 P1 N1 C8 72.0(2) . . . . ? C17 P1 N1 C8 -36.2(2) . . . . ? Fe1 P1 N1 C8 -164.65(17) . . . . ? C11 P1 N1 P2 -102.13(13) . . . . ? C17 P1 N1 P2 149.72(12) . . . . ? Fe1 P1 N1 P2 21.23(13) . . . . ? C29 P2 N1 C8 -63.81(18) . . . . ? C23 P2 N1 C8 44.40(18) . . . . ? Fe2 P2 N1 C8 162.40(13) . . . . ? C29 P2 N1 P1 111.02(13) . . . . ? C23 P2 N1 P1 -140.77(12) . . . . ? Fe2 P2 N1 P1 -22.77(13) . . . . ? C2 Fe1 C1 O1 -116(4) . . . . ? P1 Fe1 C1 O1 143(4) . . . . ? S1 Fe1 C1 O1 -11(4) . . . . ? S2 Fe1 C1 O1 59(4) . . . . ? Fe2 Fe1 C1 O1 45(4) . . . . ? C1 Fe1 C2 O2 68(6) . . . . ? P1 Fe1 C2 O2 162(6) . . . . ? S1 Fe1 C2 O2 -20(6) . . . . ? S2 Fe1 C2 O2 -109(6) . . . . ? Fe2 Fe1 C2 O2 -63(6) . . . . ? C4 Fe2 C3 O3 51(4) . . . . ? P2 Fe2 C3 O3 153(4) . . . . ? S1 Fe2 C3 O3 -56(4) . . . . ? S2 Fe2 C3 O3 -114(4) . . . . ? Fe1 Fe2 C3 O3 -110(4) . . . . ? C3 Fe2 C4 O4 -171(4) . . . . ? P2 Fe2 C4 O4 90(4) . . . . ? S1 Fe2 C4 O4 -81(4) . . . . ? S2 Fe2 C4 O4 5(4) . . . . ? Fe1 Fe2 C4 O4 -25(4) . . . . ? Fe2 S1 C5 C6 63.7(2) . . . . ? Fe1 S1 C5 C6 -9.2(3) . . . . ? S1 C5 C6 C7 -60.3(3) . . . . ? C5 C6 C7 S2 61.4(3) . . . . ? Fe2 S2 C7 C6 -66.0(2) . . . . ? Fe1 S2 C7 C6 6.7(2) . . . . ? P1 N1 C8 C9 -66.6(3) . . . . ? P2 N1 C8 C9 107.5(2) . . . . ? P1 N1 C8 C10 62.3(3) . . . . ? P2 N1 C8 C10 -123.58(19) . . . . ? N1 P1 C11 C12 18.0(2) . . . . ? C17 P1 C11 C12 129.4(2) . . . . ? Fe1 P1 C11 C12 -106.6(2) . . . . ? N1 P1 C11 C16 -171.76(18) . . . . ? C17 P1 C11 C16 -60.4(2) . . . . ? Fe1 P1 C11 C16 63.7(2) . . . . ? C16 C11 C12 C13 0.5(4) . . . . ? P1 C11 C12 C13 170.52(19) . . . . ? C11 C12 C13 C14 -0.6(4) . . . . ? C12 C13 C14 C15 0.3(4) . . . . ? C13 C14 C15 C16 0.0(4) . . . . ? C14 C15 C16 C11 -0.1(4) . . . . ? C12 C11 C16 C15 -0.1(4) . . . . ? P1 C11 C16 C15 -171.1(2) . . . . ? N1 P1 C17 C18 -91.7(2) . . . . ? C11 P1 C17 C18 153.5(2) . . . . ? Fe1 P1 C17 C18 34.1(2) . . . . ? N1 P1 C17 C22 88.8(2) . . . . ? C11 P1 C17 C22 -26.0(2) . . . . ? Fe1 P1 C17 C22 -145.40(19) . . . . ? C22 C17 C18 C19 -2.6(4) . . . . ? P1 C17 C18 C19 177.9(2) . . . . ? C17 C18 C19 C20 0.3(4) . . . . ? C18 C19 C20 C21 1.8(5) . . . . ? C19 C20 C21 C22 -1.5(5) . . . . ? C20 C21 C22 C17 -0.8(5) . . . . ? C18 C17 C22 C21 2.8(4) . . . . ? P1 C17 C22 C21 -177.7(2) . . . . ? N1 P2 C23 C28 33.9(2) . . . . ? C29 P2 C23 C28 141.8(2) . . . . ? Fe2 P2 C23 C28 -90.1(2) . . . . ? N1 P2 C23 C24 -160.01(17) . . . . ? C29 P2 C23 C24 -52.2(2) . . . . ? Fe2 P2 C23 C24 76.00(18) . . . . ? C28 C23 C24 C25 1.0(4) . . . . ? P2 C23 C24 C25 -165.76(19) . . . . ? C23 C24 C25 C26 -1.0(4) . . . . ? C24 C25 C26 C27 0.1(4) . . . . ? C25 C26 C27 C28 0.9(4) . . . . ? C24 C23 C28 C27 0.0(4) . . . . ? P2 C23 C28 C27 165.7(2) . . . . ? C26 C27 C28 C23 -0.9(4) . . . . ? N1 P2 C29 C34 87.3(2) . . . . ? C23 P2 C29 C34 -24.4(2) . . . . ? Fe2 P2 C29 C34 -142.32(18) . . . . ? N1 P2 C29 C30 -85.88(19) . . . . ? C23 P2 C29 C30 162.41(18) . . . . ? Fe2 P2 C29 C30 44.5(2) . . . . ? C34 C29 C30 C31 -0.8(3) . . . . ? P2 C29 C30 C31 172.77(19) . . . . ? C29 C30 C31 C32 0.6(4) . . . . ? C30 C31 C32 C33 0.2(4) . . . . ? C31 C32 C33 C34 -1.0(4) . . . . ? C32 C33 C34 C29 0.9(4) . . . . ? C30 C29 C34 C33 0.0(4) . . . . ? P2 C29 C34 C33 -173.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.825 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.094 data_str0954 _database_code_depnum_ccdc_archive 'CCDC 919236' #TrackingRef 'STR0954.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 B Cl4 F4 Fe2 N O4 P2 S2' _chemical_formula_weight 1013.03 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/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 9.321(3) _cell_length_b 31.564(9) _cell_length_c 13.987(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.751(5) _cell_angle_gamma 90.00 _cell_volume 4042.9(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 1.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6402 _exptl_absorpt_correction_T_max 0.7918 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34315 _diffrn_reflns_av_R_equivalents 0.1001 _diffrn_reflns_av_sigmaI/netI 0.1699 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 28.45 _reflns_number_total 9563 _reflns_number_gt 4650 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0418P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9563 _refine_ls_number_parameters 509 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1164 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1019 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 0.795 _refine_ls_restrained_S_all 0.795 _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 0.57945(6) 0.129788(17) 0.77916(4) 0.02380(15) Uani 1 1 d . . . Fe2 Fe 0.50937(6) 0.052246(17) 0.79004(4) 0.02559(15) Uani 1 1 d . . . H1 H 0.566(4) 0.0835(12) 0.717(3) 0.051(12) Uiso 1 1 d . . . N1 N 0.6885(3) 0.16166(9) 0.6162(2) 0.0224(7) Uani 1 1 d . . . P1 P 0.77700(11) 0.13938(3) 0.71907(7) 0.0234(2) Uani 1 1 d . . . P2 P 0.51685(11) 0.15999(3) 0.63756(7) 0.0238(2) Uani 1 1 d . . . S1 S 0.67680(11) 0.08699(3) 0.89985(7) 0.0257(2) Uani 1 1 d . . . S2 S 0.36377(11) 0.10786(3) 0.80363(7) 0.0262(2) Uani 1 1 d . . . C1 C 0.5747(4) 0.17628(13) 0.8426(3) 0.0262(9) Uani 1 1 d . . . C2 C 0.4330(4) 0.01678(13) 0.8656(3) 0.0284(10) Uani 1 1 d . . . C3 C 0.6481(5) 0.01557(13) 0.7692(3) 0.0295(10) Uani 1 1 d . . . C4 C 0.3939(5) 0.03458(12) 0.6791(3) 0.0305(10) Uani 1 1 d . . . O1 O 0.5607(3) 0.20614(9) 0.8882(2) 0.0390(8) Uani 1 1 d . . . O2 O 0.3812(3) -0.00506(9) 0.9129(2) 0.0348(7) Uani 1 1 d . . . O3 O 0.7291(3) -0.00877(9) 0.7550(2) 0.0384(8) Uani 1 1 d . . . O4 O 0.3276(3) 0.02319(9) 0.6086(2) 0.0434(8) Uani 1 1 d . . . C5 C 0.6110(4) 0.10306(12) 1.0095(3) 0.0290(10) Uani 1 1 d . . . H5A H 0.6673 0.0874 1.0655 0.035 Uiso 1 1 calc R . . H5B H 0.6324 0.1336 1.0208 0.035 Uiso 1 1 calc R . . C6 C 0.4521(4) 0.09612(12) 1.0082(3) 0.0310(10) Uani 1 1 d . . . H6A H 0.4328 0.0653 1.0030 0.037 Uiso 1 1 calc R . . H6B H 0.4305 0.1056 1.0715 0.037 Uiso 1 1 calc R . . C7 C 0.3480(4) 0.11776(12) 0.9293(3) 0.0325(10) Uani 1 1 d . . . H7A H 0.3578 0.1487 0.9407 0.039 Uiso 1 1 calc R . . H7B H 0.2478 0.1098 0.9365 0.039 Uiso 1 1 calc R . . C8 C 0.7352(4) 0.19054(12) 0.5446(3) 0.0269(10) Uani 1 1 d . . . H8A H 0.7878 0.2147 0.5804 0.032 Uiso 1 1 calc R . . H8B H 0.6466 0.2021 0.5024 0.032 Uiso 1 1 calc R . . C9 C 0.8297(5) 0.17199(13) 0.4814(3) 0.0328(10) Uani 1 1 d . . . H9A H 0.8072 0.1444 0.4555 0.039 Uiso 1 1 calc R . . C10 C 0.9409(5) 0.19144(14) 0.4599(3) 0.0403(12) Uani 1 1 d . . . H10A H 0.9654 0.2190 0.4850 0.048 Uiso 1 1 calc R . . H10B H 0.9983 0.1782 0.4191 0.048 Uiso 1 1 calc R . . C11 C 0.9233(4) 0.17267(11) 0.7795(3) 0.0233(9) Uani 1 1 d . . . C12 C 0.9335(4) 0.18084(12) 0.8772(3) 0.0283(10) Uani 1 1 d . . . H12A H 0.8589 0.1711 0.9098 0.034 Uiso 1 1 calc R . . C13 C 1.0500(5) 0.20290(13) 0.9283(3) 0.0334(11) Uani 1 1 d . . . H13A H 1.0565 0.2081 0.9958 0.040 Uiso 1 1 calc R . . C14 C 1.1557(4) 0.21718(12) 0.8817(3) 0.0291(10) Uani 1 1 d . . . H14A H 1.2364 0.2325 0.9168 0.035 Uiso 1 1 calc R . . C15 C 1.1469(4) 0.20965(12) 0.7845(3) 0.0315(10) Uani 1 1 d . . . H15A H 1.2201 0.2203 0.7520 0.038 Uiso 1 1 calc R . . C16 C 1.0318(4) 0.18665(12) 0.7337(3) 0.0286(10) Uani 1 1 d . . . H16A H 1.0279 0.1805 0.6668 0.034 Uiso 1 1 calc R . . C17 C 0.8710(4) 0.09343(11) 0.6884(3) 0.0239(9) Uani 1 1 d . . . C18 C 0.9801(4) 0.07583(12) 0.7577(3) 0.0283(10) Uani 1 1 d . . . H18A H 1.0125 0.0902 0.8175 0.034 Uiso 1 1 calc R . . C19 C 1.0419(4) 0.03771(13) 0.7407(3) 0.0323(10) Uani 1 1 d . . . H19A H 1.1143 0.0253 0.7896 0.039 Uiso 1 1 calc R . . C20 C 0.9990(4) 0.01761(12) 0.6532(3) 0.0317(10) Uani 1 1 d . . . H20A H 1.0449 -0.0081 0.6408 0.038 Uiso 1 1 calc R . . C21 C 0.8916(4) 0.03401(13) 0.5840(3) 0.0323(10) Uani 1 1 d . . . H21A H 0.8610 0.0195 0.5242 0.039 Uiso 1 1 calc R . . C22 C 0.8270(4) 0.07223(12) 0.6015(3) 0.0298(10) Uani 1 1 d . . . H22A H 0.7520 0.0838 0.5533 0.036 Uiso 1 1 calc R . . C23 C 0.4536(4) 0.21421(12) 0.6294(3) 0.0232(9) Uani 1 1 d . . . C24 C 0.3185(4) 0.22672(12) 0.5793(3) 0.0286(10) Uani 1 1 d . . . H24A H 0.2584 0.2070 0.5388 0.034 Uiso 1 1 calc R . . C25 C 0.2701(5) 0.26741(13) 0.5874(3) 0.0340(11) Uani 1 1 d . . . H25A H 0.1762 0.2755 0.5534 0.041 Uiso 1 1 calc R . . C26 C 0.3559(5) 0.29617(13) 0.6441(3) 0.0354(11) Uani 1 1 d . . . H26A H 0.3205 0.3240 0.6512 0.042 Uiso 1 1 calc R . . C27 C 0.4928(5) 0.28510(12) 0.6908(3) 0.0331(11) Uani 1 1 d . . . H27A H 0.5544 0.3055 0.7279 0.040 Uiso 1 1 calc R . . C28 C 0.5410(4) 0.24429(12) 0.6838(3) 0.0278(10) Uani 1 1 d . . . H28A H 0.6358 0.2366 0.7169 0.033 Uiso 1 1 calc R . . C29 C 0.4010(4) 0.13146(12) 0.5412(3) 0.0241(9) Uani 1 1 d . . . C30 C 0.2588(4) 0.12399(12) 0.5496(3) 0.0294(10) Uani 1 1 d . . . H30A H 0.2235 0.1345 0.6045 0.035 Uiso 1 1 calc R . . C31 C 0.1681(5) 0.10177(12) 0.4800(3) 0.0335(11) Uani 1 1 d . . . H31A H 0.0691 0.0975 0.4855 0.040 Uiso 1 1 calc R . . C32 C 0.2192(5) 0.08557(13) 0.4018(3) 0.0385(11) Uani 1 1 d . . . H32A H 0.1564 0.0700 0.3530 0.046 Uiso 1 1 calc R . . C33 C 0.3616(5) 0.09219(13) 0.3950(3) 0.0363(11) Uani 1 1 d . . . H33A H 0.3982 0.0806 0.3416 0.044 Uiso 1 1 calc R . . C34 C 0.4520(4) 0.11505(11) 0.4636(3) 0.0281(10) Uani 1 1 d . . . H34A H 0.5507 0.1196 0.4576 0.034 Uiso 1 1 calc R . . C40 C 0.0247(5) 0.05934(13) 0.0826(3) 0.0438(12) Uani 1 1 d . . . H40A H -0.0757 0.0573 0.0443 0.053 Uiso 1 1 calc R . . H40B H 0.0264 0.0449 0.1456 0.053 Uiso 1 1 calc R . . C50 C 0.9431(8) 0.3204(2) 0.7432(4) 0.093(2) Uani 1 1 d . . . H50A H 1.0508 0.3188 0.7615 0.111 Uiso 1 1 calc R . . H50B H 0.9151 0.3506 0.7453 0.111 Uiso 1 1 calc R . . Cl1 Cl 0.14573(13) 0.03381(4) 0.01966(9) 0.0478(3) Uani 1 1 d . . . Cl2 Cl 0.0698(2) 0.11161(4) 0.10335(12) 0.0898(6) Uani 1 1 d . . . Cl3 Cl 0.89189(15) 0.30245(4) 0.62597(9) 0.0560(4) Uani 1 1 d . . . Cl4 Cl 0.86910(14) 0.29339(4) 0.82755(9) 0.0536(3) Uani 1 1 d . . . B1 B 0.7189(6) 0.08011(17) 0.2750(4) 0.0377(13) Uani 1 1 d . . . F1 F 0.5840(3) 0.06170(9) 0.2494(2) 0.0668(9) Uani 1 1 d . . . F2 F 0.7669(3) 0.07629(8) 0.37246(18) 0.0650(8) Uani 1 1 d . . . F3 F 0.8136(3) 0.05972(8) 0.22627(17) 0.0512(7) Uani 1 1 d . . . F4 F 0.7078(3) 0.12173(8) 0.24931(19) 0.0652(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0280(3) 0.0170(3) 0.0259(3) -0.0005(3) 0.0039(3) -0.0001(3) Fe2 0.0298(3) 0.0171(3) 0.0293(3) -0.0007(3) 0.0039(3) -0.0002(3) N1 0.0261(19) 0.0158(17) 0.0251(19) 0.0003(14) 0.0042(15) -0.0005(14) P1 0.0270(6) 0.0178(6) 0.0244(6) -0.0008(4) 0.0022(5) 0.0007(4) P2 0.0277(6) 0.0179(6) 0.0251(6) 0.0000(4) 0.0033(5) 0.0012(5) S1 0.0302(6) 0.0191(5) 0.0267(6) 0.0002(4) 0.0025(5) 0.0003(4) S2 0.0286(6) 0.0201(5) 0.0302(6) 0.0005(5) 0.0059(5) 0.0006(5) C1 0.027(2) 0.025(2) 0.025(2) 0.0105(19) 0.0021(19) 0.0001(19) C2 0.029(3) 0.023(2) 0.030(2) -0.0027(19) -0.004(2) 0.0036(19) C3 0.032(3) 0.026(3) 0.027(2) -0.002(2) -0.003(2) -0.007(2) C4 0.038(3) 0.016(2) 0.040(3) 0.004(2) 0.014(2) 0.0024(19) O1 0.054(2) 0.0244(17) 0.0376(18) -0.0076(14) 0.0067(15) 0.0047(14) O2 0.047(2) 0.0204(17) 0.0381(18) 0.0022(13) 0.0111(15) -0.0075(14) O3 0.0403(19) 0.0266(18) 0.050(2) -0.0055(14) 0.0127(16) 0.0046(15) O4 0.050(2) 0.039(2) 0.037(2) -0.0056(15) -0.0028(16) -0.0053(16) C5 0.039(3) 0.022(2) 0.025(2) -0.0032(18) 0.004(2) -0.0035(19) C6 0.040(3) 0.025(2) 0.029(2) 0.0004(18) 0.009(2) 0.0011(19) C7 0.037(3) 0.024(2) 0.038(3) 0.0009(19) 0.013(2) 0.0012(19) C8 0.026(2) 0.022(2) 0.030(2) 0.0021(18) 0.0014(19) -0.0026(18) C9 0.043(3) 0.026(2) 0.030(3) 0.0048(19) 0.011(2) 0.007(2) C10 0.040(3) 0.037(3) 0.047(3) 0.008(2) 0.014(2) 0.006(2) C11 0.026(2) 0.016(2) 0.028(2) -0.0013(17) 0.0045(19) 0.0043(17) C12 0.030(3) 0.024(2) 0.030(3) -0.0008(19) 0.002(2) -0.0054(19) C13 0.042(3) 0.033(3) 0.026(2) -0.0068(19) 0.005(2) -0.007(2) C14 0.027(3) 0.023(2) 0.034(3) -0.0029(19) -0.003(2) -0.0059(19) C15 0.029(3) 0.033(3) 0.032(3) 0.003(2) 0.006(2) -0.007(2) C16 0.033(3) 0.027(2) 0.027(2) -0.0030(19) 0.008(2) -0.0013(19) C17 0.023(2) 0.020(2) 0.028(2) 0.0003(18) 0.0037(19) -0.0045(17) C18 0.033(3) 0.019(2) 0.031(2) -0.0033(18) 0.000(2) -0.0030(19) C19 0.027(2) 0.027(2) 0.040(3) 0.003(2) 0.000(2) 0.0042(19) C20 0.030(3) 0.019(2) 0.048(3) 0.001(2) 0.013(2) 0.0032(19) C21 0.040(3) 0.026(2) 0.031(3) -0.0070(19) 0.008(2) 0.002(2) C22 0.031(3) 0.027(2) 0.030(2) 0.0005(19) 0.003(2) -0.0016(19) C23 0.027(2) 0.025(2) 0.019(2) 0.0006(17) 0.0068(18) 0.0008(18) C24 0.037(3) 0.026(2) 0.022(2) 0.0024(18) 0.006(2) -0.001(2) C25 0.037(3) 0.032(3) 0.034(3) 0.012(2) 0.009(2) 0.009(2) C26 0.048(3) 0.027(3) 0.033(3) 0.007(2) 0.012(2) 0.012(2) C27 0.048(3) 0.020(2) 0.035(3) 0.0006(19) 0.016(2) -0.006(2) C28 0.037(3) 0.025(2) 0.021(2) 0.0045(18) 0.0048(19) 0.000(2) C29 0.028(2) 0.018(2) 0.025(2) 0.0017(17) 0.0008(18) 0.0020(18) C30 0.031(3) 0.029(2) 0.029(2) -0.0004(19) 0.006(2) 0.003(2) C31 0.029(3) 0.026(2) 0.044(3) 0.003(2) 0.004(2) -0.001(2) C32 0.042(3) 0.032(3) 0.037(3) -0.006(2) -0.004(2) -0.007(2) C33 0.042(3) 0.034(3) 0.032(3) -0.007(2) 0.008(2) 0.000(2) C34 0.030(2) 0.018(2) 0.037(3) 0.0001(19) 0.008(2) -0.0005(18) C40 0.039(3) 0.037(3) 0.057(3) 0.002(2) 0.015(2) 0.007(2) C50 0.138(6) 0.091(5) 0.048(4) -0.018(3) 0.017(4) -0.067(4) Cl1 0.0480(8) 0.0434(7) 0.0552(8) -0.0063(6) 0.0180(6) -0.0056(6) Cl2 0.1294(14) 0.0358(8) 0.1222(14) -0.0125(8) 0.0701(12) -0.0068(8) Cl3 0.0784(10) 0.0400(8) 0.0489(8) -0.0013(6) 0.0101(7) -0.0066(7) Cl4 0.0690(9) 0.0417(8) 0.0466(8) 0.0009(6) 0.0017(7) -0.0064(6) B1 0.049(4) 0.034(3) 0.031(3) -0.003(2) 0.011(3) 0.002(3) F1 0.061(2) 0.074(2) 0.072(2) -0.0267(16) 0.0299(17) -0.0171(16) F2 0.113(2) 0.0512(18) 0.0276(15) -0.0005(13) 0.0038(15) 0.0042(17) F3 0.0495(17) 0.0540(18) 0.0498(17) -0.0068(13) 0.0088(14) 0.0183(13) F4 0.100(2) 0.0273(16) 0.069(2) 0.0110(13) 0.0168(17) 0.0104(15) _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 C1 1.720(4) . ? Fe1 P2 2.1773(12) . ? Fe1 P1 2.1831(13) . ? Fe1 S2 2.2124(13) . ? Fe1 S1 2.2195(12) . ? Fe1 Fe2 2.5451(10) . ? Fe2 C2 1.777(5) . ? Fe2 C3 1.799(5) . ? Fe2 C4 1.805(5) . ? Fe2 S2 2.2485(12) . ? Fe2 S1 2.2590(12) . ? N1 C8 1.479(4) . ? N1 P1 1.674(3) . ? N1 P2 1.683(3) . ? P1 C17 1.788(4) . ? P1 C11 1.802(4) . ? P1 P2 2.5635(15) . ? P2 C29 1.803(4) . ? P2 C23 1.807(4) . ? S1 C5 1.827(4) . ? S2 C7 1.818(4) . ? C1 O1 1.159(4) . ? C2 O2 1.125(4) . ? C3 O3 1.121(4) . ? C4 O4 1.120(4) . ? C5 C6 1.494(5) . ? C6 C7 1.492(5) . ? C8 C9 1.479(5) . ? C9 C10 1.288(5) . ? C11 C16 1.367(5) . ? C11 C12 1.377(5) . ? C12 C13 1.373(5) . ? C13 C14 1.356(5) . ? C14 C15 1.366(5) . ? C15 C16 1.378(5) . ? C17 C22 1.381(5) . ? C17 C18 1.384(5) . ? C18 C19 1.374(5) . ? C19 C20 1.370(5) . ? C20 C21 1.358(5) . ? C21 C22 1.390(5) . ? C23 C24 1.380(5) . ? C23 C28 1.383(5) . ? C24 C25 1.373(5) . ? C25 C26 1.362(6) . ? C26 C27 1.366(6) . ? C27 C28 1.374(5) . ? C29 C34 1.365(5) . ? C29 C30 1.372(5) . ? C30 C31 1.359(5) . ? C31 C32 1.371(5) . ? C32 C33 1.365(6) . ? C33 C34 1.360(5) . ? C40 Cl2 1.714(4) . ? C40 Cl1 1.751(4) . ? C50 Cl4 1.702(5) . ? C50 Cl3 1.716(5) . ? B1 F2 1.358(5) . ? B1 F4 1.361(6) . ? B1 F1 1.371(6) . ? B1 F3 1.372(5) . ? 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 C1 Fe1 P2 93.88(13) . . ? C1 Fe1 P1 100.68(13) . . ? P2 Fe1 P1 72.02(4) . . ? C1 Fe1 S2 94.32(13) . . ? P2 Fe1 S2 100.40(4) . . ? P1 Fe1 S2 163.53(5) . . ? C1 Fe1 S1 99.96(13) . . ? P2 Fe1 S1 163.83(5) . . ? P1 Fe1 S1 97.05(4) . . ? S2 Fe1 S1 86.92(4) . . ? C1 Fe1 Fe2 139.28(13) . . ? P2 Fe1 Fe2 116.56(4) . . ? P1 Fe1 Fe2 113.62(4) . . ? S2 Fe1 Fe2 55.88(3) . . ? S1 Fe1 Fe2 56.10(3) . . ? C2 Fe2 C3 94.06(18) . . ? C2 Fe2 C4 94.37(18) . . ? C3 Fe2 C4 89.61(17) . . ? C2 Fe2 S2 97.26(13) . . ? C3 Fe2 S2 168.32(13) . . ? C4 Fe2 S2 92.37(13) . . ? C2 Fe2 S1 101.77(13) . . ? C3 Fe2 S1 89.79(12) . . ? C4 Fe2 S1 163.85(13) . . ? S2 Fe2 S1 85.12(4) . . ? C2 Fe2 Fe1 141.00(13) . . ? C3 Fe2 Fe1 114.13(13) . . ? C4 Fe2 Fe1 111.37(12) . . ? S2 Fe2 Fe1 54.55(3) . . ? S1 Fe2 Fe1 54.64(3) . . ? C8 N1 P1 133.0(2) . . ? C8 N1 P2 123.3(2) . . ? P1 N1 P2 99.60(16) . . ? N1 P1 C17 108.63(16) . . ? N1 P1 C11 111.48(17) . . ? C17 P1 C11 102.92(17) . . ? N1 P1 Fe1 94.21(11) . . ? C17 P1 Fe1 117.80(13) . . ? C11 P1 Fe1 121.28(13) . . ? N1 P1 P2 40.33(11) . . ? C17 P1 P2 124.37(13) . . ? C11 P1 P2 129.11(13) . . ? Fe1 P1 P2 53.89(4) . . ? N1 P2 C29 109.87(17) . . ? N1 P2 C23 105.61(16) . . ? C29 P2 C23 106.45(17) . . ? N1 P2 Fe1 94.17(11) . . ? C29 P2 Fe1 118.87(13) . . ? C23 P2 Fe1 120.07(12) . . ? N1 P2 P1 40.07(10) . . ? C29 P2 P1 126.20(13) . . ? C23 P2 P1 122.61(13) . . ? Fe1 P2 P1 54.10(4) . . ? C5 S1 Fe1 108.42(13) . . ? C5 S1 Fe2 114.09(13) . . ? Fe1 S1 Fe2 69.25(4) . . ? C7 S2 Fe1 109.61(14) . . ? C7 S2 Fe2 112.03(13) . . ? Fe1 S2 Fe2 69.57(4) . . ? O1 C1 Fe1 173.9(4) . . ? O2 C2 Fe2 178.1(4) . . ? O3 C3 Fe2 176.5(4) . . ? O4 C4 Fe2 176.9(4) . . ? C6 C5 S1 115.9(3) . . ? C7 C6 C5 116.7(3) . . ? C6 C7 S2 118.5(3) . . ? N1 C8 C9 116.3(3) . . ? C10 C9 C8 123.1(4) . . ? C16 C11 C12 119.0(4) . . ? C16 C11 P1 122.0(3) . . ? C12 C11 P1 118.7(3) . . ? C13 C12 C11 120.8(4) . . ? C14 C13 C12 119.6(4) . . ? C13 C14 C15 120.4(4) . . ? C14 C15 C16 120.1(4) . . ? C11 C16 C15 120.1(4) . . ? C22 C17 C18 118.7(4) . . ? C22 C17 P1 121.7(3) . . ? C18 C17 P1 119.1(3) . . ? C19 C18 C17 120.5(4) . . ? C20 C19 C18 119.8(4) . . ? C21 C20 C19 120.9(4) . . ? C20 C21 C22 119.4(4) . . ? C17 C22 C21 120.5(4) . . ? C24 C23 C28 118.1(4) . . ? C24 C23 P2 124.0(3) . . ? C28 C23 P2 117.6(3) . . ? C25 C24 C23 120.6(4) . . ? C26 C25 C24 120.3(4) . . ? C25 C26 C27 120.2(4) . . ? C26 C27 C28 119.6(4) . . ? C27 C28 C23 121.1(4) . . ? C34 C29 C30 119.2(4) . . ? C34 C29 P2 122.3(3) . . ? C30 C29 P2 118.4(3) . . ? C31 C30 C29 120.6(4) . . ? C30 C31 C32 120.1(4) . . ? C33 C32 C31 119.0(4) . . ? C34 C33 C32 121.0(4) . . ? C33 C34 C29 120.0(4) . . ? Cl2 C40 Cl1 111.6(2) . . ? Cl4 C50 Cl3 114.9(3) . . ? F2 B1 F4 110.2(4) . . ? F2 B1 F1 109.8(4) . . ? F4 B1 F1 108.6(4) . . ? F2 B1 F3 109.6(4) . . ? F4 B1 F3 110.2(4) . . ? F1 B1 F3 108.4(4) . . ? 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 C1 Fe1 Fe2 C2 -1.1(3) . . . . ? P2 Fe1 Fe2 C2 -135.3(2) . . . . ? P1 Fe1 Fe2 C2 143.8(2) . . . . ? S2 Fe1 Fe2 C2 -50.8(2) . . . . ? S1 Fe1 Fe2 C2 61.4(2) . . . . ? C1 Fe1 Fe2 C3 -133.7(2) . . . . ? P2 Fe1 Fe2 C3 92.12(14) . . . . ? P1 Fe1 Fe2 C3 11.22(14) . . . . ? S2 Fe1 Fe2 C3 176.68(14) . . . . ? S1 Fe1 Fe2 C3 -71.16(14) . . . . ? C1 Fe1 Fe2 C4 126.7(2) . . . . ? P2 Fe1 Fe2 C4 -7.51(15) . . . . ? P1 Fe1 Fe2 C4 -88.41(14) . . . . ? S2 Fe1 Fe2 C4 77.05(14) . . . . ? S1 Fe1 Fe2 C4 -170.80(14) . . . . ? C1 Fe1 Fe2 S2 49.6(2) . . . . ? P2 Fe1 Fe2 S2 -84.56(5) . . . . ? P1 Fe1 Fe2 S2 -165.46(5) . . . . ? S1 Fe1 Fe2 S2 112.15(5) . . . . ? C1 Fe1 Fe2 S1 -62.5(2) . . . . ? P2 Fe1 Fe2 S1 163.29(5) . . . . ? P1 Fe1 Fe2 S1 82.38(5) . . . . ? S2 Fe1 Fe2 S1 -112.15(5) . . . . ? C8 N1 P1 C17 -81.7(3) . . . . ? P2 N1 P1 C17 121.55(17) . . . . ? C8 N1 P1 C11 31.0(4) . . . . ? P2 N1 P1 C11 -125.72(17) . . . . ? C8 N1 P1 Fe1 157.0(3) . . . . ? P2 N1 P1 Fe1 0.33(13) . . . . ? C8 N1 P1 P2 156.7(4) . . . . ? C1 Fe1 P1 N1 -90.90(16) . . . . ? P2 Fe1 P1 N1 -0.26(10) . . . . ? S2 Fe1 P1 N1 64.4(2) . . . . ? S1 Fe1 P1 N1 167.52(11) . . . . ? Fe2 Fe1 P1 N1 111.52(11) . . . . ? C1 Fe1 P1 C17 155.45(19) . . . . ? P2 Fe1 P1 C17 -113.91(15) . . . . ? S2 Fe1 P1 C17 -49.3(2) . . . . ? S1 Fe1 P1 C17 53.88(15) . . . . ? Fe2 Fe1 P1 C17 -2.12(15) . . . . ? C1 Fe1 P1 C11 27.42(19) . . . . ? P2 Fe1 P1 C11 118.06(15) . . . . ? S2 Fe1 P1 C11 -177.30(19) . . . . ? S1 Fe1 P1 C11 -74.16(15) . . . . ? Fe2 Fe1 P1 C11 -130.15(14) . . . . ? C1 Fe1 P1 P2 -90.64(13) . . . . ? S2 Fe1 P1 P2 64.64(16) . . . . ? S1 Fe1 P1 P2 167.78(5) . . . . ? Fe2 Fe1 P1 P2 111.79(4) . . . . ? C8 N1 P2 C29 77.2(3) . . . . ? P1 N1 P2 C29 -123.08(17) . . . . ? C8 N1 P2 C23 -37.3(3) . . . . ? P1 N1 P2 C23 122.49(17) . . . . ? C8 N1 P2 Fe1 -160.1(3) . . . . ? P1 N1 P2 Fe1 -0.33(13) . . . . ? C8 N1 P2 P1 -159.7(4) . . . . ? C1 Fe1 P2 N1 100.24(17) . . . . ? P1 Fe1 P2 N1 0.26(10) . . . . ? S2 Fe1 P2 N1 -164.64(11) . . . . ? S1 Fe1 P2 N1 -48.7(2) . . . . ? Fe2 Fe1 P2 N1 -107.72(11) . . . . ? C1 Fe1 P2 C29 -144.3(2) . . . . ? P1 Fe1 P2 C29 115.69(15) . . . . ? S2 Fe1 P2 C29 -49.21(16) . . . . ? S1 Fe1 P2 C29 66.7(2) . . . . ? Fe2 Fe1 P2 C29 7.71(16) . . . . ? C1 Fe1 P2 C23 -10.5(2) . . . . ? P1 Fe1 P2 C23 -110.46(15) . . . . ? S2 Fe1 P2 C23 84.63(15) . . . . ? S1 Fe1 P2 C23 -159.4(2) . . . . ? Fe2 Fe1 P2 C23 141.56(15) . . . . ? C1 Fe1 P2 P1 99.98(13) . . . . ? S2 Fe1 P2 P1 -164.90(5) . . . . ? S1 Fe1 P2 P1 -48.96(17) . . . . ? Fe2 Fe1 P2 P1 -107.98(4) . . . . ? C17 P1 P2 N1 -78.0(2) . . . . ? C11 P1 P2 N1 76.8(2) . . . . ? Fe1 P1 P2 N1 -179.59(16) . . . . ? N1 P1 P2 C29 77.5(2) . . . . ? C17 P1 P2 C29 -0.5(2) . . . . ? C11 P1 P2 C29 154.4(2) . . . . ? Fe1 P1 P2 C29 -102.04(17) . . . . ? N1 P1 P2 C23 -74.7(2) . . . . ? C17 P1 P2 C23 -152.7(2) . . . . ? C11 P1 P2 C23 2.1(2) . . . . ? Fe1 P1 P2 C23 105.74(15) . . . . ? N1 P1 P2 Fe1 179.59(16) . . . . ? C17 P1 P2 Fe1 101.56(16) . . . . ? C11 P1 P2 Fe1 -103.60(18) . . . . ? C1 Fe1 S1 C5 34.51(19) . . . . ? P2 Fe1 S1 C5 -177.00(19) . . . . ? P1 Fe1 S1 C5 136.71(14) . . . . ? S2 Fe1 S1 C5 -59.34(14) . . . . ? Fe2 Fe1 S1 C5 -109.50(14) . . . . ? C1 Fe1 S1 Fe2 144.01(13) . . . . ? P2 Fe1 S1 Fe2 -67.50(17) . . . . ? P1 Fe1 S1 Fe2 -113.79(4) . . . . ? S2 Fe1 S1 Fe2 50.16(4) . . . . ? C2 Fe2 S1 C5 -44.06(19) . . . . ? C3 Fe2 S1 C5 -138.16(19) . . . . ? C4 Fe2 S1 C5 134.0(5) . . . . ? S2 Fe2 S1 C5 52.36(15) . . . . ? Fe1 Fe2 S1 C5 101.58(15) . . . . ? C2 Fe2 S1 Fe1 -145.64(13) . . . . ? C3 Fe2 S1 Fe1 120.26(13) . . . . ? C4 Fe2 S1 Fe1 32.4(5) . . . . ? S2 Fe2 S1 Fe1 -49.22(4) . . . . ? C1 Fe1 S2 C7 -43.13(18) . . . . ? P2 Fe1 S2 C7 -137.88(14) . . . . ? P1 Fe1 S2 C7 161.21(19) . . . . ? S1 Fe1 S2 C7 56.64(14) . . . . ? Fe2 Fe1 S2 C7 106.98(14) . . . . ? C1 Fe1 S2 Fe2 -150.11(13) . . . . ? P2 Fe1 S2 Fe2 115.14(4) . . . . ? P1 Fe1 S2 Fe2 54.23(16) . . . . ? S1 Fe1 S2 Fe2 -50.34(4) . . . . ? C2 Fe2 S2 C7 46.94(19) . . . . ? C3 Fe2 S2 C7 -118.8(6) . . . . ? C4 Fe2 S2 C7 141.65(19) . . . . ? S1 Fe2 S2 C7 -54.34(15) . . . . ? Fe1 Fe2 S2 C7 -103.63(15) . . . . ? C2 Fe2 S2 Fe1 150.57(13) . . . . ? C3 Fe2 S2 Fe1 -15.1(6) . . . . ? C4 Fe2 S2 Fe1 -114.72(13) . . . . ? S1 Fe2 S2 Fe1 49.30(4) . . . . ? P2 Fe1 C1 O1 111(3) . . . . ? P1 Fe1 C1 O1 -176(3) . . . . ? S2 Fe1 C1 O1 10(3) . . . . ? S1 Fe1 C1 O1 -77(3) . . . . ? Fe2 Fe1 C1 O1 -29(3) . . . . ? C3 Fe2 C2 O2 -159(12) . . . . ? C4 Fe2 C2 O2 -69(12) . . . . ? S2 Fe2 C2 O2 24(12) . . . . ? S1 Fe2 C2 O2 111(12) . . . . ? Fe1 Fe2 C2 O2 64(12) . . . . ? C2 Fe2 C3 O3 50(6) . . . . ? C4 Fe2 C3 O3 -44(6) . . . . ? S2 Fe2 C3 O3 -144(6) . . . . ? S1 Fe2 C3 O3 152(6) . . . . ? Fe1 Fe2 C3 O3 -157(6) . . . . ? C2 Fe2 C4 O4 -122(7) . . . . ? C3 Fe2 C4 O4 -28(7) . . . . ? S2 Fe2 C4 O4 140(7) . . . . ? S1 Fe2 C4 O4 60(7) . . . . ? Fe1 Fe2 C4 O4 88(7) . . . . ? Fe1 S1 C5 C6 67.9(3) . . . . ? Fe2 S1 C5 C6 -7.1(3) . . . . ? S1 C5 C6 C7 -58.9(4) . . . . ? C5 C6 C7 S2 56.3(4) . . . . ? Fe1 S2 C7 C6 -62.1(3) . . . . ? Fe2 S2 C7 C6 13.1(4) . . . . ? P1 N1 C8 C9 71.5(5) . . . . ? P2 N1 C8 C9 -136.3(3) . . . . ? N1 C8 C9 C10 -138.4(4) . . . . ? N1 P1 C11 C16 -55.8(4) . . . . ? C17 P1 C11 C16 60.4(4) . . . . ? Fe1 P1 C11 C16 -165.2(3) . . . . ? P2 P1 C11 C16 -98.5(3) . . . . ? N1 P1 C11 C12 130.5(3) . . . . ? C17 P1 C11 C12 -113.2(3) . . . . ? Fe1 P1 C11 C12 21.2(4) . . . . ? P2 P1 C11 C12 87.9(3) . . . . ? C16 C11 C12 C13 0.4(6) . . . . ? P1 C11 C12 C13 174.3(3) . . . . ? C11 C12 C13 C14 0.6(6) . . . . ? C12 C13 C14 C15 -0.1(6) . . . . ? C13 C14 C15 C16 -1.4(6) . . . . ? C12 C11 C16 C15 -2.0(6) . . . . ? P1 C11 C16 C15 -175.6(3) . . . . ? C14 C15 C16 C11 2.5(6) . . . . ? N1 P1 C17 C22 -23.6(4) . . . . ? C11 P1 C17 C22 -141.9(3) . . . . ? Fe1 P1 C17 C22 81.8(3) . . . . ? P2 P1 C17 C22 18.3(4) . . . . ? N1 P1 C17 C18 163.9(3) . . . . ? C11 P1 C17 C18 45.6(3) . . . . ? Fe1 P1 C17 C18 -90.7(3) . . . . ? P2 P1 C17 C18 -154.2(3) . . . . ? C22 C17 C18 C19 -0.9(6) . . . . ? P1 C17 C18 C19 171.9(3) . . . . ? C17 C18 C19 C20 2.3(6) . . . . ? C18 C19 C20 C21 -2.6(6) . . . . ? C19 C20 C21 C22 1.5(6) . . . . ? C18 C17 C22 C21 -0.2(6) . . . . ? P1 C17 C22 C21 -172.8(3) . . . . ? C20 C21 C22 C17 -0.1(6) . . . . ? N1 P2 C23 C24 134.4(3) . . . . ? C29 P2 C23 C24 17.6(4) . . . . ? Fe1 P2 C23 C24 -121.2(3) . . . . ? P1 P2 C23 C24 174.5(3) . . . . ? N1 P2 C23 C28 -51.6(3) . . . . ? C29 P2 C23 C28 -168.3(3) . . . . ? Fe1 P2 C23 C28 52.9(3) . . . . ? P1 P2 C23 C28 -11.4(4) . . . . ? C28 C23 C24 C25 -3.2(6) . . . . ? P2 C23 C24 C25 170.9(3) . . . . ? C23 C24 C25 C26 1.0(6) . . . . ? C24 C25 C26 C27 2.1(6) . . . . ? C25 C26 C27 C28 -2.9(6) . . . . ? C26 C27 C28 C23 0.6(6) . . . . ? C24 C23 C28 C27 2.3(6) . . . . ? P2 C23 C28 C27 -172.1(3) . . . . ? N1 P2 C29 C34 -1.0(4) . . . . ? C23 P2 C29 C34 112.9(3) . . . . ? Fe1 P2 C29 C34 -107.7(3) . . . . ? P1 P2 C29 C34 -42.9(4) . . . . ? N1 P2 C29 C30 175.2(3) . . . . ? C23 P2 C29 C30 -70.9(3) . . . . ? Fe1 P2 C29 C30 68.5(3) . . . . ? P1 P2 C29 C30 133.2(3) . . . . ? C34 C29 C30 C31 -2.2(6) . . . . ? P2 C29 C30 C31 -178.5(3) . . . . ? C29 C30 C31 C32 1.8(6) . . . . ? C30 C31 C32 C33 -0.2(6) . . . . ? C31 C32 C33 C34 -1.0(6) . . . . ? C32 C33 C34 C29 0.6(6) . . . . ? C30 C29 C34 C33 1.0(6) . . . . ? P2 C29 C34 C33 177.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.780 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.089