# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Shaowu Du' _publ_contact_author_email swdu@fjirsm.ac.cn _publ_section_title ; Synthesis and characterization of diiron dithiolate complexes containing a quinoxaline bridge ; loop_ _publ_author_name 'Shaowu Du' 'Fenfen Xu' 'Jie Zhang' A.Bond # Attachment '- cifs.txt' data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 816112' #TrackingRef '- cifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16.50 H9 Cl Fe2 N2 O6 S2' _chemical_formula_weight 542.53 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.801(2) _cell_length_b 11.254(4) _cell_length_c 13.330(5) _cell_angle_alpha 89.908(12) _cell_angle_beta 81.324(10) _cell_angle_gamma 77.667(10) _cell_volume 984.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2653 _cell_measurement_theta_min 3.78 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max .20 _exptl_crystal_size_mid .12 _exptl_crystal_size_min .09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 542 _exptl_absorpt_coefficient_mu 1.859 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5642 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku Crystalclear)' _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 'Saturn70 (4x4 bin mode)' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 7453 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4329 _reflns_number_gt 3758 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1065P)^2^+2.3408P] 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 4329 _refine_ls_number_parameters 290 _refine_ls_number_restraints 1 _refine_ls_R_factor_ref 0.0546 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1584 _refine_ls_wR_factor_gt 0.1376 _refine_ls_goodness_of_fit_ref 1.040 _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 -2.16092(7) 0.34988(4) 1.29189(4) 0.01466(17) Uani 1 1 d . . . Fe2 Fe -2.26778(7) 0.19496(4) 1.41309(4) 0.01587(17) Uani 1 1 d . . . S1 S -1.94768(13) 0.17884(8) 1.33045(6) 0.0161(2) Uani 1 1 d . . . S2 S -2.37958(12) 0.23303(7) 1.26249(6) 0.0155(2) Uani 1 1 d . . . N1 N -1.7354(5) 0.1178(3) 1.0670(2) 0.0168(6) Uani 1 1 d . . . N2 N -2.1217(4) 0.1658(3) 1.0042(2) 0.0172(6) Uani 1 1 d . . . O1 O -2.0321(6) 0.4194(3) 1.0829(2) 0.0361(7) Uani 1 1 d . . . O2 O -1.9193(5) 0.4928(3) 1.3859(3) 0.0363(7) Uani 1 1 d . . . O3 O -2.5145(5) 0.5503(3) 1.3475(3) 0.0383(8) Uani 1 1 d . . . O4 O -2.3038(6) -0.0593(3) 1.4255(3) 0.0476(10) Uani 1 1 d . . . O5 O -2.6797(4) 0.3150(3) 1.5093(2) 0.0282(6) Uani 1 1 d . . . O6 O -2.1204(5) 0.2250(4) 1.6054(2) 0.0419(8) Uani 1 1 d . . . C1 C -2.0786(6) 0.3918(3) 1.1642(3) 0.0226(7) Uani 1 1 d . . . C2 C -2.0122(6) 0.4350(4) 1.3515(3) 0.0225(7) Uani 1 1 d . . . C3 C -2.3798(6) 0.4723(4) 1.3252(3) 0.0244(8) Uani 1 1 d . . . C4 C -2.2885(6) 0.0386(4) 1.4232(3) 0.0276(8) Uani 1 1 d . . . C5 C -2.5213(6) 0.2687(3) 1.4716(3) 0.0199(7) Uani 1 1 d . . . C6 C -2.1749(6) 0.2143(4) 1.5300(3) 0.0261(8) Uani 1 1 d . . . C7 C -1.8720(5) 0.0578(3) 1.2302(3) 0.0178(7) Uani 1 1 d . . . H7A H -1.7304 0.0185 1.2302 0.021 Uiso 1 1 calc R . . H7B H -1.9530 -0.0029 1.2462 0.021 Uiso 1 1 calc R . . C8 C -2.2773(6) 0.1089(3) 1.1662(3) 0.0177(7) Uani 1 1 d . . . C9 C -1.8968(5) 0.1021(3) 1.1261(3) 0.0161(6) Uani 1 1 d . . . C10 C -2.0945(5) 0.1266(3) 1.0952(3) 0.0173(7) Uani 1 1 d . . . C11 C -1.7586(5) 0.1593(3) 0.9713(3) 0.0166(7) Uani 1 1 d . . . C12 C -1.9534(5) 0.1840(3) 0.9403(3) 0.0169(7) Uani 1 1 d . . . C13 C -1.9746(6) 0.2283(4) 0.8426(3) 0.0222(7) Uani 1 1 d . . . C14 C -1.8075(6) 0.2464(4) 0.7782(3) 0.0248(8) Uani 1 1 d . . . C15 C -1.6130(6) 0.2212(4) 0.8093(3) 0.0250(8) Uani 1 1 d . . . C16 C -1.5880(6) 0.1784(4) 0.9035(3) 0.0219(7) Uani 1 1 d . . . C17 C -1.5255(18) 0.4340(10) 1.0006(8) 0.048(2) Uiso 0.50 1 d PD . . Cl Cl -1.5914(4) 0.5012(3) 1.1098(2) 0.1138(11) Uani 1 1 d D . . H8A H -2.379(7) 0.107(4) 1.128(3) 0.013(10) Uiso 1 1 d . . . H8B H -2.246(8) 0.039(5) 1.203(4) 0.028(12) Uiso 1 1 d . . . H13 H -2.113(7) 0.249(4) 0.825(3) 0.015(10) Uiso 1 1 d . . . H14 H -1.838(8) 0.276(5) 0.713(4) 0.032(13) Uiso 1 1 d . . . H15 H -1.498(7) 0.231(4) 0.758(4) 0.019(11) Uiso 1 1 d . . . H16 H -1.474(8) 0.161(5) 0.916(4) 0.024(12) Uiso 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 0.0144(3) 0.0151(3) 0.0147(3) 0.00212(18) -0.00200(19) -0.00362(19) Fe2 0.0159(3) 0.0169(3) 0.0129(3) 0.00292(18) 0.00074(19) -0.00146(19) S1 0.0139(4) 0.0205(4) 0.0128(4) 0.0017(3) -0.0024(3) -0.0012(3) S2 0.0128(4) 0.0172(4) 0.0160(4) 0.0017(3) -0.0013(3) -0.0031(3) N1 0.0157(14) 0.0184(14) 0.0154(14) -0.0006(11) -0.0031(11) -0.0016(11) N2 0.0134(14) 0.0221(14) 0.0154(14) -0.0002(11) -0.0017(11) -0.0030(11) O1 0.052(2) 0.0369(17) 0.0207(14) 0.0086(12) 0.0012(13) -0.0175(15) O2 0.0352(17) 0.0361(17) 0.0434(19) -0.0038(14) -0.0147(15) -0.0143(14) O3 0.0236(15) 0.0236(15) 0.062(2) -0.0065(14) -0.0017(15) 0.0031(12) O4 0.053(2) 0.0208(15) 0.057(2) 0.0028(15) 0.0251(18) -0.0057(15) O5 0.0231(15) 0.0284(14) 0.0269(15) -0.0008(12) 0.0042(12) 0.0023(12) O6 0.0376(18) 0.064(2) 0.0194(15) -0.0036(15) -0.0090(13) 0.0033(16) C1 0.0226(18) 0.0205(17) 0.0258(19) 0.0040(14) -0.0043(15) -0.0067(14) C2 0.0202(18) 0.0230(17) 0.0236(18) 0.0024(14) -0.0038(14) -0.0029(14) C3 0.0244(19) 0.0218(18) 0.029(2) 0.0013(15) -0.0049(15) -0.0094(15) C4 0.026(2) 0.0227(19) 0.027(2) 0.0044(15) 0.0109(16) -0.0001(15) C5 0.0224(18) 0.0195(16) 0.0178(16) 0.0050(13) -0.0027(14) -0.0048(14) C6 0.0196(18) 0.033(2) 0.0212(19) 0.0035(15) 0.0001(14) 0.0020(15) C7 0.0169(16) 0.0199(16) 0.0139(15) 0.0007(13) -0.0011(12) 0.0014(13) C8 0.0179(17) 0.0183(16) 0.0171(16) -0.0019(13) -0.0025(13) -0.0049(13) C9 0.0174(16) 0.0148(15) 0.0157(16) 0.0008(12) -0.0037(13) -0.0018(12) C10 0.0163(16) 0.0177(15) 0.0177(16) -0.0001(13) -0.0023(13) -0.0034(13) C11 0.0151(16) 0.0207(16) 0.0135(15) -0.0013(13) -0.0008(12) -0.0035(13) C12 0.0166(16) 0.0201(16) 0.0146(16) -0.0004(13) -0.0039(13) -0.0044(13) C13 0.0236(19) 0.0256(18) 0.0176(17) 0.0031(14) -0.0063(14) -0.0040(14) C14 0.031(2) 0.0273(19) 0.0163(17) 0.0068(14) -0.0039(15) -0.0072(16) C15 0.0251(19) 0.0273(19) 0.0216(18) 0.0034(15) 0.0025(15) -0.0075(15) C16 0.0160(18) 0.0262(18) 0.0237(19) 0.0010(15) -0.0025(14) -0.0055(14) Cl 0.0804(14) 0.151(2) 0.140(2) 0.0868(19) -0.0692(15) -0.0556(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 C2 1.798(4) . ? Fe1 C3 1.799(4) . ? Fe1 C1 1.804(4) . ? Fe1 S1 2.2587(11) . ? Fe1 S2 2.2598(11) . ? Fe1 Fe2 2.5211(9) . ? Fe2 C6 1.797(4) . ? Fe2 C4 1.798(4) . ? Fe2 C5 1.804(4) . ? Fe2 S1 2.2569(12) . ? Fe2 S2 2.2604(12) . ? S1 C7 1.846(4) . ? S2 C8 1.846(4) . ? N1 C9 1.296(5) . ? N1 C11 1.377(4) . ? N2 C10 1.316(5) . ? N2 C12 1.372(5) . ? O1 C1 1.145(5) . ? O2 C2 1.138(5) . ? O3 C3 1.129(5) . ? O4 C4 1.129(5) . ? O5 C5 1.133(5) . ? O6 C6 1.138(5) . ? C7 C9 1.494(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C10 1.493(5) . ? C8 H8A 0.92(5) . ? C8 H8B 0.93(6) . ? C9 C10 1.436(5) . ? C11 C16 1.414(5) . ? C11 C12 1.418(5) . ? C12 C13 1.411(5) . ? C13 C14 1.369(6) . ? C13 H13 0.98(5) . ? C14 C15 1.417(6) . ? C14 H14 0.97(6) . ? C15 C16 1.365(6) . ? C15 H15 0.98(5) . ? C16 H16 0.80(5) . ? C17 C17 1.59(2) 2_267 ? C17 Cl 1.597(11) . ? C17 Cl 1.795(12) 2_267 ? Cl C17 1.795(12) 2_267 ? 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 C2 Fe1 C3 89.08(18) . . ? C2 Fe1 C1 95.53(18) . . ? C3 Fe1 C1 99.00(18) . . ? C2 Fe1 S1 87.71(13) . . ? C3 Fe1 S1 151.24(14) . . ? C1 Fe1 S1 109.76(13) . . ? C2 Fe1 S2 163.95(13) . . ? C3 Fe1 S2 87.25(13) . . ? C1 Fe1 S2 100.47(13) . . ? S1 Fe1 S2 88.02(4) . . ? C2 Fe1 Fe2 109.16(13) . . ? C3 Fe1 Fe2 98.52(13) . . ? C1 Fe1 Fe2 149.80(12) . . ? S1 Fe1 Fe2 56.03(3) . . ? S2 Fe1 Fe2 56.11(3) . . ? C6 Fe2 C4 99.4(2) . . ? C6 Fe2 C5 89.84(17) . . ? C4 Fe2 C5 99.63(18) . . ? C6 Fe2 S1 88.57(13) . . ? C4 Fe2 S1 102.49(13) . . ? C5 Fe2 S1 157.79(12) . . ? C6 Fe2 S2 161.90(14) . . ? C4 Fe2 S2 98.66(15) . . ? C5 Fe2 S2 86.63(12) . . ? S1 Fe2 S2 88.05(4) . . ? C6 Fe2 Fe1 107.86(15) . . ? C4 Fe2 Fe1 143.83(13) . . ? C5 Fe2 Fe1 103.66(12) . . ? S1 Fe2 Fe1 56.10(3) . . ? S2 Fe2 Fe1 56.09(3) . . ? C7 S1 Fe2 113.57(13) . . ? C7 S1 Fe1 115.56(12) . . ? Fe2 S1 Fe1 67.88(3) . . ? C8 S2 Fe1 115.64(12) . . ? C8 S2 Fe2 113.76(13) . . ? Fe1 S2 Fe2 67.80(3) . . ? C9 N1 C11 117.5(3) . . ? C10 N2 C12 117.2(3) . . ? O1 C1 Fe1 178.0(4) . . ? O2 C2 Fe1 176.8(4) . . ? O3 C3 Fe1 178.3(4) . . ? O4 C4 Fe2 177.0(5) . . ? O5 C5 Fe2 179.2(3) . . ? O6 C6 Fe2 178.0(4) . . ? C9 C7 S1 114.0(2) . . ? C9 C7 H7A 108.8 . . ? S1 C7 H7A 108.8 . . ? C9 C7 H7B 108.8 . . ? S1 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C10 C8 S2 114.0(2) . . ? C10 C8 H8A 107(3) . . ? S2 C8 H8A 107(3) . . ? C10 C8 H8B 111(3) . . ? S2 C8 H8B 105(3) . . ? H8A C8 H8B 113(4) . . ? N1 C9 C10 122.4(3) . . ? N1 C9 C7 117.6(3) . . ? C10 C9 C7 120.0(3) . . ? N2 C10 C9 121.6(3) . . ? N2 C10 C8 117.7(3) . . ? C9 C10 C8 120.7(3) . . ? N1 C11 C16 120.1(3) . . ? N1 C11 C12 120.4(3) . . ? C16 C11 C12 119.5(3) . . ? N2 C12 C13 119.5(3) . . ? N2 C12 C11 120.9(3) . . ? C13 C12 C11 119.6(3) . . ? C14 C13 C12 120.0(3) . . ? C14 C13 H13 123(3) . . ? C12 C13 H13 117(3) . . ? C13 C14 C15 120.3(4) . . ? C13 C14 H14 114(3) . . ? C15 C14 H14 126(3) . . ? C16 C15 C14 121.0(4) . . ? C16 C15 H15 122(3) . . ? C14 C15 H15 117(3) . . ? C15 C16 C11 119.7(4) . . ? C15 C16 H16 117(4) . . ? C11 C16 H16 123(4) . . ? C17 C17 Cl 68.4(7) 2_267 . ? C17 C17 Cl 55.8(7) 2_267 2_267 ? Cl C17 Cl 124.3(7) . 2_267 ? C17 Cl C17 55.7(7) . 2_267 ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 2.532 _refine_diff_density_min -2.780 _refine_diff_density_rms 0.191 _publ_section_references ; Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ; #==END data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 816113' #TrackingRef '- cifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H30 Fe2 N2 O5 P2 S2' _chemical_formula_weight 856.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 9.2471(6) _cell_length_b 12.8115(8) _cell_length_c 16.3337(10) _cell_angle_alpha 98.516(4) _cell_angle_beta 95.659(2) _cell_angle_gamma 96.527(3) _cell_volume 1888.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4370 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max .21 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 1.011 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4027 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku Crystalclear)' _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 'Saturn70 (4x4 bin mode)' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 14834 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8510 _reflns_number_gt 6297 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0726P)^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 8510 _refine_ls_number_parameters 594 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0643 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1294 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 0.39790(4) 0.50049(3) 0.23693(2) 0.02134(12) Uani 1 1 d . . . Fe2 Fe 0.46786(5) 0.31880(4) 0.24553(3) 0.02679(12) Uani 1 1 d . . . S1 S 0.46920(8) 0.44659(6) 0.35899(4) 0.02259(16) Uani 1 1 d . . . S2 S 0.23610(8) 0.34903(6) 0.20818(4) 0.02544(17) Uani 1 1 d . . . P1 P 0.26535(8) 0.63399(6) 0.26223(4) 0.01995(16) Uani 1 1 d . . . P2 P 0.42961(9) 0.77456(6) 0.15525(5) 0.02490(17) Uani 1 1 d . . . N1 N 0.3189(3) 0.24585(19) 0.47061(15) 0.0274(5) Uani 1 1 d . . . N2 N 0.1013(3) 0.15812(19) 0.33593(17) 0.0298(6) Uani 1 1 d . . . O1 O 0.3887(3) 0.4973(2) 0.05729(13) 0.0409(6) Uani 1 1 d . . . O2 O 0.6779(3) 0.6381(2) 0.27971(17) 0.0467(6) Uani 1 1 d . . . O3 O 0.7840(3) 0.3814(3) 0.2613(2) 0.0625(8) Uani 1 1 d . . . O4 O 0.4665(4) 0.2363(3) 0.06803(17) 0.0808(12) Uani 1 1 d . . . O5 O 0.4471(3) 0.1136(2) 0.30839(17) 0.0475(7) Uani 1 1 d . . . C1 C 0.3914(3) 0.5011(3) 0.12779(19) 0.0290(6) Uani 1 1 d . . . C2 C 0.5674(3) 0.5846(3) 0.25975(19) 0.0303(7) Uani 1 1 d . . . C3 C 0.6619(4) 0.3552(3) 0.2562(2) 0.0413(8) Uani 1 1 d . . . C4 C 0.4682(5) 0.2672(3) 0.1376(2) 0.0500(10) Uani 1 1 d . . . C5 C 0.4530(4) 0.1936(3) 0.2848(2) 0.0334(7) Uani 1 1 d . . . C6 C 0.3286(3) 0.4179(2) 0.42830(18) 0.0245(6) Uani 1 1 d . . . C7 C 0.1098(3) 0.3270(3) 0.2863(2) 0.0267(6) Uani 1 1 d . . . C8 C 0.1604(3) 0.2591(2) 0.34734(18) 0.0244(6) Uani 1 1 d . . . C9 C 0.2683(3) 0.3030(2) 0.41612(18) 0.0233(6) Uani 1 1 d . . . C10 C 0.2610(4) 0.1404(2) 0.4586(2) 0.0289(6) Uani 1 1 d . . . C11 C 0.3153(4) 0.0739(3) 0.5135(2) 0.0386(8) Uani 1 1 d . . . C12 C 0.2580(5) -0.0304(3) 0.5028(2) 0.0434(9) Uani 1 1 d . . . C13 C 0.1452(4) -0.0730(3) 0.4378(2) 0.0425(9) Uani 1 1 d . . . C14 C 0.0945(4) -0.0119(3) 0.3834(2) 0.0385(8) Uani 1 1 d . . . C15 C 0.1527(3) 0.0974(2) 0.3925(2) 0.0297(7) Uani 1 1 d . . . C16 C 0.3673(3) 0.7660(2) 0.25916(19) 0.0252(6) Uani 1 1 d . . . C17 C 0.0933(3) 0.6341(2) 0.19788(16) 0.0214(6) Uani 1 1 d . . . C18 C 0.0164(3) 0.7222(2) 0.20969(19) 0.0262(6) Uani 1 1 d . . . C19 C -0.1147(4) 0.7234(3) 0.1622(2) 0.0298(7) Uani 1 1 d . . . C20 C -0.1741(4) 0.6372(3) 0.1028(2) 0.0321(7) Uani 1 1 d . . . C21 C -0.0995(4) 0.5494(3) 0.0899(2) 0.0321(7) Uani 1 1 d . . . C22 C 0.0338(3) 0.5479(2) 0.13683(18) 0.0267(6) Uani 1 1 d . . . C23 C 0.2095(3) 0.6499(2) 0.36695(17) 0.0201(5) Uani 1 1 d . . . C24 C 0.0649(3) 0.6205(2) 0.38059(19) 0.0260(6) Uani 1 1 d . . . C25 C 0.0280(4) 0.6274(3) 0.4618(2) 0.0333(7) Uani 1 1 d . . . C26 C 0.1336(4) 0.6635(3) 0.5293(2) 0.0353(8) Uani 1 1 d . . . C27 C 0.2765(4) 0.6913(2) 0.51591(19) 0.0293(7) Uani 1 1 d . . . C28 C 0.3156(3) 0.6846(2) 0.43625(18) 0.0235(6) Uani 1 1 d . . . C29 C 0.2703(4) 0.8186(3) 0.1020(2) 0.0356(8) Uani 1 1 d . . . C30 C 0.1983(5) 0.7541(4) 0.0305(3) 0.0552(13) Uani 1 1 d . . . C31 C 0.0675(7) 0.7813(7) -0.0081(4) 0.092(3) Uani 1 1 d . . . C32 C 0.0148(6) 0.8688(7) 0.0228(5) 0.112(3) Uani 1 1 d . . . C33 C 0.0860(5) 0.9360(5) 0.0930(5) 0.087(2) Uani 1 1 d . . . H33A H 0.0475 0.9973 0.1133 0.104 Uiso 1 1 calc R . . C34 C 0.2136(4) 0.9121(3) 0.1328(3) 0.0510(11) Uani 1 1 d . . . C35 C 0.5586(3) 0.8983(2) 0.17465(19) 0.0256(6) Uani 1 1 d . . . C36 C 0.5783(4) 0.9507(3) 0.1072(2) 0.0407(8) Uani 1 1 d . . . C37 C 0.6847(4) 1.0374(3) 0.1139(3) 0.0483(10) Uani 1 1 d . . . C38 C 0.7713(4) 1.0748(3) 0.1890(3) 0.0427(9) Uani 1 1 d . . . C39 C 0.7506(4) 1.0248(3) 0.2562(2) 0.0397(8) Uani 1 1 d . . . C40 C 0.6463(4) 0.9360(3) 0.2492(2) 0.0318(7) Uani 1 1 d . . . H36 H 0.524(4) 0.920(3) 0.053(2) 0.032(9) Uiso 1 1 d . . . H26 H 0.113(4) 0.662(3) 0.584(2) 0.030(9) Uiso 1 1 d . . . H40 H 0.638(4) 0.895(3) 0.294(2) 0.039(10) Uiso 1 1 d . . . H22 H 0.089(4) 0.488(3) 0.1291(19) 0.023(8) Uiso 1 1 d . . . H14 H 0.023(4) -0.036(3) 0.341(2) 0.031(9) Uiso 1 1 d . . . H28 H 0.405(4) 0.698(2) 0.4274(19) 0.022(8) Uiso 1 1 d . . . H18 H 0.058(4) 0.783(3) 0.254(2) 0.032(9) Uiso 1 1 d . . . H39 H 0.814(4) 1.048(3) 0.307(2) 0.042(10) Uiso 1 1 d . . . H19 H -0.157(4) 0.771(3) 0.173(2) 0.035(10) Uiso 1 1 d . . . H7A H 0.028(4) 0.297(3) 0.254(2) 0.034(9) Uiso 1 1 d . . . H25 H -0.064(5) 0.616(3) 0.467(2) 0.045(11) Uiso 1 1 d . . . H24 H -0.008(4) 0.600(3) 0.336(2) 0.040(10) Uiso 1 1 d . . . H6B H 0.262(4) 0.461(3) 0.421(2) 0.035(10) Uiso 1 1 d . . . H20 H -0.265(5) 0.638(3) 0.073(3) 0.054(12) Uiso 1 1 d . . . H27 H 0.336(5) 0.714(3) 0.552(2) 0.044(12) Uiso 1 1 d . . . H37 H 0.694(5) 1.072(3) 0.064(3) 0.055(12) Uiso 1 1 d . . . H11 H 0.393(5) 0.099(3) 0.558(3) 0.052(12) Uiso 1 1 d . . . H31 H 0.033(6) 0.744(4) -0.047(3) 0.071(17) Uiso 1 1 d . . . H21 H -0.136(5) 0.487(3) 0.050(3) 0.053(12) Uiso 1 1 d . . . H12 H 0.276(6) -0.072(4) 0.540(3) 0.073(15) Uiso 1 1 d . . . H13 H 0.110(5) -0.151(4) 0.435(3) 0.070(14) Uiso 1 1 d . . . H30 H 0.248(5) 0.697(4) 0.010(3) 0.057(14) Uiso 1 1 d . . . H16B H 0.307(3) 0.828(2) 0.2761(17) 0.013(7) Uiso 1 1 d . . . H16A H 0.453(4) 0.770(2) 0.296(2) 0.024(8) Uiso 1 1 d . . . H6A H 0.382(4) 0.444(3) 0.484(2) 0.035(9) Uiso 1 1 d . . . H7B H 0.095(4) 0.395(3) 0.315(2) 0.029(9) Uiso 1 1 d . . . H34 H 0.258(5) 0.959(3) 0.180(3) 0.056(13) Uiso 1 1 d . . . H32 H -0.077(7) 0.895(4) 0.004(3) 0.095(18) Uiso 1 1 d . . . H38 H 0.821(5) 1.124(4) 0.189(3) 0.066(15) Uiso 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 0.0163(2) 0.0245(2) 0.0226(2) 0.00203(17) 0.00148(15) 0.00254(16) Fe2 0.0225(2) 0.0297(2) 0.0282(2) -0.00024(18) 0.00191(17) 0.01054(18) S1 0.0172(3) 0.0243(3) 0.0240(3) 0.0022(3) -0.0013(3) -0.0013(3) S2 0.0222(4) 0.0232(4) 0.0274(3) -0.0028(3) -0.0046(3) 0.0032(3) P1 0.0164(3) 0.0207(4) 0.0217(3) 0.0024(3) 0.0016(3) -0.0002(3) P2 0.0269(4) 0.0214(4) 0.0252(4) 0.0041(3) 0.0029(3) -0.0023(3) N1 0.0280(14) 0.0209(12) 0.0312(13) 0.0021(11) 0.0015(11) -0.0009(10) N2 0.0212(13) 0.0201(12) 0.0449(15) 0.0006(11) -0.0027(11) 0.0004(10) O1 0.0438(15) 0.0528(15) 0.0244(11) 0.0009(11) 0.0049(10) 0.0051(12) O2 0.0230(13) 0.0595(17) 0.0558(15) 0.0199(14) -0.0007(11) -0.0119(11) O3 0.0213(14) 0.084(2) 0.090(2) 0.0289(19) 0.0137(14) 0.0157(14) O4 0.116(3) 0.096(3) 0.0327(15) -0.0119(16) 0.0129(17) 0.054(2) O5 0.0515(17) 0.0333(14) 0.0635(17) 0.0088(13) 0.0189(14) 0.0186(12) C1 0.0220(16) 0.0322(16) 0.0321(16) 0.0032(13) 0.0026(12) 0.0041(12) C2 0.0243(16) 0.0383(18) 0.0316(16) 0.0133(14) 0.0056(13) 0.0063(14) C3 0.036(2) 0.050(2) 0.0451(19) 0.0176(17) 0.0102(16) 0.0201(17) C4 0.058(3) 0.054(2) 0.041(2) 0.0000(18) 0.0074(18) 0.029(2) C5 0.0295(18) 0.0322(18) 0.0374(17) -0.0047(15) 0.0036(14) 0.0130(14) C6 0.0240(15) 0.0221(14) 0.0243(14) -0.0017(12) 0.0032(12) -0.0032(12) C7 0.0138(14) 0.0277(16) 0.0367(16) 0.0031(14) -0.0024(12) 0.0017(12) C8 0.0154(14) 0.0229(14) 0.0332(15) -0.0006(12) 0.0017(11) 0.0025(11) C9 0.0228(15) 0.0175(13) 0.0282(14) -0.0010(11) 0.0065(12) -0.0005(11) C10 0.0303(17) 0.0192(14) 0.0366(16) 0.0021(13) 0.0039(13) 0.0037(12) C11 0.051(2) 0.0284(17) 0.0366(17) 0.0088(15) -0.0007(16) 0.0043(15) C12 0.059(3) 0.0286(18) 0.044(2) 0.0109(16) 0.0047(18) 0.0065(17) C13 0.054(2) 0.0155(15) 0.057(2) 0.0044(16) 0.0080(19) 0.0025(15) C14 0.040(2) 0.0188(15) 0.052(2) -0.0020(15) -0.0013(17) -0.0006(14) C15 0.0263(16) 0.0159(14) 0.0455(18) 0.0020(13) 0.0048(14) 0.0001(11) C16 0.0235(15) 0.0218(14) 0.0287(14) 0.0047(12) 0.0017(12) -0.0037(12) C17 0.0183(14) 0.0247(14) 0.0200(12) 0.0039(11) 0.0011(10) -0.0009(11) C18 0.0202(15) 0.0261(15) 0.0308(15) 0.0008(13) 0.0037(12) 0.0020(12) C19 0.0227(16) 0.0319(17) 0.0368(17) 0.0057(14) 0.0058(13) 0.0096(13) C20 0.0224(16) 0.0404(18) 0.0322(16) 0.0056(14) -0.0040(13) 0.0050(13) C21 0.0288(17) 0.0321(17) 0.0309(15) 0.0003(14) -0.0079(13) 0.0010(13) C22 0.0285(16) 0.0235(15) 0.0269(14) 0.0025(12) -0.0013(12) 0.0041(12) C23 0.0237(14) 0.0131(12) 0.0236(13) 0.0034(10) 0.0035(11) 0.0018(10) C24 0.0243(16) 0.0243(15) 0.0291(15) 0.0043(12) 0.0045(12) 0.0010(12) C25 0.0309(18) 0.0320(17) 0.0419(18) 0.0129(15) 0.0152(15) 0.0060(14) C26 0.049(2) 0.0350(18) 0.0264(15) 0.0083(14) 0.0130(15) 0.0136(16) C27 0.041(2) 0.0223(15) 0.0246(15) 0.0035(13) -0.0020(14) 0.0080(13) C28 0.0227(16) 0.0186(14) 0.0284(14) 0.0027(12) 0.0012(12) 0.0022(11) C29 0.0297(17) 0.0347(18) 0.0412(18) 0.0226(15) -0.0076(14) -0.0116(14) C30 0.052(3) 0.060(3) 0.046(2) 0.031(2) -0.0168(19) -0.033(2) C31 0.068(4) 0.112(5) 0.084(4) 0.073(4) -0.047(3) -0.058(4) C32 0.043(3) 0.138(6) 0.168(7) 0.134(6) -0.039(4) -0.034(4) C33 0.037(3) 0.085(4) 0.161(6) 0.095(4) 0.011(3) 0.009(2) C34 0.035(2) 0.045(2) 0.080(3) 0.036(2) 0.003(2) 0.0021(17) C35 0.0187(14) 0.0240(15) 0.0335(15) 0.0023(12) 0.0045(12) 0.0018(11) C36 0.042(2) 0.0386(19) 0.0362(18) 0.0101(16) -0.0007(16) -0.0158(16) C37 0.044(2) 0.044(2) 0.055(2) 0.0209(19) 0.0041(18) -0.0185(17) C38 0.0306(19) 0.0268(18) 0.067(3) 0.0071(18) 0.0030(17) -0.0083(15) C39 0.0266(18) 0.0395(19) 0.047(2) -0.0028(17) -0.0013(15) -0.0036(14) C40 0.0253(16) 0.0337(17) 0.0344(16) 0.0046(15) 0.0017(13) -0.0018(13) _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 C2 1.771(3) . ? Fe1 C1 1.779(3) . ? Fe1 P1 2.2284(8) . ? Fe1 S1 2.2668(8) . ? Fe1 S2 2.2706(8) . ? Fe1 Fe2 2.5056(6) . ? Fe2 C3 1.786(4) . ? Fe2 C4 1.789(4) . ? Fe2 C5 1.810(4) . ? Fe2 S2 2.2619(8) . ? Fe2 S1 2.2819(8) . ? S1 C6 1.847(3) . ? S2 C7 1.844(3) . ? P1 C17 1.819(3) . ? P1 C23 1.824(3) . ? P1 C16 1.851(3) . ? P2 C29 1.824(3) . ? P2 C35 1.839(3) . ? P2 C16 1.860(3) . ? N1 C9 1.317(4) . ? N1 C10 1.374(4) . ? N2 C8 1.325(4) . ? N2 C15 1.376(4) . ? O1 C1 1.143(4) . ? O2 C2 1.153(4) . ? O3 C3 1.132(5) . ? O4 C4 1.144(4) . ? O5 C5 1.144(4) . ? C6 C9 1.492(4) . ? C6 H6B 0.89(4) . ? C6 H6A 0.99(4) . ? C7 C8 1.492(4) . ? C7 H7A 0.89(4) . ? C7 H7B 0.95(3) . ? C8 C9 1.427(4) . ? C10 C15 1.400(4) . ? C10 C11 1.419(5) . ? C11 C12 1.360(5) . ? C11 H11 0.96(4) . ? C12 C13 1.411(5) . ? C12 H12 0.88(5) . ? C13 C14 1.354(5) . ? C13 H13 1.01(5) . ? C14 C15 1.423(4) . ? C14 H14 0.89(4) . ? C16 H16B 1.05(3) . ? C16 H16A 0.94(3) . ? C17 C22 1.394(4) . ? C17 C18 1.400(4) . ? C18 C19 1.376(4) . ? C18 H18 1.00(4) . ? C19 C20 1.379(5) . ? C19 H19 0.77(4) . ? C20 C21 1.386(5) . ? C20 H20 0.93(4) . ? C21 C22 1.389(4) . ? C21 H21 0.96(4) . ? C22 H22 0.96(3) . ? C23 C24 1.397(4) . ? C23 C28 1.405(4) . ? C24 C25 1.395(4) . ? C24 H24 0.93(4) . ? C25 C26 1.385(5) . ? C25 H25 0.86(4) . ? C26 C27 1.376(5) . ? C26 H26 0.92(3) . ? C27 C28 1.378(4) . ? C27 H27 0.77(4) . ? C28 H28 0.85(3) . ? C29 C30 1.388(5) . ? C29 C34 1.407(6) . ? C30 C31 1.411(8) . ? C30 H30 0.95(4) . ? C31 C32 1.324(12) . ? C31 H31 0.76(5) . ? C32 C33 1.385(11) . ? C32 H32 0.99(6) . ? C33 C34 1.378(6) . ? C33 H33A 0.9300 . ? C34 H34 0.93(4) . ? C35 C40 1.384(4) . ? C35 C36 1.389(5) . ? C36 C37 1.382(5) . ? C36 H36 0.97(4) . ? C37 C38 1.386(6) . ? C37 H37 0.99(4) . ? C38 C39 1.368(6) . ? C38 H38 0.74(5) . ? C39 C40 1.389(5) . ? C39 H39 0.96(4) . ? C40 H40 0.96(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 C2 Fe1 C1 93.33(14) . . ? C2 Fe1 P1 93.76(10) . . ? C1 Fe1 P1 95.75(10) . . ? C2 Fe1 S1 83.38(10) . . ? C1 Fe1 S1 155.24(10) . . ? P1 Fe1 S1 108.92(3) . . ? C2 Fe1 S2 159.67(10) . . ? C1 Fe1 S2 88.27(11) . . ? P1 Fe1 S2 106.26(3) . . ? S1 Fe1 S2 86.72(3) . . ? C2 Fe1 Fe2 103.61(10) . . ? C1 Fe1 Fe2 100.68(10) . . ? P1 Fe1 Fe2 155.21(3) . . ? S1 Fe1 Fe2 56.86(2) . . ? S2 Fe1 Fe2 56.27(2) . . ? C3 Fe2 C4 90.43(19) . . ? C3 Fe2 C5 101.83(15) . . ? C4 Fe2 C5 98.17(17) . . ? C3 Fe2 S2 151.74(12) . . ? C4 Fe2 S2 85.44(13) . . ? C5 Fe2 S2 106.43(11) . . ? C3 Fe2 S1 86.14(13) . . ? C4 Fe2 S1 156.30(14) . . ? C5 Fe2 S1 105.48(10) . . ? S2 Fe2 S1 86.57(3) . . ? C3 Fe2 Fe1 97.12(12) . . ? C4 Fe2 Fe1 101.07(12) . . ? C5 Fe2 Fe1 152.78(10) . . ? S2 Fe2 Fe1 56.61(2) . . ? S1 Fe2 Fe1 56.29(2) . . ? C6 S1 Fe1 118.31(11) . . ? C6 S1 Fe2 115.07(9) . . ? Fe1 S1 Fe2 66.85(2) . . ? C7 S2 Fe2 114.02(10) . . ? C7 S2 Fe1 116.55(11) . . ? Fe2 S2 Fe1 67.12(3) . . ? C17 P1 C23 102.05(13) . . ? C17 P1 C16 103.51(13) . . ? C23 P1 C16 102.63(13) . . ? C17 P1 Fe1 120.09(9) . . ? C23 P1 Fe1 113.18(9) . . ? C16 P1 Fe1 113.34(10) . . ? C29 P2 C35 100.72(14) . . ? C29 P2 C16 100.69(15) . . ? C35 P2 C16 103.16(13) . . ? C9 N1 C10 116.4(3) . . ? C8 N2 C15 116.4(3) . . ? O1 C1 Fe1 177.1(3) . . ? O2 C2 Fe1 175.7(3) . . ? O3 C3 Fe2 177.3(3) . . ? O4 C4 Fe2 178.2(4) . . ? O5 C5 Fe2 177.9(3) . . ? C9 C6 S1 112.9(2) . . ? C9 C6 H6B 114(2) . . ? S1 C6 H6B 107(2) . . ? C9 C6 H6A 113(2) . . ? S1 C6 H6A 102(2) . . ? H6B C6 H6A 107(3) . . ? C8 C7 S2 114.3(2) . . ? C8 C7 H7A 112(2) . . ? S2 C7 H7A 102(2) . . ? C8 C7 H7B 109.8(19) . . ? S2 C7 H7B 108(2) . . ? H7A C7 H7B 110(3) . . ? N2 C8 C9 121.6(3) . . ? N2 C8 C7 118.0(3) . . ? C9 C8 C7 120.4(3) . . ? N1 C9 C8 122.7(3) . . ? N1 C9 C6 117.3(3) . . ? C8 C9 C6 119.9(3) . . ? N1 C10 C15 121.2(3) . . ? N1 C10 C11 118.9(3) . . ? C15 C10 C11 119.9(3) . . ? C12 C11 C10 119.5(3) . . ? C12 C11 H11 118(2) . . ? C10 C11 H11 122(2) . . ? C11 C12 C13 120.7(3) . . ? C11 C12 H12 123(3) . . ? C13 C12 H12 116(3) . . ? C14 C13 C12 120.9(3) . . ? C14 C13 H13 124(3) . . ? C12 C13 H13 115(3) . . ? C13 C14 C15 119.9(3) . . ? C13 C14 H14 124(2) . . ? C15 C14 H14 116(2) . . ? N2 C15 C10 121.7(3) . . ? N2 C15 C14 119.2(3) . . ? C10 C15 C14 119.1(3) . . ? P1 C16 P2 111.79(16) . . ? P1 C16 H16B 112.4(16) . . ? P2 C16 H16B 109.9(15) . . ? P1 C16 H16A 104.5(19) . . ? P2 C16 H16A 105.6(19) . . ? H16B C16 H16A 112(2) . . ? C22 C17 C18 118.3(3) . . ? C22 C17 P1 121.8(2) . . ? C18 C17 P1 119.8(2) . . ? C19 C18 C17 120.7(3) . . ? C19 C18 H18 120.9(19) . . ? C17 C18 H18 118.4(19) . . ? C18 C19 C20 120.7(3) . . ? C18 C19 H19 117(3) . . ? C20 C19 H19 122(3) . . ? C19 C20 C21 119.5(3) . . ? C19 C20 H20 120(3) . . ? C21 C20 H20 121(3) . . ? C20 C21 C22 120.3(3) . . ? C20 C21 H21 123(2) . . ? C22 C21 H21 116(2) . . ? C21 C22 C17 120.5(3) . . ? C21 C22 H22 122.4(19) . . ? C17 C22 H22 117.1(19) . . ? C24 C23 C28 118.7(3) . . ? C24 C23 P1 121.4(2) . . ? C28 C23 P1 119.7(2) . . ? C23 C24 C25 119.9(3) . . ? C23 C24 H24 120(2) . . ? C25 C24 H24 120(2) . . ? C26 C25 C24 120.6(3) . . ? C26 C25 H25 122(3) . . ? C24 C25 H25 117(3) . . ? C27 C26 C25 119.5(3) . . ? C27 C26 H26 118(2) . . ? C25 C26 H26 122(2) . . ? C28 C27 C26 120.9(3) . . ? C28 C27 H27 117(3) . . ? C26 C27 H27 122(3) . . ? C27 C28 C23 120.4(3) . . ? C27 C28 H28 121(2) . . ? C23 C28 H28 118(2) . . ? C30 C29 C34 118.9(4) . . ? C30 C29 P2 118.3(3) . . ? C34 C29 P2 122.7(3) . . ? C29 C30 C31 119.7(6) . . ? C29 C30 H30 114(3) . . ? C31 C30 H30 126(3) . . ? C32 C31 C30 120.4(6) . . ? C32 C31 H31 124(4) . . ? C30 C31 H31 115(5) . . ? C31 C32 C33 121.3(5) . . ? C31 C32 H32 129(3) . . ? C33 C32 H32 110(3) . . ? C34 C33 C32 120.2(6) . . ? C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C33 C34 C29 119.5(5) . . ? C33 C34 H34 118(3) . . ? C29 C34 H34 122(3) . . ? C40 C35 C36 118.5(3) . . ? C40 C35 P2 124.2(2) . . ? C36 C35 P2 117.0(2) . . ? C37 C36 C35 120.8(3) . . ? C37 C36 H36 120(2) . . ? C35 C36 H36 119(2) . . ? C36 C37 C38 120.1(4) . . ? C36 C37 H37 118(3) . . ? C38 C37 H37 122(3) . . ? C39 C38 C37 119.4(3) . . ? C39 C38 H38 126(4) . . ? C37 C38 H38 114(4) . . ? C38 C39 C40 120.6(3) . . ? C38 C39 H39 120(2) . . ? C40 C39 H39 120(2) . . ? C35 C40 C39 120.5(3) . . ? C35 C40 H40 118(2) . . ? C39 C40 H40 121(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.678 _refine_diff_density_min -0.856 _refine_diff_density_rms 0.111 _publ_section_references ; Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ; #==END data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 816114' #TrackingRef '- cifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H32 Cl2 Fe2 N2 O4 P2 S2' _chemical_formula_weight 913.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.199(7) _cell_length_b 13.712(9) _cell_length_c 14.582(9) _cell_angle_alpha 92.981(8) _cell_angle_beta 91.827(7) _cell_angle_gamma 100.728(13) _cell_volume 1999(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5133 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 23.99 _exptl_crystal_description Plate _exptl_crystal_colour orange-red _exptl_crystal_size_max .17 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 1.087 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3267 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku Crystalclear)' _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 'Saturn70 (4x4 bin mode)' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11750 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 23.99 _reflns_number_total 6216 _reflns_number_gt 4750 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1178P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6216 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0625 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1704 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.76400(6) 0.75719(4) 0.27630(4) 0.0156(2) Uani 1 1 d . . . Fe2 Fe 0.81913(6) 0.81558(5) 0.44691(4) 0.0208(2) Uani 1 1 d . . . S1 S 0.91756(11) 0.89000(8) 0.32494(8) 0.0202(3) Uani 1 1 d . . . S2 S 0.84968(11) 0.66921(8) 0.37875(8) 0.0204(3) Uani 1 1 d . . . P1 P 0.64057(11) 0.84684(8) 0.20184(7) 0.0163(3) Uani 1 1 d . . . P2 P 0.55867(11) 0.66883(8) 0.26998(8) 0.0166(3) Uani 1 1 d . . . N1 N 1.1488(4) 0.8252(3) 0.1709(3) 0.0279(9) Uani 1 1 d . . . N2 N 1.0884(4) 0.6210(3) 0.2077(3) 0.0294(10) Uani 1 1 d . . . O1 O 0.8226(3) 0.6570(2) 0.1053(2) 0.0293(8) Uani 1 1 d . . . O2 O 0.6418(3) 0.6938(2) 0.5696(2) 0.0314(8) Uani 1 1 d . . . O3 O 0.6767(4) 0.9821(3) 0.4756(2) 0.0368(9) Uani 1 1 d . . . O4 O 1.0497(4) 0.8670(3) 0.5791(3) 0.0493(11) Uani 1 1 d . . . C1 C 0.8025(4) 0.6990(3) 0.1736(3) 0.0199(10) Uani 1 1 d . . . C2 C 0.7090(5) 0.7421(3) 0.5196(3) 0.0257(11) Uani 1 1 d . . . C3 C 0.7318(5) 0.9176(4) 0.4617(3) 0.0265(11) Uani 1 1 d . . . C4 C 0.9588(5) 0.8484(3) 0.5294(3) 0.0290(11) Uani 1 1 d . . . C5 C 1.0928(4) 0.8729(4) 0.3222(3) 0.0270(11) Uani 1 1 d . . . H5A H 1.1496 0.9352 0.3094 0.032 Uiso 1 1 calc R . . H5B H 1.1208 0.8543 0.3820 0.032 Uiso 1 1 calc R . . C6 C 1.1095(4) 0.7957(3) 0.2519(3) 0.0253(11) Uani 1 1 d . . . C7 C 1.1547(5) 0.7520(4) 0.1039(4) 0.0314(12) Uani 1 1 d . . . C8 C 1.1923(5) 0.7798(4) 0.0149(4) 0.0401(13) Uani 1 1 d . . . H8A H 1.2095 0.8466 0.0019 0.048 Uiso 1 1 calc R . . C9 C 1.2031(6) 0.7095(5) -0.0512(4) 0.0469(15) Uani 1 1 d . . . H9A H 1.2292 0.7284 -0.1092 0.056 Uiso 1 1 calc R . . C10 C 1.1755(5) 0.6078(5) -0.0339(4) 0.0444(14) Uani 1 1 d . . . H10A H 1.1829 0.5602 -0.0803 0.053 Uiso 1 1 calc R . . C11 C 1.1378(5) 0.5791(4) 0.0513(4) 0.0365(13) Uani 1 1 d . . . H11A H 1.1192 0.5119 0.0625 0.044 Uiso 1 1 calc R . . C12 C 1.1268(5) 0.6509(4) 0.1229(4) 0.0308(12) Uani 1 1 d . . . C13 C 1.0779(4) 0.6927(3) 0.2711(3) 0.0256(11) Uani 1 1 d . . . C14 C 1.0274(4) 0.6613(4) 0.3619(3) 0.0279(11) Uani 1 1 d . . . H14A H 1.0823 0.7026 0.4100 0.033 Uiso 1 1 calc R . . H14B H 1.0382 0.5932 0.3688 0.033 Uiso 1 1 calc R . . C15 C 0.4880(4) 0.7491(3) 0.1905(3) 0.0204(10) Uani 1 1 d . . . H15A H 0.4701 0.7192 0.1285 0.024 Uiso 1 1 calc R . . H15B H 0.4096 0.7713 0.2133 0.024 Uiso 1 1 calc R . . C16 C 0.6825(4) 0.8796(3) 0.0849(3) 0.0201(10) Uani 1 1 d . . . C17 C 0.8141(5) 0.8897(4) 0.0581(3) 0.0269(11) Uani 1 1 d . . . H17A H 0.8812 0.8792 0.0990 0.032 Uiso 1 1 calc R . . C18 C 0.8434(5) 0.9158(4) -0.0316(3) 0.0365(13) Uani 1 1 d . . . H18A H 0.9312 0.9246 -0.0498 0.044 Uiso 1 1 calc R . . C19 C 0.7436(5) 0.9285(3) -0.0931(3) 0.0319(12) Uani 1 1 d . . . H19A H 0.7640 0.9439 -0.1530 0.038 Uiso 1 1 calc R . . C20 C 0.6117(5) 0.9185(3) -0.0659(3) 0.0288(11) Uani 1 1 d . . . H20A H 0.5442 0.9285 -0.1068 0.035 Uiso 1 1 calc R . . C21 C 0.5832(5) 0.8933(3) 0.0236(3) 0.0230(10) Uani 1 1 d . . . H21A H 0.4956 0.8856 0.0421 0.028 Uiso 1 1 calc R . . C22 C 0.5935(4) 0.9616(3) 0.2467(3) 0.0165(9) Uani 1 1 d . . . C23 C 0.6955(5) 1.0459(3) 0.2528(3) 0.0221(10) Uani 1 1 d . . . H23A H 0.7809 1.0408 0.2352 0.026 Uiso 1 1 calc R . . C24 C 0.6692(5) 1.1374(3) 0.2854(3) 0.0247(10) Uani 1 1 d . . . H24A H 0.7368 1.1935 0.2892 0.030 Uiso 1 1 calc R . . C25 C 0.5410(5) 1.1445(4) 0.3121(3) 0.0255(11) Uani 1 1 d . . . H25A H 0.5228 1.2055 0.3336 0.031 Uiso 1 1 calc R . . C26 C 0.4416(5) 1.0613(3) 0.3067(3) 0.0249(10) Uani 1 1 d . . . H26A H 0.3563 1.0658 0.3251 0.030 Uiso 1 1 calc R . . C27 C 0.4683(5) 0.9713(3) 0.2741(3) 0.0217(10) Uani 1 1 d . . . H27A H 0.4001 0.9156 0.2706 0.026 Uiso 1 1 calc R . . C28 C 0.5265(4) 0.5442(3) 0.2159(3) 0.0214(10) Uani 1 1 d . . . C29 C 0.6055(5) 0.4777(3) 0.2455(3) 0.0288(11) Uani 1 1 d . . . H29A H 0.6738 0.4980 0.2900 0.035 Uiso 1 1 calc R . . C30 C 0.5803(6) 0.3810(4) 0.2073(4) 0.0412(14) Uani 1 1 d . . . H30A H 0.6317 0.3362 0.2271 0.049 Uiso 1 1 calc R . . C31 C 0.4795(6) 0.3500(4) 0.1401(5) 0.0493(16) Uani 1 1 d . . . H31A H 0.4631 0.2847 0.1155 0.059 Uiso 1 1 calc R . . C32 C 0.4049(6) 0.4156(4) 0.1105(4) 0.0472(16) Uani 1 1 d . . . H32A H 0.3389 0.3950 0.0644 0.057 Uiso 1 1 calc R . . C33 C 0.4254(5) 0.5131(4) 0.1479(4) 0.0363(13) Uani 1 1 d . . . H33A H 0.3726 0.5569 0.1279 0.044 Uiso 1 1 calc R . . C34 C 0.4504(4) 0.6590(3) 0.3676(3) 0.0182(9) Uani 1 1 d . . . C35 C 0.4169(4) 0.7461(3) 0.4086(3) 0.0229(10) Uani 1 1 d . . . H35A H 0.4466 0.8068 0.3836 0.027 Uiso 1 1 calc R . . C36 C 0.3413(4) 0.7425(4) 0.4849(3) 0.0262(11) Uani 1 1 d . . . H36A H 0.3192 0.8004 0.5108 0.031 Uiso 1 1 calc R . . C37 C 0.2972(5) 0.6512(4) 0.5238(3) 0.0312(12) Uani 1 1 d . . . H37A H 0.2463 0.6484 0.5758 0.037 Uiso 1 1 calc R . . C38 C 0.3297(5) 0.5659(4) 0.4847(3) 0.0319(12) Uani 1 1 d . . . H38A H 0.3007 0.5055 0.5106 0.038 Uiso 1 1 calc R . . C39 C 0.4053(4) 0.5689(3) 0.4071(3) 0.0243(10) Uani 1 1 d . . . H39A H 0.4260 0.5104 0.3813 0.029 Uiso 1 1 calc R . . C40 C 0.8695(6) 0.6132(5) -0.2728(5) 0.0535(16) Uani 1 1 d . . . H40A H 0.7765 0.6053 -0.2933 0.064 Uiso 1 1 calc R . . H40B H 0.8792 0.5557 -0.2389 0.064 Uiso 1 1 calc R . . Cl1 Cl 0.9104(3) 0.7171(3) -0.2015(2) 0.1521(15) Uani 1 1 d . . . Cl2 Cl 0.9697(2) 0.61656(14) -0.37038(15) 0.0788(6) 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 0.0155(3) 0.0188(3) 0.0126(4) 0.0022(2) 0.0028(3) 0.0032(3) Fe2 0.0237(4) 0.0245(4) 0.0138(4) 0.0017(3) 0.0012(3) 0.0032(3) S1 0.0187(6) 0.0219(6) 0.0191(6) 0.0021(4) 0.0019(5) 0.0013(5) S2 0.0212(6) 0.0224(6) 0.0184(6) 0.0047(4) 0.0011(5) 0.0053(5) P1 0.0180(6) 0.0204(6) 0.0109(6) 0.0023(4) 0.0025(5) 0.0039(5) P2 0.0169(6) 0.0181(6) 0.0138(6) 0.0004(4) 0.0030(5) 0.0009(5) N1 0.0144(19) 0.034(2) 0.036(3) 0.0015(19) 0.0048(18) 0.0041(17) N2 0.016(2) 0.031(2) 0.041(3) 0.0033(19) 0.0014(19) 0.0032(17) O1 0.0263(18) 0.0369(19) 0.026(2) -0.0053(15) 0.0075(15) 0.0091(15) O2 0.0328(19) 0.038(2) 0.026(2) 0.0086(16) 0.0094(16) 0.0083(16) O3 0.052(2) 0.040(2) 0.024(2) 0.0042(16) 0.0141(17) 0.0177(19) O4 0.051(2) 0.052(2) 0.039(2) -0.0009(19) -0.022(2) -0.002(2) C1 0.016(2) 0.022(2) 0.022(3) 0.006(2) 0.0033(19) 0.0033(19) C2 0.029(3) 0.027(2) 0.020(3) 0.000(2) -0.003(2) 0.006(2) C3 0.033(3) 0.034(3) 0.009(2) 0.0046(19) 0.005(2) -0.002(2) C4 0.036(3) 0.023(2) 0.025(3) 0.002(2) 0.001(2) 0.000(2) C5 0.013(2) 0.037(3) 0.028(3) 0.003(2) 0.000(2) -0.002(2) C6 0.013(2) 0.032(3) 0.032(3) 0.005(2) 0.000(2) 0.006(2) C7 0.017(2) 0.041(3) 0.037(3) 0.006(2) 0.008(2) 0.005(2) C8 0.036(3) 0.053(3) 0.033(3) 0.005(3) 0.011(3) 0.010(3) C9 0.042(3) 0.058(4) 0.042(4) 0.004(3) 0.016(3) 0.012(3) C10 0.035(3) 0.056(4) 0.044(4) -0.010(3) 0.008(3) 0.015(3) C11 0.029(3) 0.037(3) 0.045(4) -0.002(2) 0.004(3) 0.013(2) C12 0.018(2) 0.043(3) 0.033(3) 0.003(2) 0.006(2) 0.010(2) C13 0.015(2) 0.030(3) 0.033(3) 0.003(2) -0.002(2) 0.005(2) C14 0.020(2) 0.036(3) 0.031(3) 0.011(2) -0.002(2) 0.015(2) C15 0.020(2) 0.020(2) 0.018(2) -0.0014(18) 0.0030(19) -0.0040(18) C16 0.028(2) 0.017(2) 0.016(2) 0.0021(17) 0.009(2) 0.0055(19) C17 0.028(3) 0.037(3) 0.016(2) 0.005(2) 0.004(2) 0.006(2) C18 0.038(3) 0.045(3) 0.024(3) 0.007(2) 0.014(2) 0.000(3) C19 0.046(3) 0.027(3) 0.020(3) 0.003(2) 0.012(2) -0.001(2) C20 0.045(3) 0.030(3) 0.012(2) 0.0006(19) -0.002(2) 0.011(2) C21 0.028(3) 0.021(2) 0.021(3) 0.0017(18) 0.006(2) 0.009(2) C22 0.020(2) 0.020(2) 0.010(2) 0.0030(17) 0.0009(18) 0.0059(19) C23 0.022(2) 0.025(2) 0.020(2) 0.0032(19) 0.0043(19) 0.007(2) C24 0.029(3) 0.020(2) 0.024(3) -0.0010(19) -0.001(2) 0.002(2) C25 0.033(3) 0.033(3) 0.014(2) -0.0021(19) 0.002(2) 0.016(2) C26 0.027(3) 0.037(3) 0.012(2) 0.0025(19) 0.0068(19) 0.008(2) C27 0.027(2) 0.026(2) 0.011(2) 0.0038(18) 0.0046(19) 0.003(2) C28 0.022(2) 0.020(2) 0.020(3) -0.0015(18) 0.0092(19) -0.0018(19) C29 0.034(3) 0.029(3) 0.022(3) 0.002(2) 0.004(2) 0.001(2) C30 0.051(3) 0.022(3) 0.054(4) 0.004(2) 0.029(3) 0.011(3) C31 0.056(4) 0.020(3) 0.066(4) -0.019(3) 0.026(3) -0.007(3) C32 0.045(3) 0.039(3) 0.050(4) -0.024(3) -0.009(3) -0.002(3) C33 0.030(3) 0.031(3) 0.044(3) -0.012(2) -0.006(2) 0.001(2) C34 0.013(2) 0.028(2) 0.015(2) 0.0023(18) 0.0031(18) 0.0052(18) C35 0.023(2) 0.026(2) 0.020(3) 0.0003(19) 0.000(2) 0.006(2) C36 0.022(2) 0.041(3) 0.018(3) -0.006(2) 0.000(2) 0.013(2) C37 0.021(2) 0.052(3) 0.019(3) 0.004(2) 0.007(2) 0.002(2) C38 0.029(3) 0.041(3) 0.024(3) 0.009(2) 0.007(2) 0.001(2) C39 0.025(2) 0.028(2) 0.018(3) 0.0018(19) 0.006(2) -0.001(2) C40 0.048(4) 0.052(4) 0.063(4) 0.015(3) 0.007(3) 0.012(3) Cl1 0.134(2) 0.162(3) 0.121(2) -0.080(2) 0.037(2) -0.054(2) Cl2 0.0922(14) 0.0592(11) 0.0912(15) 0.0279(10) 0.0470(12) 0.0162(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 1.751(5) . ? Fe1 P2 2.2121(17) . ? Fe1 P1 2.2142(14) . ? Fe1 S2 2.2243(14) . ? Fe1 S1 2.2373(16) . ? Fe1 Fe2 2.5851(17) . ? Fe2 C2 1.780(5) . ? Fe2 C3 1.801(5) . ? Fe2 C4 1.810(5) . ? Fe2 S1 2.2658(16) . ? Fe2 S2 2.2712(18) . ? S1 C5 1.847(5) . ? S2 C14 1.859(5) . ? P1 C22 1.824(4) . ? P1 C16 1.830(5) . ? P1 C15 1.852(4) . ? P1 P2 2.681(2) . ? P2 C28 1.812(5) . ? P2 C34 1.824(5) . ? P2 C15 1.857(4) . ? N1 C6 1.318(6) . ? N1 C7 1.374(7) . ? N2 C13 1.335(6) . ? N2 C12 1.370(7) . ? O1 C1 1.167(5) . ? O2 C2 1.163(6) . ? O3 C3 1.145(6) . ? O4 C4 1.140(6) . ? C5 C6 1.472(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C13 1.434(6) . ? C7 C12 1.407(7) . ? C7 C8 1.416(8) . ? C8 C9 1.350(8) . ? C8 H8A 0.9300 . ? C9 C10 1.408(8) . ? C9 H9A 0.9300 . ? C10 C11 1.368(8) . ? C10 H10A 0.9300 . ? C11 C12 1.419(7) . ? C11 H11A 0.9300 . ? C13 C14 1.491(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C21 1.376(6) . ? C16 C17 1.393(7) . ? C17 C18 1.401(7) . ? C17 H17A 0.9300 . ? C18 C19 1.376(7) . ? C18 H18A 0.9300 . ? C19 C20 1.399(7) . ? C19 H19A 0.9300 . ? C20 C21 1.393(7) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C27 1.378(6) . ? C22 C23 1.401(6) . ? C23 C24 1.394(6) . ? C23 H23A 0.9300 . ? C24 C25 1.396(7) . ? C24 H24A 0.9300 . ? C25 C26 1.375(7) . ? C25 H25A 0.9300 . ? C26 C27 1.377(6) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 C29 1.400(7) . ? C28 C33 1.399(7) . ? C29 C30 1.385(7) . ? C29 H29A 0.9300 . ? C30 C31 1.389(9) . ? C30 H30A 0.9300 . ? C31 C32 1.360(8) . ? C31 H31A 0.9300 . ? C32 C33 1.393(7) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? C34 C39 1.397(6) . ? C34 C35 1.411(6) . ? C35 C36 1.372(7) . ? C35 H35A 0.9300 . ? C36 C37 1.404(7) . ? C36 H36A 0.9300 . ? C37 C38 1.375(7) . ? C37 H37A 0.9300 . ? C38 C39 1.387(7) . ? C38 H38A 0.9300 . ? C39 H39A 0.9300 . ? C40 Cl1 1.698(7) . ? C40 Cl2 1.776(7) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 P2 92.04(14) . . ? C1 Fe1 P1 91.79(14) . . ? P2 Fe1 P1 74.57(6) . . ? C1 Fe1 S2 100.71(14) . . ? P2 Fe1 S2 96.87(6) . . ? P1 Fe1 S2 165.18(5) . . ? C1 Fe1 S1 113.52(15) . . ? P2 Fe1 S1 152.33(5) . . ? P1 Fe1 S1 93.41(6) . . ? S2 Fe1 S1 88.90(6) . . ? C1 Fe1 Fe2 151.01(14) . . ? P2 Fe1 Fe2 106.35(4) . . ? P1 Fe1 Fe2 114.35(5) . . ? S2 Fe1 Fe2 55.75(5) . . ? S1 Fe1 Fe2 55.48(4) . . ? C2 Fe2 C3 91.5(2) . . ? C2 Fe2 C4 96.8(2) . . ? C3 Fe2 C4 103.2(2) . . ? C2 Fe2 S1 164.59(15) . . ? C3 Fe2 S1 88.34(15) . . ? C4 Fe2 S1 98.22(17) . . ? C2 Fe2 S2 86.19(16) . . ? C3 Fe2 S2 153.17(15) . . ? C4 Fe2 S2 103.61(16) . . ? S1 Fe2 S2 87.05(6) . . ? C2 Fe2 Fe1 110.74(15) . . ? C3 Fe2 Fe1 102.64(14) . . ? C4 Fe2 Fe1 141.34(17) . . ? S1 Fe2 Fe1 54.45(5) . . ? S2 Fe2 Fe1 54.05(3) . . ? C5 S1 Fe1 115.51(16) . . ? C5 S1 Fe2 109.73(16) . . ? Fe1 S1 Fe2 70.07(5) . . ? C14 S2 Fe1 114.06(15) . . ? C14 S2 Fe2 114.31(17) . . ? Fe1 S2 Fe2 70.19(5) . . ? C22 P1 C16 100.53(19) . . ? C22 P1 C15 108.0(2) . . ? C16 P1 C15 106.2(2) . . ? C22 P1 Fe1 125.84(14) . . ? C16 P1 Fe1 118.81(15) . . ? C15 P1 Fe1 95.70(15) . . ? C22 P1 P2 123.92(15) . . ? C16 P1 P2 130.43(14) . . ? C15 P1 P2 43.78(13) . . ? Fe1 P1 P2 52.68(5) . . ? C28 P2 C34 103.7(2) . . ? C28 P2 C15 106.9(2) . . ? C34 P2 C15 105.3(2) . . ? C28 P2 Fe1 119.58(15) . . ? C34 P2 Fe1 123.43(14) . . ? C15 P2 Fe1 95.61(14) . . ? C28 P2 P1 131.59(16) . . ? C34 P2 P1 119.42(15) . . ? C15 P2 P1 43.63(13) . . ? Fe1 P2 P1 52.75(4) . . ? C6 N1 C7 116.8(4) . . ? C13 N2 C12 116.6(4) . . ? O1 C1 Fe1 176.8(4) . . ? O2 C2 Fe2 177.0(4) . . ? O3 C3 Fe2 176.7(4) . . ? O4 C4 Fe2 177.2(5) . . ? C6 C5 S1 111.5(3) . . ? C6 C5 H5A 109.3 . . ? S1 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? S1 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? N1 C6 C13 122.3(5) . . ? N1 C6 C5 117.4(4) . . ? C13 C6 C5 120.2(4) . . ? N1 C7 C12 121.1(5) . . ? N1 C7 C8 119.0(5) . . ? C12 C7 C8 119.9(5) . . ? C9 C8 C7 120.0(6) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 121.1(6) . . ? C8 C9 H9A 119.4 . . ? C10 C9 H9A 119.4 . . ? C11 C10 C9 119.9(5) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? C10 C11 C12 120.7(5) . . ? C10 C11 H11A 119.7 . . ? C12 C11 H11A 119.7 . . ? N2 C12 C7 121.6(5) . . ? N2 C12 C11 120.0(5) . . ? C7 C12 C11 118.4(5) . . ? N2 C13 C6 121.4(5) . . ? N2 C13 C14 117.4(4) . . ? C6 C13 C14 121.1(4) . . ? C13 C14 S2 114.6(3) . . ? C13 C14 H14A 108.6 . . ? S2 C14 H14A 108.6 . . ? C13 C14 H14B 108.6 . . ? S2 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? P1 C15 P2 92.6(2) . . ? P1 C15 H15A 113.2 . . ? P2 C15 H15A 113.2 . . ? P1 C15 H15B 113.2 . . ? P2 C15 H15B 113.2 . . ? H15A C15 H15B 110.5 . . ? C21 C16 C17 120.4(4) . . ? C21 C16 P1 119.5(3) . . ? C17 C16 P1 120.1(3) . . ? C16 C17 C18 118.8(4) . . ? C16 C17 H17A 120.6 . . ? C18 C17 H17A 120.6 . . ? C19 C18 C17 120.6(5) . . ? C19 C18 H18A 119.7 . . ? C17 C18 H18A 119.7 . . ? C18 C19 C20 120.4(5) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C21 C20 C19 118.8(4) . . ? C21 C20 H20A 120.6 . . ? C19 C20 H20A 120.6 . . ? C16 C21 C20 121.0(5) . . ? C16 C21 H21A 119.5 . . ? C20 C21 H21A 119.5 . . ? C27 C22 C23 118.6(4) . . ? C27 C22 P1 125.7(3) . . ? C23 C22 P1 115.7(3) . . ? C24 C23 C22 120.1(4) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C23 C24 C25 119.7(4) . . ? C23 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? C26 C25 C24 119.9(4) . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C25 C26 C27 120.0(4) . . ? C25 C26 H26A 120.0 . . ? C27 C26 H26A 120.0 . . ? C26 C27 C22 121.6(4) . . ? C26 C27 H27A 119.2 . . ? C22 C27 H27A 119.2 . . ? C29 C28 C33 119.9(4) . . ? C29 C28 P2 117.8(3) . . ? C33 C28 P2 122.3(4) . . ? C30 C29 C28 119.0(5) . . ? C30 C29 H29A 120.5 . . ? C28 C29 H29A 120.5 . . ? C29 C30 C31 121.1(5) . . ? C29 C30 H30A 119.4 . . ? C31 C30 H30A 119.4 . . ? C32 C31 C30 119.6(5) . . ? C32 C31 H31A 120.2 . . ? C30 C31 H31A 120.2 . . ? C31 C32 C33 121.2(5) . . ? C31 C32 H32A 119.4 . . ? C33 C32 H32A 119.4 . . ? C32 C33 C28 119.1(5) . . ? C32 C33 H33A 120.4 . . ? C28 C33 H33A 120.4 . . ? C39 C34 C35 118.2(4) . . ? C39 C34 P2 122.4(3) . . ? C35 C34 P2 119.3(3) . . ? C36 C35 C34 121.1(4) . . ? C36 C35 H35A 119.5 . . ? C34 C35 H35A 119.5 . . ? C35 C36 C37 119.9(5) . . ? C35 C36 H36A 120.1 . . ? C37 C36 H36A 120.1 . . ? C38 C37 C36 119.6(5) . . ? C38 C37 H37A 120.2 . . ? C36 C37 H37A 120.2 . . ? C37 C38 C39 120.9(5) . . ? C37 C38 H38A 119.6 . . ? C39 C38 H38A 119.6 . . ? C38 C39 C34 120.4(5) . . ? C38 C39 H39A 119.8 . . ? C34 C39 H39A 119.8 . . ? Cl1 C40 Cl2 112.9(4) . . ? Cl1 C40 H40A 109.0 . . ? Cl2 C40 H40A 109.0 . . ? Cl1 C40 H40B 109.0 . . ? Cl2 C40 H40B 109.0 . . ? H40A C40 H40B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 23.99 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.665 _refine_diff_density_min -1.013 _refine_diff_density_rms 0.138 _publ_section_references ; Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ; #==END data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 816115' #TrackingRef '- cifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H34 Cl4 Fe2 N2 O4 P2 S2' _chemical_formula_weight 998.26 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.518(6) _cell_length_b 11.149(6) _cell_length_c 18.267(11) _cell_angle_alpha 86.244(12) _cell_angle_beta 88.721(11) _cell_angle_gamma 87.302(13) _cell_volume 2135(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6060 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 24.00 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max .13 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 1.147 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6078 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku Crystalclear' _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 'Saturn70 (4x4 bin mode)' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 14946 _diffrn_reflns_av_R_equivalents 0.1191 _diffrn_reflns_av_sigmaI/netI 0.1497 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 24.00 _reflns_number_total 6616 _reflns_number_gt 4995 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1123P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6616 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0898 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.2115 _refine_ls_wR_factor_gt 0.1936 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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 0.28402(7) 1.14781(7) -0.24148(4) 0.0161(3) Uani 1 1 d . . . Fe2 Fe 0.10969(7) 1.25475(7) -0.17180(4) 0.0157(3) Uani 1 1 d . . . S1 S 0.17928(13) 1.31971(12) -0.28429(8) 0.0167(3) Uani 1 1 d . . . S2 S 0.09109(13) 1.07391(12) -0.21635(8) 0.0187(4) Uani 1 1 d . . . P1 P 0.44121(13) 1.26719(13) -0.22677(8) 0.0169(4) Uani 1 1 d . . . P2 P 0.23632(13) 1.38829(12) -0.12928(8) 0.0154(4) Uani 1 1 d . . . N1 N 0.1605(5) 1.2031(4) -0.4597(3) 0.0236(12) Uani 1 1 d . . . N2 N 0.0841(5) 0.9765(4) -0.4003(3) 0.0222(11) Uani 1 1 d . . . O1 O 0.3922(4) 1.0257(4) -0.3673(3) 0.0332(11) Uani 1 1 d . . . O2 O 0.3789(4) 0.9825(4) -0.1225(3) 0.0338(11) Uani 1 1 d . . . O3 O -0.1378(4) 1.3828(4) -0.1788(3) 0.0376(12) Uani 1 1 d . . . O4 O 0.0710(4) 1.1252(4) -0.0298(2) 0.0275(10) Uani 1 1 d . . . C1 C 0.3492(5) 1.0738(5) -0.3187(4) 0.0242(14) Uani 1 1 d . . . C2 C 0.3427(6) 1.0468(5) -0.1697(3) 0.0215(13) Uani 1 1 d . . . C3 C -0.0406(6) 1.3320(5) -0.1748(3) 0.0221(13) Uani 1 1 d . . . C4 C 0.0887(6) 1.1792(5) -0.0841(3) 0.0205(13) Uani 1 1 d . . . C5 C 0.0653(6) 1.3011(5) -0.3579(3) 0.0211(13) Uani 1 1 d . . . H5A H -0.0198 1.2974 -0.3366 0.025 Uiso 1 1 calc R . . H5B H 0.0665 1.3709 -0.3925 0.025 Uiso 1 1 calc R . . C6 C 0.0943(5) 1.1920(5) -0.3976(3) 0.0208(13) Uani 1 1 d . . . C7 C 0.1903(5) 1.0998(6) -0.4953(3) 0.0235(14) Uani 1 1 d . . . C8 C 0.2590(6) 1.1085(7) -0.5618(4) 0.0360(16) Uani 1 1 d . . . H8A H 0.2838 1.1829 -0.5817 0.043 Uiso 1 1 calc R . . C9 C 0.2894(6) 1.0057(7) -0.5975(4) 0.0354(17) Uani 1 1 d . . . H9A H 0.3355 1.0101 -0.6415 0.042 Uiso 1 1 calc R . . C10 C 0.2511(6) 0.8956(6) -0.5676(4) 0.0349(18) Uani 1 1 d . . . H10A H 0.2731 0.8267 -0.5920 0.042 Uiso 1 1 calc R . . C11 C 0.1829(6) 0.8848(6) -0.5043(4) 0.0310(16) Uani 1 1 d . . . H11A H 0.1569 0.8098 -0.4862 0.037 Uiso 1 1 calc R . . C12 C 0.1511(6) 0.9886(6) -0.4654(3) 0.0248(14) Uani 1 1 d . . . C13 C 0.0569(5) 1.0769(5) -0.3677(3) 0.0237(14) Uani 1 1 d . . . C14 C -0.0138(6) 1.0676(5) -0.2960(3) 0.0222(13) Uani 1 1 d . . . H14A H -0.0571 0.9925 -0.2918 0.027 Uiso 1 1 calc R . . H14B H -0.0781 1.1328 -0.2950 0.027 Uiso 1 1 calc R . . C15 C 0.3840(5) 1.4066(5) -0.1854(3) 0.0201(13) Uani 1 1 d . . . H15A H 0.3684 1.4689 -0.2242 0.024 Uiso 1 1 calc R . . H15B H 0.4501 1.4330 -0.1548 0.024 Uiso 1 1 calc R . . C16 C 0.5249(5) 1.3288(5) -0.3090(3) 0.0206(13) Uani 1 1 d . . . C17 C 0.4774(6) 1.3230(6) -0.3789(3) 0.0253(14) Uani 1 1 d . . . H17A H 0.4017 1.2852 -0.3848 0.030 Uiso 1 1 calc R . . C18 C 0.5412(6) 1.3729(6) -0.4403(4) 0.0315(16) Uani 1 1 d . . . H18A H 0.5106 1.3653 -0.4871 0.038 Uiso 1 1 calc R . . C19 C 0.6505(7) 1.4338(6) -0.4311(4) 0.0386(18) Uani 1 1 d . . . H19A H 0.6916 1.4708 -0.4715 0.046 Uiso 1 1 calc R . . C20 C 0.6990(7) 1.4396(6) -0.3612(4) 0.0353(16) Uani 1 1 d . . . H20A H 0.7746 1.4777 -0.3554 0.042 Uiso 1 1 calc R . . C21 C 0.6364(6) 1.3900(6) -0.3007(4) 0.0282(14) Uani 1 1 d . . . H21A H 0.6682 1.3968 -0.2541 0.034 Uiso 1 1 calc R . . C22 C 0.5729(6) 1.2045(5) -0.1711(3) 0.0214(13) Uani 1 1 d . . . C23 C 0.6426(6) 1.1057(5) -0.1972(4) 0.0264(14) Uani 1 1 d . . . H23A H 0.6244 1.0788 -0.2428 0.032 Uiso 1 1 calc R . . C24 C 0.7372(6) 1.0484(6) -0.1564(4) 0.0342(16) Uani 1 1 d . . . H24A H 0.7820 0.9826 -0.1747 0.041 Uiso 1 1 calc R . . C25 C 0.7674(6) 1.0849(6) -0.0901(4) 0.0353(17) Uani 1 1 d . . . H25A H 0.8324 1.0453 -0.0631 0.042 Uiso 1 1 calc R . . C26 C 0.6999(6) 1.1821(6) -0.0631(4) 0.0338(16) Uani 1 1 d . . . H26A H 0.7195 1.2077 -0.0174 0.041 Uiso 1 1 calc R . . C27 C 0.6022(6) 1.2426(6) -0.1034(3) 0.0252(14) Uani 1 1 d . . . H27A H 0.5573 1.3080 -0.0847 0.030 Uiso 1 1 calc R . . C28 C 0.2942(5) 1.3607(5) -0.0354(3) 0.0190(13) Uani 1 1 d . . . C29 C 0.3372(5) 1.2445(5) -0.0118(3) 0.0212(13) Uani 1 1 d . . . H29A H 0.3337 1.1829 -0.0435 0.025 Uiso 1 1 calc R . . C30 C 0.3849(6) 1.2191(6) 0.0577(4) 0.0343(16) Uani 1 1 d . . . H30A H 0.4157 1.1419 0.0724 0.041 Uiso 1 1 calc R . . C31 C 0.3860(6) 1.3116(7) 0.1052(4) 0.0369(17) Uani 1 1 d . . . H31A H 0.4164 1.2959 0.1524 0.044 Uiso 1 1 calc R . . C32 C 0.3423(6) 1.4265(6) 0.0827(4) 0.0327(16) Uani 1 1 d . . . H32A H 0.3432 1.4877 0.1149 0.039 Uiso 1 1 calc R . . C33 C 0.2975(6) 1.4507(6) 0.0128(3) 0.0265(14) Uani 1 1 d . . . H33A H 0.2692 1.5286 -0.0022 0.032 Uiso 1 1 calc R . . C34 C 0.1707(6) 1.5427(5) -0.1280(3) 0.0182(12) Uani 1 1 d . . . C35 C 0.2353(6) 1.6412(5) -0.1576(3) 0.0227(13) Uani 1 1 d . . . H35A H 0.3145 1.6303 -0.1805 0.027 Uiso 1 1 calc R . . C36 C 0.1800(6) 1.7555(5) -0.1526(4) 0.0284(15) Uani 1 1 d . . . H36A H 0.2235 1.8213 -0.1721 0.034 Uiso 1 1 calc R . . C37 C 0.0618(6) 1.7751(6) -0.1193(4) 0.0301(15) Uani 1 1 d . . . H37A H 0.0260 1.8526 -0.1164 0.036 Uiso 1 1 calc R . . C38 C -0.0017(6) 1.6760(5) -0.0905(3) 0.0268(14) Uani 1 1 d . . . H38A H -0.0808 1.6867 -0.0674 0.032 Uiso 1 1 calc R . . C39 C 0.0520(5) 1.5613(5) -0.0960(3) 0.0214(13) Uani 1 1 d . . . H39A H 0.0073 1.4955 -0.0778 0.026 Uiso 1 1 calc R . . C40 C 0.6284(10) 0.2440(8) 0.3552(6) 0.070(3) Uani 1 1 d . . . H40A H 0.6011 0.2118 0.4033 0.084 Uiso 1 1 calc R . . H40B H 0.6994 0.1932 0.3389 0.084 Uiso 1 1 calc R . . Cl1 Cl 0.5030(3) 0.2380(3) 0.29417(16) 0.0936(10) Uani 1 1 d . . . Cl2 Cl 0.6788(2) 0.38591(18) 0.36246(11) 0.0570(6) Uani 1 1 d . . . C41 C 0.0093(9) 1.3020(9) -0.6891(5) 0.067(3) Uani 1 1 d . . . H41A H -0.0316 1.2260 -0.6807 0.081 Uiso 1 1 calc R . . H41B H -0.0445 1.3542 -0.7212 0.081 Uiso 1 1 calc R . . Cl3 Cl 0.1566(2) 1.2764(2) -0.73321(13) 0.0694(7) Uani 1 1 d . . . Cl4 Cl 0.0206(2) 1.36738(19) -0.60524(13) 0.0605(6) 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 0.0139(5) 0.0146(4) 0.0197(5) 0.0003(4) -0.0030(3) -0.0003(3) Fe2 0.0147(5) 0.0149(4) 0.0174(5) 0.0012(4) -0.0011(3) -0.0022(3) S1 0.0163(7) 0.0156(7) 0.0181(7) 0.0011(6) -0.0022(6) -0.0006(6) S2 0.0190(8) 0.0166(7) 0.0206(8) 0.0012(6) -0.0026(6) -0.0037(6) P1 0.0145(8) 0.0190(7) 0.0167(8) 0.0023(6) -0.0008(6) -0.0017(6) P2 0.0158(8) 0.0133(7) 0.0170(8) 0.0013(6) -0.0017(6) -0.0022(6) N1 0.020(3) 0.029(3) 0.022(3) -0.005(2) -0.005(2) 0.000(2) N2 0.020(3) 0.024(3) 0.023(3) -0.005(2) -0.005(2) -0.003(2) O1 0.020(2) 0.046(3) 0.034(3) -0.016(2) 0.004(2) 0.003(2) O2 0.028(3) 0.027(2) 0.045(3) 0.013(2) -0.012(2) -0.004(2) O3 0.018(2) 0.043(3) 0.050(3) 0.003(2) -0.007(2) 0.005(2) O4 0.036(3) 0.026(2) 0.021(2) 0.004(2) -0.001(2) -0.007(2) C1 0.012(3) 0.026(3) 0.034(4) 0.006(3) -0.012(3) -0.004(3) C2 0.020(3) 0.019(3) 0.026(3) 0.001(3) -0.005(3) -0.005(3) C3 0.021(3) 0.028(3) 0.018(3) -0.007(3) 0.000(3) -0.003(3) C4 0.023(3) 0.017(3) 0.022(3) -0.004(3) -0.003(3) -0.006(3) C5 0.021(3) 0.027(3) 0.015(3) 0.000(3) -0.009(2) 0.004(3) C6 0.017(3) 0.027(3) 0.019(3) -0.004(3) -0.009(3) 0.000(3) C7 0.016(3) 0.034(4) 0.022(3) -0.011(3) -0.007(3) 0.002(3) C8 0.027(4) 0.051(4) 0.031(4) -0.003(3) -0.002(3) -0.013(3) C9 0.025(4) 0.055(5) 0.028(4) -0.014(4) 0.001(3) 0.001(3) C10 0.028(4) 0.043(4) 0.036(4) -0.029(4) -0.007(3) 0.014(3) C11 0.029(4) 0.031(4) 0.032(4) -0.002(3) -0.012(3) 0.006(3) C12 0.017(3) 0.033(3) 0.025(3) -0.007(3) -0.005(3) 0.002(3) C13 0.016(3) 0.030(3) 0.025(3) 0.001(3) -0.010(3) -0.001(3) C14 0.022(3) 0.024(3) 0.022(3) -0.011(3) -0.002(3) -0.004(3) C15 0.023(3) 0.016(3) 0.021(3) 0.004(2) -0.005(3) -0.004(2) C16 0.019(3) 0.015(3) 0.027(3) -0.001(3) 0.006(3) 0.003(2) C17 0.019(3) 0.032(3) 0.024(3) 0.006(3) -0.004(3) 0.001(3) C18 0.036(4) 0.035(4) 0.022(3) 0.005(3) 0.007(3) 0.009(3) C19 0.033(4) 0.043(4) 0.035(4) 0.025(3) 0.011(3) 0.004(3) C20 0.026(4) 0.040(4) 0.039(4) 0.009(3) 0.005(3) -0.009(3) C21 0.026(4) 0.031(3) 0.027(3) 0.007(3) -0.005(3) -0.005(3) C22 0.019(3) 0.026(3) 0.018(3) 0.008(3) 0.000(2) -0.001(3) C23 0.020(3) 0.030(3) 0.028(3) 0.003(3) 0.003(3) 0.003(3) C24 0.021(3) 0.036(4) 0.042(4) 0.019(3) 0.003(3) 0.004(3) C25 0.018(3) 0.036(4) 0.049(4) 0.024(3) -0.010(3) -0.005(3) C26 0.023(3) 0.046(4) 0.033(4) 0.014(3) -0.013(3) -0.013(3) C27 0.020(3) 0.032(3) 0.023(3) 0.011(3) -0.003(3) -0.005(3) C28 0.017(3) 0.023(3) 0.016(3) 0.009(3) -0.004(2) -0.007(2) C29 0.018(3) 0.025(3) 0.021(3) 0.004(3) -0.001(2) -0.003(3) C30 0.026(4) 0.038(4) 0.037(4) 0.015(3) -0.002(3) -0.003(3) C31 0.024(4) 0.063(5) 0.023(3) 0.013(3) -0.008(3) -0.012(3) C32 0.029(4) 0.043(4) 0.029(4) -0.014(3) 0.002(3) -0.013(3) C33 0.018(3) 0.031(3) 0.031(4) 0.004(3) -0.004(3) -0.015(3) C34 0.030(3) 0.010(3) 0.015(3) 0.000(2) -0.003(2) -0.001(2) C35 0.023(3) 0.021(3) 0.024(3) -0.003(3) 0.003(3) -0.003(3) C36 0.038(4) 0.016(3) 0.031(4) -0.003(3) 0.011(3) -0.003(3) C37 0.036(4) 0.020(3) 0.034(4) 0.001(3) 0.001(3) -0.001(3) C38 0.028(3) 0.025(3) 0.028(3) -0.003(3) 0.003(3) -0.001(3) C39 0.016(3) 0.020(3) 0.028(3) 0.004(3) 0.003(3) -0.007(2) C40 0.084(7) 0.062(6) 0.067(6) -0.006(5) -0.015(5) -0.010(5) Cl1 0.0736(18) 0.120(2) 0.0838(19) 0.0591(17) -0.0419(15) -0.0444(16) Cl2 0.0793(15) 0.0507(12) 0.0403(11) 0.0028(9) -0.0045(10) -0.0007(11) C41 0.055(6) 0.077(6) 0.069(6) 0.003(5) -0.023(5) -0.004(5) Cl3 0.0595(14) 0.0948(18) 0.0535(13) 0.0065(13) -0.0034(11) -0.0140(13) Cl4 0.0621(14) 0.0515(12) 0.0688(15) -0.0021(11) -0.0058(11) -0.0134(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 C2 1.774(6) . ? Fe1 C1 1.787(7) . ? Fe1 P1 2.2025(19) . ? Fe1 S2 2.252(2) . ? Fe1 S1 2.2675(18) . ? Fe1 Fe2 2.5085(14) . ? Fe2 C3 1.764(6) . ? Fe2 C4 1.774(7) . ? Fe2 P2 2.2311(17) . ? Fe2 S2 2.2416(18) . ? Fe2 S1 2.252(2) . ? S1 C5 1.850(5) . ? S2 C14 1.853(6) . ? P1 C22 1.822(6) . ? P1 C16 1.835(6) . ? P1 C15 1.842(6) . ? P2 C34 1.825(5) . ? P2 C28 1.835(6) . ? P2 C15 1.854(6) . ? N1 C6 1.320(8) . ? N1 C7 1.379(7) . ? N2 C13 1.319(7) . ? N2 C12 1.371(8) . ? O1 C1 1.143(7) . ? O2 C2 1.145(7) . ? O3 C3 1.146(7) . ? O4 C4 1.144(7) . ? C5 C6 1.472(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C13 1.429(9) . ? C7 C12 1.399(9) . ? C7 C8 1.400(9) . ? C8 C9 1.377(9) . ? C8 H8A 0.9300 . ? C9 C10 1.384(11) . ? C9 H9A 0.9300 . ? C10 C11 1.348(10) . ? C10 H10A 0.9300 . ? C11 C12 1.420(8) . ? C11 H11A 0.9300 . ? C13 C14 1.492(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.387(8) . ? C16 C21 1.401(9) . ? C17 C18 1.392(9) . ? C17 H17A 0.9300 . ? C18 C19 1.381(10) . ? C18 H18A 0.9300 . ? C19 C20 1.392(10) . ? C19 H19A 0.9300 . ? C20 C21 1.371(10) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C27 1.379(8) . ? C22 C23 1.398(8) . ? C23 C24 1.365(9) . ? C23 H23A 0.9300 . ? C24 C25 1.353(10) . ? C24 H24A 0.9300 . ? C25 C26 1.379(10) . ? C25 H25A 0.9300 . ? C26 C27 1.399(9) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 C33 1.379(8) . ? C28 C29 1.396(8) . ? C29 C30 1.383(9) . ? C29 H29A 0.9300 . ? C30 C31 1.390(10) . ? C30 H30A 0.9300 . ? C31 C32 1.379(10) . ? C31 H31A 0.9300 . ? C32 C33 1.377(9) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? C34 C39 1.380(8) . ? C34 C35 1.391(8) . ? C35 C36 1.384(8) . ? C35 H35A 0.9300 . ? C36 C37 1.386(9) . ? C36 H36A 0.9300 . ? C37 C38 1.386(9) . ? C37 H37A 0.9300 . ? C38 C39 1.382(8) . ? C38 H38A 0.9300 . ? C39 H39A 0.9300 . ? C40 Cl2 1.706(10) . ? C40 Cl1 1.751(10) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 Cl3 1.751(10) . ? C41 Cl4 1.747(9) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 C1 99.5(3) . . ? C2 Fe1 P1 90.40(19) . . ? C1 Fe1 P1 98.03(19) . . ? C2 Fe1 S2 87.1(2) . . ? C1 Fe1 S2 107.10(19) . . ? P1 Fe1 S2 154.81(6) . . ? C2 Fe1 S1 152.58(19) . . ? C1 Fe1 S1 107.8(2) . . ? P1 Fe1 S1 83.91(7) . . ? S2 Fe1 S1 86.84(7) . . ? C2 Fe1 Fe2 99.06(19) . . ? C1 Fe1 Fe2 153.93(17) . . ? P1 Fe1 Fe2 99.97(6) . . ? S2 Fe1 Fe2 55.86(5) . . ? S1 Fe1 Fe2 55.99(5) . . ? C3 Fe2 C4 96.8(3) . . ? C3 Fe2 P2 103.39(19) . . ? C4 Fe2 P2 93.12(18) . . ? C3 Fe2 S2 108.45(19) . . ? C4 Fe2 S2 85.72(18) . . ? P2 Fe2 S2 148.06(6) . . ? C3 Fe2 S1 97.1(2) . . ? C4 Fe2 S1 165.8(2) . . ? P2 Fe2 S1 86.10(7) . . ? S2 Fe2 S1 87.49(6) . . ? C3 Fe2 Fe1 147.15(19) . . ? C4 Fe2 Fe1 109.46(19) . . ? P2 Fe2 Fe1 94.70(6) . . ? S2 Fe2 Fe1 56.28(5) . . ? S1 Fe2 Fe1 56.58(5) . . ? C5 S1 Fe2 113.9(2) . . ? C5 S1 Fe1 115.00(19) . . ? Fe2 S1 Fe1 67.43(5) . . ? C14 S2 Fe2 116.74(19) . . ? C14 S2 Fe1 115.7(2) . . ? Fe2 S2 Fe1 67.86(5) . . ? C22 P1 C16 101.8(3) . . ? C22 P1 C15 106.5(3) . . ? C16 P1 C15 100.8(3) . . ? C22 P1 Fe1 116.5(2) . . ? C16 P1 Fe1 118.1(2) . . ? C15 P1 Fe1 111.4(2) . . ? C34 P2 C28 101.8(3) . . ? C34 P2 C15 102.3(3) . . ? C28 P2 C15 103.7(3) . . ? C34 P2 Fe2 116.23(19) . . ? C28 P2 Fe2 117.99(19) . . ? C15 P2 Fe2 112.82(18) . . ? C6 N1 C7 117.5(5) . . ? C13 N2 C12 115.8(5) . . ? O1 C1 Fe1 178.9(5) . . ? O2 C2 Fe1 178.7(5) . . ? O3 C3 Fe2 178.1(6) . . ? O4 C4 Fe2 175.6(5) . . ? C6 C5 S1 112.8(4) . . ? C6 C5 H5A 109.0 . . ? S1 C5 H5A 109.0 . . ? C6 C5 H5B 109.0 . . ? S1 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N1 C6 C13 121.2(5) . . ? N1 C6 C5 118.0(6) . . ? C13 C6 C5 120.7(6) . . ? N1 C7 C12 120.1(6) . . ? N1 C7 C8 119.0(6) . . ? C12 C7 C8 120.9(6) . . ? C9 C8 C7 119.2(7) . . ? C9 C8 H8A 120.4 . . ? C7 C8 H8A 120.4 . . ? C8 C9 C10 119.8(6) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? C11 C10 C9 122.2(6) . . ? C11 C10 H10A 118.9 . . ? C9 C10 H10A 118.9 . . ? C10 C11 C12 119.7(7) . . ? C10 C11 H11A 120.1 . . ? C12 C11 H11A 120.1 . . ? N2 C12 C7 122.5(5) . . ? N2 C12 C11 119.3(6) . . ? C7 C12 C11 118.1(6) . . ? N2 C13 C6 122.8(6) . . ? N2 C13 C14 117.6(6) . . ? C6 C13 C14 119.6(5) . . ? C13 C14 S2 112.8(4) . . ? C13 C14 H14A 109.0 . . ? S2 C14 H14A 109.0 . . ? C13 C14 H14B 109.0 . . ? S2 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? P1 C15 P2 113.1(3) . . ? P1 C15 H15A 109.0 . . ? P2 C15 H15A 109.0 . . ? P1 C15 H15B 109.0 . . ? P2 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C17 C16 C21 118.8(6) . . ? C17 C16 P1 122.2(5) . . ? C21 C16 P1 118.9(5) . . ? C16 C17 C18 121.1(6) . . ? C16 C17 H17A 119.5 . . ? C18 C17 H17A 119.5 . . ? C19 C18 C17 119.3(6) . . ? C19 C18 H18A 120.4 . . ? C17 C18 H18A 120.4 . . ? C18 C19 C20 119.9(6) . . ? C18 C19 H19A 120.1 . . ? C20 C19 H19A 120.1 . . ? C21 C20 C19 120.7(7) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C20 C21 C16 120.1(6) . . ? C20 C21 H21A 120.0 . . ? C16 C21 H21A 120.0 . . ? C27 C22 C23 118.5(6) . . ? C27 C22 P1 124.4(5) . . ? C23 C22 P1 116.9(4) . . ? C24 C23 C22 120.6(6) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C25 C24 C23 121.7(6) . . ? C25 C24 H24A 119.2 . . ? C23 C24 H24A 119.2 . . ? C24 C25 C26 118.8(6) . . ? C24 C25 H25A 120.6 . . ? C26 C25 H25A 120.6 . . ? C25 C26 C27 121.0(6) . . ? C25 C26 H26A 119.5 . . ? C27 C26 H26A 119.5 . . ? C22 C27 C26 119.5(6) . . ? C22 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C33 C28 C29 118.6(5) . . ? C33 C28 P2 122.4(4) . . ? C29 C28 P2 118.9(4) . . ? C30 C29 C28 121.4(6) . . ? C30 C29 H29A 119.3 . . ? C28 C29 H29A 119.3 . . ? C29 C30 C31 118.5(6) . . ? C29 C30 H30A 120.7 . . ? C31 C30 H30A 120.7 . . ? C32 C31 C30 120.5(6) . . ? C32 C31 H31A 119.7 . . ? C30 C31 H31A 119.7 . . ? C31 C32 C33 120.2(6) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C28 C33 C32 120.7(6) . . ? C28 C33 H33A 119.7 . . ? C32 C33 H33A 119.7 . . ? C39 C34 C35 119.2(5) . . ? C39 C34 P2 118.0(4) . . ? C35 C34 P2 122.9(4) . . ? C36 C35 C34 119.1(6) . . ? C36 C35 H35A 120.5 . . ? C34 C35 H35A 120.5 . . ? C35 C36 C37 122.1(6) . . ? C35 C36 H36A 118.9 . . ? C37 C36 H36A 118.9 . . ? C38 C37 C36 118.1(6) . . ? C38 C37 H37A 120.9 . . ? C36 C37 H37A 120.9 . . ? C37 C38 C39 120.2(6) . . ? C37 C38 H38A 119.9 . . ? C39 C38 H38A 119.9 . . ? C34 C39 C38 121.3(6) . . ? C34 C39 H39A 119.4 . . ? C38 C39 H39A 119.4 . . ? Cl2 C40 Cl1 113.4(6) . . ? Cl2 C40 H40A 108.9 . . ? Cl1 C40 H40A 108.9 . . ? Cl2 C40 H40B 108.9 . . ? Cl1 C40 H40B 108.9 . . ? H40A C40 H40B 107.7 . . ? Cl3 C41 Cl4 113.5(5) . . ? Cl3 C41 H41A 108.9 . . ? Cl4 C41 H41A 108.9 . . ? Cl3 C41 H41B 108.9 . . ? Cl4 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.272 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.181 _publ_section_references ; Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ; #==END data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 816116' #TrackingRef '- cifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H23 Fe2 N2 O5 P S2' _chemical_formula_weight 590.20 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 6.934(4) _cell_length_b 12.827(7) _cell_length_c 13.646(7) _cell_angle_alpha 87.864(11) _cell_angle_beta 86.760(12) _cell_angle_gamma 81.660(12) _cell_volume 1198.5(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3055 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max .16 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 1.487 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6104 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku Crystalclear)' _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 'Saturn70 (4x4 bin mode)' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 9427 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5387 _reflns_number_gt 4052 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+3.3872P] 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 5387 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0616 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1575 _refine_ls_wR_factor_gt 0.1327 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 0.08605(9) 0.73373(5) 0.70201(4) 0.01393(17) Uani 1 1 d . . . Fe2 Fe 0.22621(9) 0.58827(5) 0.82186(5) 0.01582(17) Uani 1 1 d . . . S1 S -0.08721(16) 0.67006(8) 0.83064(8) 0.0160(2) Uani 1 1 d . . . S2 S 0.31861(15) 0.75011(8) 0.80580(8) 0.0147(2) Uani 1 1 d . . . P P 0.29064(17) 0.76247(9) 0.57377(8) 0.0165(2) Uani 1 1 d . . . N1 N -0.3010(6) 0.9302(3) 0.9011(3) 0.0173(8) Uani 1 1 d . . . N2 N 0.0661(5) 1.0052(3) 0.8725(3) 0.0159(7) Uani 1 1 d . . . O1 O -0.1346(5) 0.9421(3) 0.6635(3) 0.0261(8) Uani 1 1 d . . . O2 O -0.0886(6) 0.5912(3) 0.5824(3) 0.0318(8) Uani 1 1 d . . . O3 O 0.6159(5) 0.5056(3) 0.7391(3) 0.0263(8) Uani 1 1 d . . . O4 O 0.0755(6) 0.3990(3) 0.7633(3) 0.0379(10) Uani 1 1 d . . . O5 O 0.2724(7) 0.5392(4) 1.0324(3) 0.0444(11) Uani 1 1 d . . . C1 C -0.0477(7) 0.8595(4) 0.6799(3) 0.0197(9) Uani 1 1 d . . . C2 C -0.0221(7) 0.6485(4) 0.6284(3) 0.0209(9) Uani 1 1 d . . . C3 C 0.4651(7) 0.5384(3) 0.7713(3) 0.0194(9) Uani 1 1 d . . . C4 C 0.1316(7) 0.4732(3) 0.7860(4) 0.0219(10) Uani 1 1 d . . . C5 C 0.2577(8) 0.5566(4) 0.9501(4) 0.0265(11) Uani 1 1 d . . . C6 C -0.1411(7) 0.7553(3) 0.9378(3) 0.0191(9) Uani 1 1 d . . . H6A H -0.2702 0.7481 0.9660 0.023 Uiso 1 1 calc R . . H6B H -0.0478 0.7320 0.9872 0.023 Uiso 1 1 calc R . . C7 C -0.1325(7) 0.8689(3) 0.9116(3) 0.0177(9) Uani 1 1 d . . . C8 C -0.2885(7) 1.0340(3) 0.8736(3) 0.0174(9) Uani 1 1 d . . . C9 C -0.4632(7) 1.1039(4) 0.8604(3) 0.0216(10) Uani 1 1 d . . . H9A H -0.5837 1.0803 0.8699 0.026 Uiso 1 1 calc R . . C10 C -0.4524(7) 1.2072(4) 0.8334(4) 0.0250(10) Uani 1 1 d . . . H10A H -0.5667 1.2535 0.8246 0.030 Uiso 1 1 calc R . . C11 C -0.2717(8) 1.2439(4) 0.8187(3) 0.0239(10) Uani 1 1 d . . . H11A H -0.2680 1.3141 0.8002 0.029 Uiso 1 1 calc R . . C12 C -0.1005(7) 1.1777(4) 0.8314(3) 0.0209(9) Uani 1 1 d . . . H12A H 0.0184 1.2030 0.8214 0.025 Uiso 1 1 calc R . . C13 C -0.1056(7) 1.0711(3) 0.8595(3) 0.0172(9) Uani 1 1 d . . . C14 C 0.0525(7) 0.9061(3) 0.8977(3) 0.0166(9) Uani 1 1 d . . . C15 C 0.2387(7) 0.8339(3) 0.9116(3) 0.0176(9) Uani 1 1 d . . . H15A H 0.2222 0.7890 0.9693 0.021 Uiso 1 1 calc R . . H15B H 0.3403 0.8757 0.9236 0.021 Uiso 1 1 calc R . . C16 C 0.4788(7) 0.8438(4) 0.5958(4) 0.0232(10) Uani 1 1 d . . . H16A H 0.5642 0.8078 0.6441 0.028 Uiso 1 1 calc R . . H16B H 0.5568 0.8510 0.5353 0.028 Uiso 1 1 calc R . . C17 C 0.3973(8) 0.9548(4) 0.6323(4) 0.0278(11) Uani 1 1 d . . . H17A H 0.5035 0.9930 0.6422 0.042 Uiso 1 1 calc R . . H17B H 0.3227 0.9486 0.6931 0.042 Uiso 1 1 calc R . . H17C H 0.3151 0.9918 0.5842 0.042 Uiso 1 1 calc R . . C18 C 0.1747(7) 0.8351(4) 0.4689(3) 0.0225(10) Uani 1 1 d . . . H18A H 0.1250 0.9062 0.4888 0.027 Uiso 1 1 calc R . . H18B H 0.2740 0.8403 0.4167 0.027 Uiso 1 1 calc R . . C19 C 0.0095(8) 0.7880(5) 0.4279(4) 0.0304(12) Uani 1 1 d . . . H19A H -0.0413 0.8314 0.3737 0.046 Uiso 1 1 calc R . . H19B H -0.0921 0.7845 0.4782 0.046 Uiso 1 1 calc R . . H19C H 0.0572 0.7184 0.4058 0.046 Uiso 1 1 calc R . . C20 C 0.4273(7) 0.6434(4) 0.5196(3) 0.0214(9) Uani 1 1 d . . . H20A H 0.5161 0.6097 0.5675 0.026 Uiso 1 1 calc R . . H20B H 0.3354 0.5953 0.5088 0.026 Uiso 1 1 calc R . . C21 C 0.5454(8) 0.6570(4) 0.4232(4) 0.0287(11) Uani 1 1 d . . . H21A H 0.6101 0.5895 0.4026 0.043 Uiso 1 1 calc R . . H21B H 0.6409 0.7024 0.4327 0.043 Uiso 1 1 calc R . . H21C H 0.4596 0.6876 0.3738 0.043 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 0.0155(3) 0.0113(3) 0.0149(3) 0.0010(2) -0.0027(2) -0.0015(2) Fe2 0.0188(3) 0.0103(3) 0.0179(3) 0.0013(2) -0.0020(2) -0.0005(2) S1 0.0169(5) 0.0118(5) 0.0197(5) -0.0004(4) -0.0007(4) -0.0034(4) S2 0.0150(5) 0.0122(5) 0.0167(5) 0.0000(4) -0.0030(4) -0.0008(4) P 0.0183(6) 0.0142(5) 0.0167(5) 0.0020(4) -0.0010(4) -0.0018(4) N1 0.0193(19) 0.0136(17) 0.0190(18) -0.0019(14) -0.0005(15) -0.0020(14) N2 0.0178(19) 0.0149(17) 0.0161(17) -0.0033(14) -0.0022(14) -0.0042(14) O1 0.032(2) 0.0141(16) 0.0304(18) 0.0045(14) -0.0061(15) 0.0046(14) O2 0.042(2) 0.031(2) 0.0263(18) -0.0050(15) -0.0073(16) -0.0153(17) O3 0.0240(19) 0.0223(17) 0.0305(18) -0.0007(14) 0.0004(15) 0.0027(14) O4 0.036(2) 0.0165(18) 0.062(3) -0.0082(17) -0.001(2) -0.0071(16) O5 0.054(3) 0.053(3) 0.0223(19) 0.0133(18) -0.0034(19) 0.002(2) C1 0.020(2) 0.022(2) 0.019(2) -0.0009(18) -0.0055(18) -0.0067(18) C2 0.020(2) 0.021(2) 0.021(2) 0.0050(18) -0.0013(18) -0.0032(18) C3 0.026(3) 0.012(2) 0.019(2) 0.0019(16) -0.0056(19) 0.0019(18) C4 0.021(2) 0.013(2) 0.031(2) 0.0020(18) 0.0005(19) -0.0012(18) C5 0.028(3) 0.021(2) 0.028(3) 0.0056(19) -0.002(2) 0.004(2) C6 0.021(2) 0.016(2) 0.020(2) 0.0006(17) 0.0025(18) -0.0043(17) C7 0.022(2) 0.015(2) 0.016(2) -0.0025(16) -0.0016(17) -0.0026(17) C8 0.021(2) 0.012(2) 0.019(2) -0.0021(16) -0.0026(18) -0.0019(17) C9 0.018(2) 0.023(2) 0.024(2) -0.0006(18) -0.0011(18) -0.0022(18) C10 0.025(3) 0.022(2) 0.025(2) 0.0010(19) -0.004(2) 0.0075(19) C11 0.035(3) 0.014(2) 0.021(2) 0.0023(17) 0.000(2) -0.0004(19) C12 0.024(2) 0.018(2) 0.021(2) 0.0025(17) -0.0015(19) -0.0046(18) C13 0.022(2) 0.013(2) 0.017(2) -0.0009(16) -0.0009(17) -0.0017(17) C14 0.022(2) 0.014(2) 0.0139(19) -0.0019(16) -0.0037(17) -0.0005(17) C15 0.018(2) 0.015(2) 0.020(2) -0.0027(17) -0.0039(17) -0.0012(17) C16 0.022(2) 0.022(2) 0.026(2) 0.0021(19) -0.001(2) -0.0051(19) C17 0.031(3) 0.019(2) 0.035(3) -0.004(2) -0.001(2) -0.009(2) C18 0.026(2) 0.020(2) 0.020(2) 0.0073(18) 0.0015(19) -0.0002(19) C19 0.027(3) 0.041(3) 0.023(2) 0.005(2) -0.008(2) -0.005(2) C20 0.024(2) 0.017(2) 0.023(2) 0.0002(17) -0.0025(19) -0.0010(18) C21 0.032(3) 0.033(3) 0.020(2) -0.005(2) 0.005(2) -0.003(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 1.765(5) . ? Fe1 C2 1.781(5) . ? Fe1 S2 2.2426(14) . ? Fe1 P 2.2436(16) . ? Fe1 S1 2.2652(15) . ? Fe1 Fe2 2.5547(12) . ? Fe2 C4 1.795(5) . ? Fe2 C3 1.796(5) . ? Fe2 C5 1.800(5) . ? Fe2 S2 2.2591(16) . ? Fe2 S1 2.2709(16) . ? S1 C6 1.848(5) . ? S2 C15 1.843(4) . ? P C16 1.828(5) . ? P C20 1.834(5) . ? P C18 1.837(5) . ? N1 C7 1.322(6) . ? N1 C8 1.384(6) . ? N2 C14 1.319(6) . ? N2 C13 1.373(6) . ? O1 C1 1.161(6) . ? O2 C2 1.145(6) . ? O3 C3 1.139(6) . ? O4 C4 1.139(6) . ? O5 C5 1.144(6) . ? C6 C7 1.496(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C14 1.433(7) . ? C8 C9 1.415(6) . ? C8 C13 1.418(6) . ? C9 C10 1.373(7) . ? C9 H9A 0.9300 . ? C10 C11 1.403(7) . ? C10 H10A 0.9300 . ? C11 C12 1.371(7) . ? C11 H11A 0.9300 . ? C12 C13 1.411(6) . ? C12 H12A 0.9300 . ? C14 C15 1.493(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.543(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.513(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.527(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? 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 104.3(2) . . ? C1 Fe1 S2 108.49(15) . . ? C2 Fe1 S2 147.21(15) . . ? C1 Fe1 P 89.31(16) . . ? C2 Fe1 P 88.90(16) . . ? S2 Fe1 P 90.28(6) . . ? C1 Fe1 S1 102.44(16) . . ? C2 Fe1 S1 86.27(16) . . ? S2 Fe1 S1 87.92(6) . . ? P Fe1 S1 168.08(5) . . ? C1 Fe1 Fe2 150.12(15) . . ? C2 Fe1 Fe2 95.10(15) . . ? S2 Fe1 Fe2 55.73(4) . . ? P Fe1 Fe2 113.92(5) . . ? S1 Fe1 Fe2 55.83(4) . . ? C4 Fe2 C3 91.2(2) . . ? C4 Fe2 C5 100.1(2) . . ? C3 Fe2 C5 100.3(2) . . ? C4 Fe2 S2 157.59(16) . . ? C3 Fe2 S2 86.75(15) . . ? C5 Fe2 S2 102.20(17) . . ? C4 Fe2 S1 86.99(16) . . ? C3 Fe2 S1 160.07(15) . . ? C5 Fe2 S1 99.52(17) . . ? S2 Fe2 S1 87.39(5) . . ? C4 Fe2 Fe1 104.44(16) . . ? C3 Fe2 Fe1 105.95(14) . . ? C5 Fe2 Fe1 143.27(16) . . ? S2 Fe2 Fe1 55.12(4) . . ? S1 Fe2 Fe1 55.62(4) . . ? C6 S1 Fe1 116.49(15) . . ? C6 S1 Fe2 112.61(16) . . ? Fe1 S1 Fe2 68.56(5) . . ? C15 S2 Fe1 115.30(15) . . ? C15 S2 Fe2 113.40(16) . . ? Fe1 S2 Fe2 69.15(4) . . ? C16 P C20 104.0(2) . . ? C16 P C18 100.6(2) . . ? C20 P C18 103.9(2) . . ? C16 P Fe1 116.43(17) . . ? C20 P Fe1 115.14(16) . . ? C18 P Fe1 114.97(17) . . ? C7 N1 C8 115.6(4) . . ? C14 N2 C13 116.9(4) . . ? O1 C1 Fe1 178.7(4) . . ? O2 C2 Fe1 178.0(4) . . ? O3 C3 Fe2 179.2(4) . . ? O4 C4 Fe2 178.5(4) . . ? O5 C5 Fe2 177.6(5) . . ? C7 C6 S1 112.5(3) . . ? C7 C6 H6A 109.1 . . ? S1 C6 H6A 109.1 . . ? C7 C6 H6B 109.1 . . ? S1 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? N1 C7 C14 123.2(4) . . ? N1 C7 C6 116.8(4) . . ? C14 C7 C6 120.0(4) . . ? N1 C8 C9 118.6(4) . . ? N1 C8 C13 121.4(4) . . ? C9 C8 C13 120.0(4) . . ? C10 C9 C8 119.0(5) . . ? C10 C9 H9A 120.5 . . ? C8 C9 H9A 120.5 . . ? C9 C10 C11 121.1(4) . . ? C9 C10 H10A 119.5 . . ? C11 C10 H10A 119.5 . . ? C12 C11 C10 120.9(4) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C13 119.7(5) . . ? C11 C12 H12A 120.2 . . ? C13 C12 H12A 120.2 . . ? N2 C13 C12 119.6(4) . . ? N2 C13 C8 121.2(4) . . ? C12 C13 C8 119.3(4) . . ? N2 C14 C7 121.7(4) . . ? N2 C14 C15 117.1(4) . . ? C7 C14 C15 121.1(4) . . ? C14 C15 S2 113.7(3) . . ? C14 C15 H15A 108.8 . . ? S2 C15 H15A 108.8 . . ? C14 C15 H15B 108.8 . . ? S2 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C17 C16 P 113.9(4) . . ? C17 C16 H16A 108.8 . . ? P C16 H16A 108.8 . . ? C17 C16 H16B 108.8 . . ? P C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 P 115.7(3) . . ? C19 C18 H18A 108.4 . . ? P C18 H18A 108.4 . . ? C19 C18 H18B 108.4 . . ? P C18 H18B 108.4 . . ? H18A C18 H18B 107.4 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 P 117.4(3) . . ? C21 C20 H20A 107.9 . . ? P C20 H20A 107.9 . . ? C21 C20 H20B 107.9 . . ? P C20 H20B 107.9 . . ? H20A C20 H20B 107.2 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.707 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.183 _publ_section_references ; Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ; #==END data_compound_7 _database_code_depnum_ccdc_archive 'CCDC 816117' #TrackingRef '- cifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H23 Cl0 Fe2 N2 O5 P S2' _chemical_formula_weight 734.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3335(0) _cell_length_b 12.7331(1) _cell_length_c 14.2960(2) _cell_angle_alpha 93.811(11) _cell_angle_beta 105.134(7) _cell_angle_gamma 109.359(7) _cell_volume 1525.35(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3715 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour orange-red _exptl_crystal_size_max .25 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 1.187 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6916 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku Crystalclear)' _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 'Saturn70 (4x4 bin mode)' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11926 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6846 _reflns_number_gt 5540 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+0.1767P] 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 6846 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0495 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.63875(4) 0.66800(3) 0.30716(2) 0.01494(10) Uani 1 1 d . . . Fe2 Fe 0.67585(4) 0.48164(3) 0.31499(3) 0.01571(10) Uani 1 1 d . . . S1 S 0.47879(7) 0.51983(5) 0.35807(4) 0.01611(13) Uani 1 1 d . . . S2 S 0.59350(7) 0.54367(5) 0.17146(4) 0.01597(13) Uani 1 1 d . . . P P 0.50539(8) 0.78281(5) 0.26029(5) 0.01507(14) Uani 1 1 d . . . N1 N 0.2050(3) 0.23658(18) 0.22952(15) 0.0187(4) Uani 1 1 d . . . N2 N 0.3084(3) 0.26685(17) 0.05990(15) 0.0180(4) Uani 1 1 d . . . O1 O 0.9310(2) 0.78759(18) 0.26028(17) 0.0339(5) Uani 1 1 d . . . O2 O 0.7743(3) 0.78550(19) 0.51036(15) 0.0393(5) Uani 1 1 d . . . O3 O 0.9704(2) 0.51552(19) 0.26432(15) 0.0331(5) Uani 1 1 d . . . O4 O 0.8567(3) 0.5348(2) 0.52418(14) 0.0340(5) Uani 1 1 d . . . O5 O 0.5551(3) 0.23270(16) 0.29399(17) 0.0343(5) Uani 1 1 d . . . C1 C 0.8157(3) 0.7439(2) 0.27928(19) 0.0213(5) Uani 1 1 d . . . C2 C 0.7190(3) 0.7384(2) 0.4308(2) 0.0239(6) Uani 1 1 d . . . C3 C 0.8558(3) 0.5019(2) 0.28433(19) 0.0229(5) Uani 1 1 d . . . C4 C 0.7833(3) 0.5122(2) 0.4428(2) 0.0222(5) Uani 1 1 d . . . C5 C 0.5987(3) 0.3288(2) 0.2985(2) 0.0232(6) Uani 1 1 d . . . C6 C 0.2774(3) 0.4373(2) 0.27441(19) 0.0193(5) Uani 1 1 d . . . H6A H 0.2063 0.4111 0.3138 0.023 Uiso 1 1 calc R . . H6B H 0.2399 0.4871 0.2346 0.023 Uiso 1 1 calc R . . C7 C 0.2654(3) 0.3370(2) 0.20706(18) 0.0160(5) Uani 1 1 d . . . C8 C 0.1951(3) 0.1457(2) 0.16722(18) 0.0178(5) Uani 1 1 d . . . C9 C 0.1322(3) 0.0358(2) 0.1869(2) 0.0220(5) Uani 1 1 d . . . H9A H 0.0987 0.0249 0.2425 0.026 Uiso 1 1 calc R . . C10 C 0.1200(3) -0.0550(2) 0.1247(2) 0.0251(6) Uani 1 1 d . . . H10A H 0.0789 -0.1273 0.1387 0.030 Uiso 1 1 calc R . . C11 C 0.1692(3) -0.0404(2) 0.0394(2) 0.0228(5) Uani 1 1 d . . . H11A H 0.1591 -0.1031 -0.0026 0.027 Uiso 1 1 calc R . . C12 C 0.2317(3) 0.0660(2) 0.01820(19) 0.0206(5) Uani 1 1 d . . . H12A H 0.2642 0.0754 -0.0379 0.025 Uiso 1 1 calc R . . C13 C 0.2464(3) 0.1614(2) 0.08232(18) 0.0165(5) Uani 1 1 d . . . C14 C 0.3175(3) 0.3521(2) 0.12136(18) 0.0168(5) Uani 1 1 d . . . C15 C 0.3833(3) 0.4680(2) 0.09891(18) 0.0183(5) Uani 1 1 d . . . H15A H 0.3203 0.5110 0.1124 0.022 Uiso 1 1 calc R . . H15B H 0.3746 0.4629 0.0295 0.022 Uiso 1 1 calc R . . C16 C 0.6246(3) 0.9217(2) 0.24103(19) 0.0181(5) Uani 1 1 d . . . C17 C 0.5636(3) 0.9739(2) 0.16504(19) 0.0202(5) Uani 1 1 d . . . H17A H 0.4622 0.9362 0.1215 0.024 Uiso 1 1 calc R . . C18 C 0.6531(3) 1.0811(2) 0.1544(2) 0.0230(6) Uani 1 1 d . . . H18A H 0.6115 1.1148 0.1037 0.028 Uiso 1 1 calc R . . C19 C 0.8039(3) 1.1381(2) 0.2187(2) 0.0239(6) Uani 1 1 d . . . H19A H 0.8641 1.2096 0.2109 0.029 Uiso 1 1 calc R . . C20 C 0.8650(3) 1.0882(2) 0.2950(2) 0.0253(6) Uani 1 1 d . . . H20A H 0.9656 1.1269 0.3391 0.030 Uiso 1 1 calc R . . C21 C 0.7761(3) 0.9809(2) 0.30530(19) 0.0206(5) Uani 1 1 d . . . H21A H 0.8185 0.9477 0.3562 0.025 Uiso 1 1 calc R . . C22 C 0.4046(3) 0.8210(2) 0.34412(18) 0.0185(5) Uani 1 1 d . . . C23 C 0.3902(3) 0.9269(2) 0.3523(2) 0.0234(6) Uani 1 1 d . . . H23A H 0.4356 0.9800 0.3166 0.028 Uiso 1 1 calc R . . C24 C 0.3086(4) 0.9534(2) 0.4134(2) 0.0288(6) Uani 1 1 d . . . H24A H 0.3006 1.0243 0.4192 0.035 Uiso 1 1 calc R . . C25 C 0.2393(4) 0.8740(3) 0.4657(2) 0.0292(6) Uani 1 1 d . . . H25A H 0.1831 0.8912 0.5057 0.035 Uiso 1 1 calc R . . C26 C 0.2534(4) 0.7685(3) 0.4585(2) 0.0315(7) Uani 1 1 d . . . H26A H 0.2077 0.7156 0.4942 0.038 Uiso 1 1 calc R . . C27 C 0.3358(4) 0.7423(2) 0.3981(2) 0.0265(6) Uani 1 1 d . . . H27A H 0.3452 0.6718 0.3935 0.032 Uiso 1 1 calc R . . C28 C 0.3475(3) 0.72750(19) 0.14314(18) 0.0158(5) Uani 1 1 d . . . C29 C 0.3902(3) 0.7157(2) 0.05700(18) 0.0183(5) Uani 1 1 d . . . H29A H 0.4971 0.7378 0.0602 0.022 Uiso 1 1 calc R . . C30 C 0.2735(3) 0.6711(2) -0.03266(19) 0.0223(6) Uani 1 1 d . . . H30A H 0.3024 0.6629 -0.0895 0.027 Uiso 1 1 calc R . . C31 C 0.1129(3) 0.6385(2) -0.0384(2) 0.0246(6) Uani 1 1 d . . . H31A H 0.0345 0.6099 -0.0988 0.030 Uiso 1 1 calc R . . C32 C 0.0714(3) 0.6494(2) 0.0476(2) 0.0243(6) Uani 1 1 d . . . H32A H -0.0355 0.6266 0.0446 0.029 Uiso 1 1 calc R . . C33 C 0.1871(3) 0.6935(2) 0.13717(19) 0.0185(5) Uani 1 1 d . . . H33A H 0.1577 0.7005 0.1939 0.022 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 0.01399(18) 0.01578(17) 0.01445(18) 0.00084(13) 0.00345(14) 0.00561(14) Fe2 0.01520(18) 0.01915(18) 0.01478(18) 0.00201(13) 0.00486(14) 0.00862(14) S1 0.0165(3) 0.0190(3) 0.0151(3) 0.0020(2) 0.0062(2) 0.0084(2) S2 0.0161(3) 0.0175(3) 0.0143(3) 0.0018(2) 0.0051(2) 0.0058(2) P 0.0145(3) 0.0149(3) 0.0151(3) 0.0002(2) 0.0039(2) 0.0052(2) N1 0.0160(10) 0.0212(10) 0.0193(11) 0.0006(8) 0.0065(9) 0.0068(9) N2 0.0181(11) 0.0183(10) 0.0169(10) 0.0011(8) 0.0050(8) 0.0061(9) O1 0.0221(11) 0.0320(11) 0.0469(13) 0.0046(10) 0.0178(10) 0.0035(9) O2 0.0432(14) 0.0438(12) 0.0196(11) -0.0069(9) -0.0027(10) 0.0132(11) O3 0.0215(10) 0.0503(13) 0.0308(11) 0.0028(10) 0.0106(9) 0.0158(10) O4 0.0345(12) 0.0529(13) 0.0184(10) 0.0031(9) 0.0028(9) 0.0250(11) O5 0.0324(12) 0.0219(10) 0.0505(14) 0.0052(9) 0.0090(10) 0.0149(9) C1 0.0211(13) 0.0205(12) 0.0215(13) 0.0002(10) 0.0041(11) 0.0088(11) C2 0.0212(13) 0.0247(13) 0.0243(14) 0.0035(11) 0.0048(11) 0.0080(11) C3 0.0237(14) 0.0288(13) 0.0175(13) 0.0009(10) 0.0051(11) 0.0124(12) C4 0.0238(14) 0.0252(13) 0.0229(14) 0.0033(11) 0.0098(11) 0.0138(11) C5 0.0208(13) 0.0308(14) 0.0225(13) 0.0034(11) 0.0062(11) 0.0154(12) C6 0.0144(12) 0.0211(12) 0.0217(13) -0.0018(10) 0.0058(10) 0.0063(10) C7 0.0126(11) 0.0187(11) 0.0169(12) 0.0011(9) 0.0048(9) 0.0061(9) C8 0.0156(12) 0.0182(11) 0.0215(13) 0.0030(10) 0.0054(10) 0.0088(10) C9 0.0216(13) 0.0219(12) 0.0271(14) 0.0071(11) 0.0131(11) 0.0084(11) C10 0.0255(14) 0.0184(12) 0.0352(16) 0.0079(11) 0.0120(12) 0.0100(11) C11 0.0231(13) 0.0184(12) 0.0273(14) -0.0008(10) 0.0071(11) 0.0091(11) C12 0.0208(13) 0.0210(12) 0.0211(13) 0.0006(10) 0.0074(11) 0.0088(11) C13 0.0141(11) 0.0171(11) 0.0179(12) 0.0017(9) 0.0040(10) 0.0058(10) C14 0.0116(11) 0.0172(11) 0.0212(12) 0.0038(9) 0.0041(10) 0.0053(9) C15 0.0167(12) 0.0172(11) 0.0175(12) 0.0026(9) 0.0022(10) 0.0041(10) C16 0.0164(12) 0.0155(11) 0.0210(12) -0.0010(9) 0.0061(10) 0.0046(10) C17 0.0207(13) 0.0181(11) 0.0222(13) 0.0011(10) 0.0074(11) 0.0072(10) C18 0.0297(15) 0.0206(12) 0.0237(13) 0.0068(10) 0.0113(11) 0.0123(11) C19 0.0257(14) 0.0159(12) 0.0314(15) 0.0006(11) 0.0148(12) 0.0049(11) C20 0.0173(13) 0.0220(12) 0.0310(15) -0.0059(11) 0.0062(11) 0.0030(11) C21 0.0198(13) 0.0207(12) 0.0191(12) 0.0001(10) 0.0036(10) 0.0069(11) C22 0.0178(12) 0.0220(12) 0.0140(12) -0.0015(9) 0.0015(10) 0.0083(10) C23 0.0255(14) 0.0233(12) 0.0230(13) 0.0004(10) 0.0068(11) 0.0117(11) C24 0.0299(15) 0.0301(14) 0.0271(14) -0.0052(12) 0.0050(12) 0.0166(13) C25 0.0326(16) 0.0416(16) 0.0184(13) -0.0015(12) 0.0097(12) 0.0194(14) C26 0.0390(17) 0.0415(17) 0.0273(15) 0.0120(13) 0.0186(13) 0.0235(15) C27 0.0326(16) 0.0295(14) 0.0246(14) 0.0049(11) 0.0145(12) 0.0157(13) C28 0.0180(12) 0.0118(10) 0.0170(12) 0.0029(9) 0.0035(10) 0.0059(9) C29 0.0200(13) 0.0157(11) 0.0210(13) 0.0048(10) 0.0077(10) 0.0071(10) C30 0.0344(15) 0.0142(11) 0.0179(12) 0.0026(9) 0.0085(11) 0.0079(11) C31 0.0260(14) 0.0192(12) 0.0206(13) -0.0044(10) -0.0017(11) 0.0060(11) C32 0.0181(13) 0.0205(12) 0.0304(15) 0.0033(11) 0.0023(11) 0.0063(11) C33 0.0183(12) 0.0160(11) 0.0215(13) 0.0014(10) 0.0058(10) 0.0071(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 C2 1.773(3) . ? Fe1 C1 1.777(3) . ? Fe1 P 2.2441(7) . ? Fe1 S2 2.2735(7) . ? Fe1 S1 2.2805(7) . ? Fe1 Fe2 2.5146(5) . ? Fe2 C3 1.786(3) . ? Fe2 C4 1.785(3) . ? Fe2 C5 1.812(3) . ? Fe2 S1 2.2679(7) . ? Fe2 S2 2.2847(7) . ? S1 C6 1.849(3) . ? S2 C15 1.845(3) . ? P C28 1.827(3) . ? P C16 1.834(2) . ? P C22 1.836(3) . ? N1 C7 1.315(3) . ? N1 C8 1.375(3) . ? N2 C14 1.315(3) . ? N2 C13 1.371(3) . ? O1 C1 1.148(3) . ? O2 C2 1.147(3) . ? O3 C3 1.140(3) . ? O4 C4 1.146(3) . ? O5 C5 1.146(3) . ? C6 C7 1.501(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C14 1.433(3) . ? C8 C9 1.405(3) . ? C8 C13 1.419(3) . ? C9 C10 1.364(4) . ? C9 H9A 0.9300 . ? C10 C11 1.414(4) . ? C10 H10A 0.9300 . ? C11 C12 1.375(4) . ? C11 H11A 0.9300 . ? C12 C13 1.417(3) . ? C12 H12A 0.9300 . ? C14 C15 1.492(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C21 1.391(4) . ? C16 C17 1.403(4) . ? C17 C18 1.387(4) . ? C17 H17A 0.9300 . ? C18 C19 1.382(4) . ? C18 H18A 0.9300 . ? C19 C20 1.388(4) . ? C19 H19A 0.9300 . ? C20 C21 1.385(4) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C27 1.395(4) . ? C22 C23 1.399(4) . ? C23 C24 1.392(4) . ? C23 H23A 0.9300 . ? C24 C25 1.386(4) . ? C24 H24A 0.9300 . ? C25 C26 1.392(4) . ? C25 H25A 0.9300 . ? C26 C27 1.389(4) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 C33 1.391(4) . ? C28 C29 1.403(4) . ? C29 C30 1.384(4) . ? C29 H29A 0.9300 . ? C30 C31 1.395(4) . ? C30 H30A 0.9300 . ? C31 C32 1.394(4) . ? C31 H31A 0.9300 . ? C32 C33 1.379(4) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? 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 C2 Fe1 C1 91.91(12) . . ? C2 Fe1 P 93.25(9) . . ? C1 Fe1 P 97.71(9) . . ? C2 Fe1 S2 159.32(9) . . ? C1 Fe1 S2 84.00(9) . . ? P Fe1 S2 107.38(3) . . ? C2 Fe1 S1 88.39(9) . . ? C1 Fe1 S1 153.75(9) . . ? P Fe1 S1 108.47(3) . . ? S2 Fe1 S1 86.52(2) . . ? C2 Fe1 Fe2 104.20(9) . . ? C1 Fe1 Fe2 98.51(9) . . ? P Fe1 Fe2 155.66(2) . . ? S2 Fe1 Fe2 56.731(19) . . ? S1 Fe1 Fe2 56.199(19) . . ? C3 Fe2 C4 90.47(12) . . ? C3 Fe2 C5 98.79(12) . . ? C4 Fe2 C5 99.31(12) . . ? C3 Fe2 S1 160.71(9) . . ? C4 Fe2 S1 87.34(9) . . ? C5 Fe2 S1 100.48(9) . . ? C3 Fe2 S2 85.67(9) . . ? C4 Fe2 S2 149.54(9) . . ? C5 Fe2 S2 111.14(9) . . ? S1 Fe2 S2 86.55(2) . . ? C3 Fe2 Fe1 104.59(9) . . ? C4 Fe2 Fe1 95.92(8) . . ? C5 Fe2 Fe1 151.89(9) . . ? S1 Fe2 Fe1 56.676(19) . . ? S2 Fe2 Fe1 56.31(2) . . ? C6 S1 Fe2 113.64(8) . . ? C6 S1 Fe1 118.56(9) . . ? Fe2 S1 Fe1 67.13(2) . . ? C15 S2 Fe1 116.32(9) . . ? C15 S2 Fe2 115.39(8) . . ? Fe1 S2 Fe2 66.96(2) . . ? C28 P C16 102.69(11) . . ? C28 P C22 103.54(12) . . ? C16 P C22 101.85(11) . . ? C28 P Fe1 114.18(8) . . ? C16 P Fe1 115.73(9) . . ? C22 P Fe1 116.92(8) . . ? C7 N1 C8 116.8(2) . . ? C14 N2 C13 116.2(2) . . ? O1 C1 Fe1 176.3(2) . . ? O2 C2 Fe1 178.3(3) . . ? O3 C3 Fe2 179.4(3) . . ? O4 C4 Fe2 177.5(3) . . ? O5 C5 Fe2 175.8(2) . . ? C7 C6 S1 115.45(18) . . ? C7 C6 H6A 108.4 . . ? S1 C6 H6A 108.4 . . ? C7 C6 H6B 108.4 . . ? S1 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? N1 C7 C14 122.1(2) . . ? N1 C7 C6 117.5(2) . . ? C14 C7 C6 120.4(2) . . ? N1 C8 C9 119.9(2) . . ? N1 C8 C13 120.7(2) . . ? C9 C8 C13 119.4(2) . . ? C10 C9 C8 120.3(2) . . ? C10 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C9 C10 C11 120.8(2) . . ? C9 C10 H10A 119.6 . . ? C11 C10 H10A 119.6 . . ? C12 C11 C10 120.4(2) . . ? C12 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? C11 C12 C13 119.6(2) . . ? C11 C12 H12A 120.2 . . ? C13 C12 H12A 120.2 . . ? N2 C13 C12 118.9(2) . . ? N2 C13 C8 121.6(2) . . ? C12 C13 C8 119.5(2) . . ? N2 C14 C7 122.6(2) . . ? N2 C14 C15 117.7(2) . . ? C7 C14 C15 119.7(2) . . ? C14 C15 S2 112.56(17) . . ? C14 C15 H15A 109.1 . . ? S2 C15 H15A 109.1 . . ? C14 C15 H15B 109.1 . . ? S2 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C21 C16 C17 118.2(2) . . ? C21 C16 P 120.29(19) . . ? C17 C16 P 121.45(19) . . ? C18 C17 C16 120.5(2) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C19 C18 C17 120.4(2) . . ? C19 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? C18 C19 C20 119.8(2) . . ? C18 C19 H19A 120.1 . . ? C20 C19 H19A 120.1 . . ? C21 C20 C19 119.9(2) . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C20 C21 C16 121.2(2) . . ? C20 C21 H21A 119.4 . . ? C16 C21 H21A 119.4 . . ? C27 C22 C23 119.0(2) . . ? C27 C22 P 119.9(2) . . ? C23 C22 P 121.0(2) . . ? C24 C23 C22 120.5(3) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C23 C24 C25 119.9(3) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C24 C25 C26 120.1(3) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C27 C26 C25 120.0(3) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 C22 120.5(3) . . ? C26 C27 H27A 119.8 . . ? C22 C27 H27A 119.8 . . ? C33 C28 C29 119.2(2) . . ? C33 C28 P 122.19(19) . . ? C29 C28 P 118.6(2) . . ? C30 C29 C28 120.1(2) . . ? C30 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? C29 C30 C31 120.5(2) . . ? C29 C30 H30A 119.8 . . ? C31 C30 H30A 119.8 . . ? C30 C31 C32 119.1(2) . . ? C30 C31 H31A 120.5 . . ? C32 C31 H31A 120.5 . . ? C33 C32 C31 120.7(3) . . ? C33 C32 H32A 119.6 . . ? C31 C32 H32A 119.6 . . ? C32 C33 C28 120.4(2) . . ? C32 C33 H33A 119.8 . . ? C28 C33 H33A 119.8 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.514 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.089 _publ_section_references ; Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ; #==END data_compound_8 _database_code_depnum_ccdc_archive 'CCDC 816118' #TrackingRef '- cifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H21 Cl2 Fe2 N3 O6 S2' _chemical_formula_weight 658.13 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.174(4) _cell_length_b 11.761(6) _cell_length_c 13.765(7) _cell_angle_alpha 89.067(15) _cell_angle_beta 81.459(14) _cell_angle_gamma 72.711(10) _cell_volume 1401.7(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3601 _cell_measurement_theta_min 3.63 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max .22 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 1.414 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5083 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku Crystalclear)' _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 'Saturn70 (4x4 bin mode)' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 10801 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.63 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6235 _reflns_number_gt 4888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1055P)^2^+2.1190P] 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 6235 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0752 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1777 _refine_ls_wR_factor_gt 0.1602 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 0.34529(6) 0.22198(5) 0.14631(4) 0.01807(16) Uani 1 1 d . . . Fe2 Fe 0.10794(6) 0.20506(5) 0.08286(4) 0.02054(17) Uani 1 1 d . . . S1 S 0.17321(11) 0.14235(9) 0.23154(7) 0.0222(2) Uani 1 1 d . . . S2 S 0.14548(11) 0.38042(8) 0.11920(7) 0.0209(2) Uani 1 1 d . . . N1 N 0.1663(4) 0.3120(4) 0.4524(3) 0.0312(8) Uani 1 1 d . . . N2 N 0.1286(4) 0.5273(3) 0.3490(2) 0.0267(7) Uani 1 1 d . . . N3 N 0.5176(4) 0.2919(3) -0.0392(2) 0.0253(7) Uani 1 1 d . . . O1 O 0.4932(4) 0.3009(3) 0.2961(2) 0.0364(7) Uani 1 1 d . . . O2 O 0.5529(4) -0.0226(3) 0.1163(3) 0.0411(8) Uani 1 1 d . . . O3 O 0.1630(4) 0.2725(3) -0.1226(2) 0.0415(8) Uani 1 1 d . . . O4 O 0.1839(4) -0.0476(3) 0.0247(3) 0.0392(8) Uani 1 1 d . . . O5 O -0.2302(4) 0.2680(4) 0.1269(3) 0.0444(9) Uani 1 1 d . . . C1 C 0.4355(4) 0.2715(4) 0.2374(3) 0.0246(8) Uani 1 1 d . . . C2 C 0.4723(4) 0.0749(4) 0.1282(3) 0.0250(8) Uani 1 1 d . . . C3 C 0.1405(5) 0.2449(4) -0.0429(3) 0.0275(9) Uani 1 1 d . . . C4 C 0.1542(5) 0.0512(4) 0.0475(3) 0.0277(9) Uani 1 1 d . . . C5 C -0.1002(5) 0.2426(4) 0.1079(3) 0.0278(9) Uani 1 1 d . . . C6 C 0.0450(5) 0.2327(4) 0.3371(3) 0.0300(9) Uani 1 1 d . . . H6A H -0.0564 0.2683 0.3185 0.036 Uiso 1 1 calc R . . H6B H 0.0337 0.1804 0.3911 0.036 Uiso 1 1 calc R . . C7 C 0.1016(4) 0.3296(4) 0.3722(3) 0.0249(8) Uani 1 1 d . . . C8 C 0.2157(5) 0.4027(5) 0.4837(3) 0.0320(10) Uani 1 1 d . . . C9 C 0.2863(5) 0.3881(5) 0.5697(3) 0.0414(12) Uani 1 1 d . . . H9A H 0.2994 0.3178 0.6040 0.050 Uiso 1 1 calc R . . C10 C 0.3355(5) 0.4785(6) 0.6022(4) 0.0471(14) Uani 1 1 d . . . H10A H 0.3813 0.4693 0.6589 0.057 Uiso 1 1 calc R . . C11 C 0.3172(5) 0.5843(6) 0.5507(4) 0.0477(15) Uani 1 1 d . . . H11A H 0.3527 0.6439 0.5731 0.057 Uiso 1 1 calc R . . C12 C 0.2476(5) 0.6013(5) 0.4676(3) 0.0371(11) Uani 1 1 d . . . H12A H 0.2344 0.6726 0.4349 0.044 Uiso 1 1 calc R . . C13 C 0.1963(5) 0.5101(4) 0.4319(3) 0.0310(10) Uani 1 1 d . . . C14 C 0.0834(4) 0.4383(4) 0.3198(3) 0.0240(8) Uani 1 1 d . . . C15 C 0.0100(5) 0.4552(4) 0.2281(3) 0.0255(8) Uani 1 1 d . . . H15A H -0.0282 0.5398 0.2166 0.031 Uiso 1 1 calc R . . H15B H -0.0776 0.4240 0.2376 0.031 Uiso 1 1 calc R . . C16 C 0.4528(4) 0.2660(3) 0.0326(3) 0.0216(8) Uani 1 1 d . . . C17 C 0.5859(5) 0.3292(4) -0.1324(3) 0.0276(9) Uani 1 1 d . . . C18 C 0.4854(7) 0.4542(4) -0.1484(4) 0.0437(12) Uani 1 1 d . . . H18A H 0.3924 0.4502 -0.1703 0.066 Uiso 1 1 calc R . . H18B H 0.5406 0.4915 -0.1973 0.066 Uiso 1 1 calc R . . H18C H 0.4598 0.4999 -0.0878 0.066 Uiso 1 1 calc R . . C19 C 0.7509(6) 0.3269(5) -0.1234(4) 0.0409(11) Uani 1 1 d . . . H19A H 0.8108 0.2470 -0.1125 0.061 Uiso 1 1 calc R . . H19B H 0.7490 0.3778 -0.0691 0.061 Uiso 1 1 calc R . . H19C H 0.7964 0.3546 -0.1829 0.061 Uiso 1 1 calc R . . C20 C 0.5831(6) 0.2429(4) -0.2121(3) 0.0384(11) Uani 1 1 d . . . H20A H 0.4781 0.2467 -0.2160 0.058 Uiso 1 1 calc R . . H20B H 0.6390 0.1634 -0.1967 0.058 Uiso 1 1 calc R . . H20C H 0.6304 0.2637 -0.2740 0.058 Uiso 1 1 calc R . . C21 C 0.0740(13) 0.1344(11) 0.6574(9) 0.110(3) Uani 1 1 d . . . H21A H 0.0207 0.2113 0.6897 0.132 Uiso 1 1 calc R . . H21B H 0.1596 0.1430 0.6104 0.132 Uiso 1 1 calc R . . Cl1 Cl 0.1453(7) 0.0274(6) 0.7470(4) 0.206(2) Uani 1 1 d . . . Cl2 Cl -0.0480(5) 0.0888(4) 0.5987(3) 0.1596(15) Uani 1 1 d . . . O6 O 0.5756(15) 0.0572(12) 0.5569(12) 0.271(10) Uani 1 1 d . . . H0A H 0.6754 0.0136 0.5519 0.325 Uiso 1 1 d R . . H0B H 0.5229 0.0762 0.6179 0.325 Uiso 1 1 d 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 0.0165(3) 0.0190(3) 0.0195(3) -0.0005(2) -0.0020(2) -0.0068(2) Fe2 0.0176(3) 0.0208(3) 0.0242(3) -0.0034(2) -0.0036(2) -0.0066(2) S1 0.0210(5) 0.0225(5) 0.0237(5) 0.0006(4) 0.0001(4) -0.0091(4) S2 0.0226(5) 0.0183(5) 0.0219(5) -0.0017(3) -0.0043(3) -0.0059(4) N1 0.0291(18) 0.039(2) 0.0238(17) 0.0000(15) 0.0019(14) -0.0098(16) N2 0.0249(17) 0.0297(18) 0.0239(17) -0.0064(14) 0.0007(13) -0.0073(14) N3 0.0279(17) 0.0258(17) 0.0231(17) 0.0016(14) -0.0018(13) -0.0103(14) O1 0.0334(17) 0.051(2) 0.0297(16) -0.0044(14) -0.0081(13) -0.0192(15) O2 0.0350(18) 0.0259(17) 0.053(2) 0.0030(15) 0.0047(15) -0.0011(14) O3 0.050(2) 0.043(2) 0.0269(17) 0.0018(14) -0.0083(14) -0.0066(16) O4 0.0434(19) 0.0215(16) 0.053(2) -0.0077(14) -0.0057(15) -0.0098(14) O5 0.0220(16) 0.057(2) 0.051(2) -0.0135(18) -0.0003(14) -0.0091(15) C1 0.0204(18) 0.032(2) 0.0213(18) -0.0020(16) 0.0023(15) -0.0109(16) C2 0.0190(18) 0.030(2) 0.027(2) 0.0020(16) -0.0002(15) -0.0106(17) C3 0.024(2) 0.027(2) 0.031(2) -0.0053(17) -0.0086(16) -0.0065(16) C4 0.0225(19) 0.034(2) 0.027(2) -0.0035(17) -0.0037(15) -0.0094(17) C5 0.025(2) 0.031(2) 0.030(2) -0.0056(17) -0.0062(16) -0.0094(17) C6 0.027(2) 0.037(2) 0.025(2) -0.0061(17) 0.0077(16) -0.0132(18) C7 0.0199(18) 0.030(2) 0.0211(18) -0.0047(16) 0.0039(14) -0.0047(16) C8 0.022(2) 0.050(3) 0.023(2) -0.0074(19) 0.0018(15) -0.0102(19) C9 0.031(2) 0.065(3) 0.024(2) -0.002(2) -0.0015(18) -0.011(2) C10 0.027(2) 0.085(4) 0.028(2) -0.016(3) -0.0032(18) -0.014(3) C11 0.026(2) 0.078(4) 0.040(3) -0.033(3) 0.005(2) -0.019(2) C12 0.024(2) 0.053(3) 0.035(2) -0.017(2) 0.0038(18) -0.015(2) C13 0.0202(19) 0.046(3) 0.025(2) -0.0144(19) 0.0036(15) -0.0093(18) C14 0.0182(18) 0.028(2) 0.0228(18) -0.0080(16) 0.0019(14) -0.0041(15) C15 0.0235(19) 0.026(2) 0.0252(19) -0.0066(16) -0.0024(15) -0.0044(16) C16 0.0177(17) 0.0219(19) 0.0258(19) -0.0041(15) -0.0030(14) -0.0065(15) C17 0.036(2) 0.028(2) 0.0222(19) 0.0029(16) 0.0019(16) -0.0176(18) C18 0.072(4) 0.033(3) 0.030(2) 0.004(2) -0.017(2) -0.017(2) C19 0.042(3) 0.052(3) 0.036(2) 0.007(2) -0.001(2) -0.028(2) C20 0.055(3) 0.037(3) 0.026(2) -0.0079(19) 0.007(2) -0.023(2) C21 0.099(7) 0.114(8) 0.120(8) -0.010(7) -0.014(6) -0.036(6) Cl1 0.249(6) 0.230(5) 0.198(5) 0.049(4) -0.085(4) -0.138(5) Cl2 0.175(3) 0.133(3) 0.184(4) 0.056(3) -0.021(3) -0.071(3) O6 0.228(12) 0.205(12) 0.323(17) -0.165(13) -0.167(13) 0.090(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 C2 1.773(4) . ? Fe1 C1 1.793(4) . ? Fe1 C16 1.873(4) . ? Fe1 S1 2.2447(13) . ? Fe1 S2 2.2632(13) . ? Fe1 Fe2 2.5241(12) . ? Fe2 C4 1.790(5) . ? Fe2 C3 1.791(5) . ? Fe2 C5 1.808(4) . ? Fe2 S2 2.2648(14) . ? Fe2 S1 2.2679(15) . ? S1 C6 1.850(4) . ? S2 C15 1.846(4) . ? N1 C7 1.315(5) . ? N1 C8 1.375(6) . ? N2 C14 1.324(5) . ? N2 C13 1.363(6) . ? N3 C16 1.160(5) . ? N3 C17 1.462(5) . ? O1 C1 1.139(5) . ? O2 C2 1.163(5) . ? O3 C3 1.146(5) . ? O4 C4 1.149(5) . ? O5 C5 1.131(5) . ? C6 C7 1.500(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C14 1.435(6) . ? C8 C13 1.418(7) . ? C8 C9 1.416(6) . ? C9 C10 1.377(8) . ? C9 H9A 0.9300 . ? C10 C11 1.400(9) . ? C10 H10A 0.9300 . ? C11 C12 1.375(7) . ? C11 H11A 0.9300 . ? C12 C13 1.414(6) . ? C12 H12A 0.9300 . ? C14 C15 1.500(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C17 C20 1.514(6) . ? C17 C18 1.518(7) . ? C17 C19 1.530(6) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 Cl2 1.683(11) . ? C21 Cl1 1.797(13) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? O6 H0A 0.9000 . ? O6 H0B 0.9000 . ? 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 C2 Fe1 C1 97.80(19) . . ? C2 Fe1 C16 89.12(18) . . ? C1 Fe1 C16 99.59(17) . . ? C2 Fe1 S1 87.01(13) . . ? C1 Fe1 S1 104.99(13) . . ? C16 Fe1 S1 155.41(12) . . ? C2 Fe1 S2 156.27(14) . . ? C1 Fe1 S2 105.88(14) . . ? C16 Fe1 S2 85.60(12) . . ? S1 Fe1 S2 88.24(5) . . ? C2 Fe1 Fe2 102.52(13) . . ? C1 Fe1 Fe2 151.13(12) . . ? C16 Fe1 Fe2 101.00(12) . . ? S1 Fe1 Fe2 56.43(4) . . ? S2 Fe1 Fe2 56.15(4) . . ? C4 Fe2 C3 91.1(2) . . ? C4 Fe2 C5 99.74(19) . . ? C3 Fe2 C5 102.31(19) . . ? C4 Fe2 S2 158.82(13) . . ? C3 Fe2 S2 85.56(14) . . ? C5 Fe2 S2 101.40(14) . . ? C4 Fe2 S1 87.05(14) . . ? C3 Fe2 S1 156.24(13) . . ? C5 Fe2 S1 101.35(14) . . ? S2 Fe2 S1 87.64(4) . . ? C4 Fe2 Fe1 104.58(13) . . ? C3 Fe2 Fe1 102.34(13) . . ? C5 Fe2 Fe1 144.73(13) . . ? S2 Fe2 Fe1 56.09(3) . . ? S1 Fe2 Fe1 55.55(3) . . ? C6 S1 Fe1 116.42(15) . . ? C6 S1 Fe2 114.23(16) . . ? Fe1 S1 Fe2 68.02(4) . . ? C15 S2 Fe1 116.93(14) . . ? C15 S2 Fe2 111.13(14) . . ? Fe1 S2 Fe2 67.76(4) . . ? C7 N1 C8 116.7(4) . . ? C14 N2 C13 116.3(4) . . ? C16 N3 C17 174.9(4) . . ? O1 C1 Fe1 178.7(4) . . ? O2 C2 Fe1 178.5(4) . . ? O3 C3 Fe2 178.3(4) . . ? O4 C4 Fe2 179.9(5) . . ? O5 C5 Fe2 177.3(4) . . ? C7 C6 S1 114.1(3) . . ? C7 C6 H6A 108.7 . . ? S1 C6 H6A 108.7 . . ? C7 C6 H6B 108.7 . . ? S1 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? N1 C7 C14 121.7(4) . . ? N1 C7 C6 117.8(4) . . ? C14 C7 C6 120.5(4) . . ? N1 C8 C13 121.2(4) . . ? N1 C8 C9 118.9(5) . . ? C13 C8 C9 119.8(5) . . ? C10 C9 C8 119.6(5) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? C9 C10 C11 120.6(5) . . ? C9 C10 H10A 119.7 . . ? C11 C10 H10A 119.7 . . ? C12 C11 C10 121.0(5) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C13 119.9(5) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? N2 C13 C8 121.4(4) . . ? N2 C13 C12 119.5(5) . . ? C8 C13 C12 119.1(4) . . ? N2 C14 C7 122.7(4) . . ? N2 C14 C15 117.0(4) . . ? C7 C14 C15 120.3(4) . . ? C14 C15 S2 112.5(3) . . ? C14 C15 H15A 109.1 . . ? S2 C15 H15A 109.1 . . ? C14 C15 H15B 109.1 . . ? S2 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? N3 C16 Fe1 178.3(3) . . ? N3 C17 C20 107.6(3) . . ? N3 C17 C18 106.4(4) . . ? C20 C17 C18 111.2(4) . . ? N3 C17 C19 108.1(3) . . ? C20 C17 C19 111.6(4) . . ? C18 C17 C19 111.6(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Cl2 C21 Cl1 109.7(7) . . ? Cl2 C21 H21A 109.7 . . ? Cl1 C21 H21A 109.7 . . ? Cl2 C21 H21B 109.7 . . ? Cl1 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? H0A O6 H0B 117.0 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.063 _refine_diff_density_min -1.306 _refine_diff_density_rms 0.126 _publ_section_references ; Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ; #==END data_compound_9 _database_code_depnum_ccdc_archive 'CCDC 816119' #TrackingRef '- cifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H26 Cl0 Fe2 N4 O4 S2' _chemical_formula_weight 610.31 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.390(3) _cell_length_b 11.082(3) _cell_length_c 13.014(4) _cell_angle_alpha 85.726(8) _cell_angle_beta 86.282(7) _cell_angle_gamma 68.586(6) _cell_volume 1389.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3453 _cell_measurement_theta_min 3.3723 _cell_measurement_theta_max 27.4565 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 1.230 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3024 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere Rigaku Crystalclear' _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 'Saturn70 (4x4 bin mode)' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11001 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6271 _reflns_number_gt 4392 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0744P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6271 _refine_ls_number_parameters 325 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1344 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 0.39193(5) 0.84397(4) 0.30137(3) 0.01541(13) Uani 1 1 d . . . Fe2 Fe 0.62280(5) 0.70488(4) 0.36832(3) 0.01643(13) Uani 1 1 d . . . S1 S 0.42406(8) 0.66778(7) 0.41097(6) 0.01620(18) Uani 1 1 d . . . S2 S 0.56867(8) 0.71625(8) 0.20076(6) 0.01590(18) Uani 1 1 d . . . O1 O 0.1334(3) 0.8965(3) 0.1965(3) 0.0474(8) Uani 1 1 d . . . O2 O 0.2759(3) 0.9936(3) 0.4835(2) 0.0409(7) Uani 1 1 d . . . O3 O 0.7867(3) 0.8642(3) 0.3003(2) 0.0316(6) Uani 1 1 d . . . O4 O 0.6076(3) 0.7884(3) 0.5775(2) 0.0389(7) Uani 1 1 d . . . N1 N 0.2049(3) 0.5646(3) 0.2605(2) 0.0212(6) Uani 1 1 d . . . N2 N 0.3412(3) 0.6104(3) 0.0744(2) 0.0189(6) Uani 1 1 d . . . N3 N 0.4785(3) 1.0544(3) 0.1936(2) 0.0240(6) Uani 1 1 d . . . N4 N 0.8397(3) 0.4328(3) 0.3866(2) 0.0245(6) Uani 1 1 d . . . C1 C 0.2354(4) 0.8749(3) 0.2368(3) 0.0259(8) Uani 1 1 d . . . C2 C 0.3202(4) 0.9359(3) 0.4105(3) 0.0270(8) Uani 1 1 d . . . C3 C 0.7258(4) 0.7994(3) 0.3273(3) 0.0238(7) Uani 1 1 d . . . C4 C 0.6147(4) 0.7549(3) 0.4962(3) 0.0226(7) Uani 1 1 d . . . C5 C 0.4074(4) 0.5257(3) 0.3569(3) 0.0210(7) Uani 1 1 d . . . H5A H 0.4990 0.4609 0.3460 0.025 Uiso 1 1 calc R . . H5B H 0.3568 0.4884 0.4067 0.025 Uiso 1 1 calc R . . C6 C 0.3347(4) 0.5566(3) 0.2570(2) 0.0176(7) Uani 1 1 d U . . C7 C 0.1371(4) 0.5989(3) 0.1696(3) 0.0196(7) Uani 1 1 d . . . C8 C -0.0033(4) 0.6142(4) 0.1695(3) 0.0296(8) Uani 1 1 d . . . H8A H -0.0483 0.5986 0.2302 0.035 Uiso 1 1 calc R . . C9 C -0.0741(4) 0.6521(4) 0.0805(3) 0.0366(10) Uani 1 1 d . . . H9A H -0.1662 0.6596 0.0805 0.044 Uiso 1 1 calc R . . C10 C -0.0074(4) 0.6799(5) -0.0118(3) 0.0387(10) Uani 1 1 d . . . H10A H -0.0566 0.7086 -0.0716 0.046 Uiso 1 1 calc R . . C11 C 0.1295(4) 0.6644(4) -0.0129(3) 0.0305(8) Uani 1 1 d . . . H11A H 0.1733 0.6806 -0.0741 0.037 Uiso 1 1 calc R . . C12 C 0.2045(4) 0.6246(3) 0.0767(3) 0.0204(7) Uani 1 1 d . . . C13 C 0.4037(3) 0.5782(3) 0.1623(2) 0.0163(6) Uani 1 1 d U . . C14 C 0.5511(3) 0.5656(3) 0.1632(3) 0.0181(7) Uani 1 1 d . . . H14A H 0.5941 0.5450 0.0951 0.022 Uiso 1 1 calc R . . H14B H 0.5994 0.4946 0.2112 0.022 Uiso 1 1 calc R . . C15 C 0.4408(4) 0.9771(3) 0.2346(2) 0.0198(7) Uani 1 1 d . . . C16 C 0.5308(4) 1.1468(3) 0.1385(3) 0.0268(8) Uani 1 1 d . . . C17 C 0.6062(5) 1.1927(4) 0.2141(3) 0.0399(10) Uani 1 1 d . . . H17A H 0.6834 1.1203 0.2395 0.060 Uiso 1 1 calc R . . H17B H 0.5441 1.2304 0.2707 0.060 Uiso 1 1 calc R . . H17C H 0.6388 1.2565 0.1798 0.060 Uiso 1 1 calc R . . C18 C 0.6298(5) 1.0814(4) 0.0513(3) 0.0395(10) Uani 1 1 d . . . H18A H 0.5815 1.0524 0.0039 0.059 Uiso 1 1 calc R . . H18B H 0.7045 1.0083 0.0789 0.059 Uiso 1 1 calc R . . H18C H 0.6659 1.1421 0.0159 0.059 Uiso 1 1 calc R . . C19 C 0.4075(5) 1.2593(4) 0.0968(4) 0.0437(11) Uani 1 1 d . . . H19A H 0.3614 1.2282 0.0493 0.066 Uiso 1 1 calc R . . H19B H 0.4389 1.3235 0.0620 0.066 Uiso 1 1 calc R . . H19C H 0.3444 1.2972 0.1529 0.066 Uiso 1 1 calc R . . C20 C 0.7574(3) 0.5359(3) 0.3796(3) 0.0213(7) Uani 1 1 d . . . C21 C 0.9467(4) 0.3034(3) 0.3987(3) 0.0251(8) Uani 1 1 d . . . C22 C 0.8884(5) 0.2065(5) 0.3629(5) 0.0531(13) Uani 1 1 d . . . H22A H 0.8100 0.2077 0.4067 0.080 Uiso 1 1 calc R . . H22B H 0.9582 0.1210 0.3665 0.080 Uiso 1 1 calc R . . H22C H 0.8604 0.2298 0.2931 0.080 Uiso 1 1 calc R . . C23 C 0.9799(5) 0.2807(5) 0.5119(3) 0.0519(13) Uani 1 1 d . . . H23A H 1.0160 0.3438 0.5310 0.078 Uiso 1 1 calc R . . H23B H 1.0474 0.1951 0.5237 0.078 Uiso 1 1 calc R . . H23C H 0.8971 0.2888 0.5528 0.078 Uiso 1 1 calc R . . C24 C 1.0705(5) 0.3017(5) 0.3302(4) 0.0538(14) Uani 1 1 d . . . H24A H 1.1072 0.3626 0.3530 0.081 Uiso 1 1 calc R . . H24B H 1.0428 0.3252 0.2603 0.081 Uiso 1 1 calc R . . H24C H 1.1403 0.2162 0.3337 0.081 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 0.0204(2) 0.0118(2) 0.0136(2) -0.00175(17) 0.00159(17) -0.00545(19) Fe2 0.0212(2) 0.0158(2) 0.0130(2) -0.00161(17) -0.00055(18) -0.0074(2) S1 0.0246(4) 0.0142(4) 0.0111(4) -0.0021(3) 0.0020(3) -0.0088(3) S2 0.0208(4) 0.0163(4) 0.0121(4) -0.0022(3) 0.0018(3) -0.0086(3) O1 0.0312(15) 0.0434(18) 0.063(2) -0.0080(15) -0.0190(15) -0.0047(14) O2 0.0611(19) 0.0289(15) 0.0309(15) -0.0189(12) 0.0173(14) -0.0140(15) O3 0.0426(15) 0.0363(15) 0.0278(14) -0.0002(12) 0.0005(12) -0.0288(14) O4 0.0564(19) 0.0529(18) 0.0173(14) -0.0097(13) 0.0041(13) -0.0308(16) N1 0.0292(15) 0.0193(14) 0.0168(14) -0.0052(11) 0.0042(12) -0.0110(13) N2 0.0232(14) 0.0212(14) 0.0128(13) -0.0027(11) 0.0039(11) -0.0092(12) N3 0.0366(17) 0.0199(15) 0.0189(15) -0.0026(12) 0.0000(13) -0.0140(14) N4 0.0269(15) 0.0214(16) 0.0223(16) -0.0002(12) -0.0010(12) -0.0056(14) C1 0.0286(19) 0.0201(18) 0.030(2) -0.0055(15) -0.0032(15) -0.0083(16) C2 0.0324(19) 0.0169(17) 0.029(2) 0.0001(15) 0.0054(16) -0.0070(16) C3 0.0244(17) 0.0264(19) 0.0172(17) -0.0036(14) -0.0028(14) -0.0044(16) C4 0.0302(18) 0.0247(18) 0.0177(17) 0.0004(14) 0.0005(14) -0.0162(16) C5 0.0348(19) 0.0173(16) 0.0131(16) 0.0004(12) 0.0016(14) -0.0128(15) C6 0.0310(18) 0.0116(15) 0.0156(15) -0.0050(12) 0.0019(13) -0.0138(14) C7 0.0277(17) 0.0175(16) 0.0180(16) -0.0069(13) 0.0048(13) -0.0133(14) C8 0.0277(19) 0.039(2) 0.0245(19) -0.0074(16) 0.0099(15) -0.0162(18) C9 0.0274(19) 0.056(3) 0.034(2) -0.010(2) 0.0047(17) -0.023(2) C10 0.034(2) 0.062(3) 0.024(2) -0.0068(19) -0.0030(17) -0.020(2) C11 0.032(2) 0.046(2) 0.0150(17) -0.0019(16) 0.0033(15) -0.0173(19) C12 0.0260(17) 0.0200(17) 0.0188(17) -0.0097(13) 0.0030(13) -0.0118(15) C13 0.0248(16) 0.0104(14) 0.0165(16) -0.0073(12) 0.0009(13) -0.0086(13) C14 0.0242(16) 0.0133(15) 0.0148(16) -0.0024(12) 0.0044(13) -0.0049(14) C15 0.0292(18) 0.0165(16) 0.0135(16) -0.0051(13) -0.0007(13) -0.0073(15) C16 0.045(2) 0.0200(18) 0.0189(18) -0.0012(14) 0.0064(16) -0.0167(17) C17 0.058(3) 0.043(3) 0.033(2) -0.0093(19) 0.005(2) -0.035(2) C18 0.058(3) 0.040(2) 0.032(2) -0.0194(18) 0.018(2) -0.031(2) C19 0.062(3) 0.033(2) 0.037(2) 0.0123(19) -0.003(2) -0.021(2) C20 0.0234(17) 0.0238(18) 0.0167(16) -0.0014(13) 0.0010(13) -0.0090(15) C21 0.0197(16) 0.0240(18) 0.0244(19) -0.0030(14) -0.0007(14) 0.0007(15) C22 0.052(3) 0.034(3) 0.076(4) -0.006(2) -0.002(3) -0.019(2) C23 0.060(3) 0.044(3) 0.030(2) -0.004(2) -0.009(2) 0.009(2) C24 0.034(2) 0.044(3) 0.061(3) 0.020(2) 0.018(2) 0.004(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 C2 1.770(4) . ? Fe1 C1 1.788(4) . ? Fe1 C15 1.867(3) . ? Fe1 S1 2.2646(10) . ? Fe1 S2 2.2707(10) . ? Fe1 Fe2 2.5020(8) . ? Fe2 C4 1.780(4) . ? Fe2 C3 1.786(4) . ? Fe2 C20 1.886(4) . ? Fe2 S2 2.2701(11) . ? Fe2 S1 2.2756(10) . ? S1 C5 1.840(3) . ? S2 C14 1.848(3) . ? O1 C1 1.151(5) . ? O2 C2 1.158(4) . ? O3 C3 1.143(4) . ? O4 C4 1.136(4) . ? N1 C6 1.317(4) . ? N1 C7 1.373(4) . ? N2 C13 1.313(4) . ? N2 C12 1.370(4) . ? N3 C15 1.149(4) . ? N3 C16 1.451(4) . ? N4 C20 1.151(4) . ? N4 C21 1.463(4) . ? C5 C6 1.500(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C13 1.434(4) . ? C7 C8 1.405(5) . ? C7 C12 1.420(4) . ? C8 C9 1.367(6) . ? C8 H8A 0.9300 . ? C9 C10 1.418(6) . ? C9 H9A 0.9300 . ? C10 C11 1.368(5) . ? C10 H10A 0.9300 . ? C11 C12 1.397(5) . ? C11 H11A 0.9300 . ? C13 C14 1.487(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C16 C18 1.515(5) . ? C16 C17 1.519(5) . ? C16 C19 1.521(6) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C21 C24 1.512(5) . ? C21 C23 1.517(6) . ? C21 C22 1.524(6) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? 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 C2 Fe1 C1 98.47(18) . . ? C2 Fe1 C15 92.47(15) . . ? C1 Fe1 C15 97.82(16) . . ? C2 Fe1 S1 85.63(12) . . ? C1 Fe1 S1 107.52(12) . . ? C15 Fe1 S1 154.60(11) . . ? C2 Fe1 S2 154.19(13) . . ? C1 Fe1 S2 107.31(12) . . ? C15 Fe1 S2 83.09(11) . . ? S1 Fe1 S2 87.67(4) . . ? C2 Fe1 Fe2 99.47(13) . . ? C1 Fe1 Fe2 154.88(12) . . ? C15 Fe1 Fe2 98.82(11) . . ? S1 Fe1 Fe2 56.77(3) . . ? S2 Fe1 Fe2 56.55(3) . . ? C4 Fe2 C3 89.79(15) . . ? C4 Fe2 C20 101.11(16) . . ? C3 Fe2 C20 101.86(15) . . ? C4 Fe2 S2 158.23(12) . . ? C3 Fe2 S2 86.85(11) . . ? C20 Fe2 S2 100.64(11) . . ? C4 Fe2 S1 87.03(11) . . ? C3 Fe2 S1 156.18(12) . . ? C20 Fe2 S1 101.91(10) . . ? S2 Fe2 S1 87.42(3) . . ? C4 Fe2 Fe1 103.32(12) . . ? C3 Fe2 Fe1 101.73(11) . . ? C20 Fe2 Fe1 145.84(11) . . ? S2 Fe2 Fe1 56.58(3) . . ? S1 Fe2 Fe1 56.35(3) . . ? C5 S1 Fe1 116.34(11) . . ? C5 S1 Fe2 116.57(12) . . ? Fe1 S1 Fe2 66.88(3) . . ? C14 S2 Fe2 112.46(11) . . ? C14 S2 Fe1 115.62(11) . . ? Fe2 S2 Fe1 66.87(3) . . ? C6 N1 C7 116.8(3) . . ? C13 N2 C12 116.9(3) . . ? C15 N3 C16 177.0(3) . . ? C20 N4 C21 177.7(4) . . ? O1 C1 Fe1 178.8(4) . . ? O2 C2 Fe1 178.1(4) . . ? O3 C3 Fe2 177.1(3) . . ? O4 C4 Fe2 178.9(4) . . ? C6 C5 S1 113.6(2) . . ? C6 C5 H5A 108.9 . . ? S1 C5 H5A 108.9 . . ? C6 C5 H5B 108.9 . . ? S1 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N1 C6 C13 121.7(3) . . ? N1 C6 C5 117.1(3) . . ? C13 C6 C5 121.2(3) . . ? N1 C7 C8 119.3(3) . . ? N1 C7 C12 121.2(3) . . ? C8 C7 C12 119.4(3) . . ? C9 C8 C7 120.3(3) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C8 C9 C10 120.2(3) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C11 C10 C9 120.0(4) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 120.9(3) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? N2 C12 C11 120.1(3) . . ? N2 C12 C7 120.8(3) . . ? C11 C12 C7 119.1(3) . . ? N2 C13 C6 122.5(3) . . ? N2 C13 C14 118.3(3) . . ? C6 C13 C14 119.1(3) . . ? C13 C14 S2 111.8(2) . . ? C13 C14 H14A 109.3 . . ? S2 C14 H14A 109.3 . . ? C13 C14 H14B 109.3 . . ? S2 C14 H14B 109.3 . . ? H14A C14 H14B 107.9 . . ? N3 C15 Fe1 176.2(3) . . ? N3 C16 C18 109.6(3) . . ? N3 C16 C17 108.0(3) . . ? C18 C16 C17 109.9(3) . . ? N3 C16 C19 107.7(3) . . ? C18 C16 C19 110.8(3) . . ? C17 C16 C19 110.8(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 Fe2 179.9(4) . . ? N4 C21 C24 107.9(3) . . ? N4 C21 C23 106.8(3) . . ? C24 C21 C23 112.3(4) . . ? N4 C21 C22 107.5(3) . . ? C24 C21 C22 109.7(4) . . ? C23 C21 C22 112.4(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.691 _refine_diff_density_min -1.206 _refine_diff_density_rms 0.111 _publ_section_references ; Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ; #==END