Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Graeme Hogarth' _publ_contact_author_address ; Chemistry Department University College London 20 Gordon Street London WC1H OAJ UNITED KINGDOM ; _publ_contact_author_email G.HOGARTH@UCL.AC.UK _publ_section_title ; Models of the iron-only hydrogenase: Structural studies of chelating diphosphine complexes [Fe2(CO)4(?-pdt)(?2-diphosphine)] ; loop_ _publ_author_name 'G. Hogarth' 'Fatima I. Adam' 'Idris Richards' 'Benjamin E. Sanchez' data_str0201 _database_code_depnum_ccdc_archive 'CCDC 614428' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H28 Fe2 O4 P2 S2' _chemical_formula_weight 714.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3556(13) _cell_length_b 12.1406(15) _cell_length_c 12.9298(16) _cell_angle_alpha 91.174(2) _cell_angle_beta 98.599(2) _cell_angle_gamma 102.055(2) _cell_volume 1569.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 1.195 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8505 _exptl_absorpt_correction_T_max 0.8798 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12622 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.1048 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.32 _reflns_number_total 7042 _reflns_number_gt 5039 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0528P] 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 7042 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1387 _refine_ls_wR_factor_gt 0.1253 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.63139(5) 0.78775(4) 0.20731(4) 0.03324(15) Uani 1 1 d . . . Fe2 Fe 0.52564(5) 0.63076(4) 0.32054(4) 0.03830(16) Uani 1 1 d . . . P1 P 0.73414(10) 0.93486(8) 0.31409(7) 0.0365(2) Uani 1 1 d . . . P2 P 0.84840(9) 0.79947(8) 0.20743(7) 0.0347(2) Uani 1 1 d . . . S1 S 0.56362(10) 0.60671(8) 0.15467(8) 0.0412(2) Uani 1 1 d . . . S2 S 0.43205(9) 0.77324(8) 0.25683(8) 0.0412(2) Uani 1 1 d . . . O1 O 0.6029(4) 0.9089(3) 0.0171(2) 0.0715(9) Uani 1 1 d . . . O2 O 0.3383(4) 0.4133(3) 0.3128(3) 0.0912(12) Uani 1 1 d . . . O3 O 0.4827(4) 0.7163(3) 0.5230(3) 0.0787(10) Uani 1 1 d . . . O4 O 0.7630(3) 0.5578(3) 0.4223(3) 0.0706(9) Uani 1 1 d . . . C1 C 0.6148(4) 0.8610(3) 0.0933(3) 0.0471(9) Uani 1 1 d . . . C2 C 0.4090(4) 0.5003(4) 0.3168(4) 0.0574(11) Uani 1 1 d . . . C3 C 0.5042(4) 0.6844(4) 0.4450(3) 0.0510(10) Uani 1 1 d . . . C4 C 0.6728(4) 0.5872(3) 0.3783(3) 0.0483(10) Uani 1 1 d . . . C5 C 0.4043(4) 0.5806(4) 0.0649(4) 0.0631(12) Uani 1 1 d . . . H5A H 0.4244 0.6009 -0.0040 0.076 Uiso 1 1 calc R . . H5B H 0.3682 0.4999 0.0606 0.076 Uiso 1 1 calc R . . C6 C 0.3039(7) 0.6327(9) 0.0846(7) 0.210(6) Uani 1 1 d . . . H6A H 0.2673 0.6528 0.0158 0.252 Uiso 1 1 calc R . . H6B H 0.2364 0.5714 0.1032 0.252 Uiso 1 1 calc R . . C7 C 0.2974(4) 0.7213(4) 0.1489(4) 0.0642(12) Uani 1 1 d . . . H7A H 0.2155 0.7004 0.1784 0.077 Uiso 1 1 calc R . . H7B H 0.2883 0.7841 0.1053 0.077 Uiso 1 1 calc R . . C8 C 0.9025(4) 0.9357(3) 0.2829(3) 0.0416(9) Uani 1 1 d . . . H8A H 0.9346 0.9978 0.2407 0.050 Uiso 1 1 calc R . . H8B H 0.9680 0.9339 0.3445 0.050 Uiso 1 1 calc R . . C10 C 0.7073(4) 1.0770(3) 0.2933(3) 0.0437(9) Uani 1 1 d . . . C11 C 0.5974(5) 1.0939(3) 0.2254(3) 0.0537(11) Uani 1 1 d . . . H11A H 0.5359 1.0325 0.1908 0.064 Uiso 1 1 calc R . . C12 C 0.5790(6) 1.2035(4) 0.2090(4) 0.0700(14) Uani 1 1 d . . . H12A H 0.5047 1.2150 0.1639 0.084 Uiso 1 1 calc R . . C13 C 0.6698(6) 1.2933(4) 0.2591(4) 0.0731(15) Uani 1 1 d . . . H13A H 0.6575 1.3661 0.2479 0.088 Uiso 1 1 calc R . . C14 C 0.7787(6) 1.2773(3) 0.3258(4) 0.0650(14) Uani 1 1 d . . . H14A H 0.8395 1.3394 0.3600 0.078 Uiso 1 1 calc R . . C15 C 0.7999(4) 1.1704(3) 0.3431(3) 0.0511(10) Uani 1 1 d . . . H15A H 0.8753 1.1604 0.3877 0.061 Uiso 1 1 calc R . . C20 C 0.7490(4) 0.9290(3) 0.4566(3) 0.0374(8) Uani 1 1 d . . . C21 C 0.6846(4) 0.9916(3) 0.5147(3) 0.0477(10) Uani 1 1 d . . . H21A H 0.6397 1.0436 0.4823 0.057 Uiso 1 1 calc R . . C22 C 0.6872(5) 0.9768(4) 0.6211(3) 0.0572(11) Uani 1 1 d . . . H22A H 0.6444 1.0193 0.6599 0.069 Uiso 1 1 calc R . . C23 C 0.7520(4) 0.9003(4) 0.6693(3) 0.0574(11) Uani 1 1 d . . . H23A H 0.7532 0.8908 0.7406 0.069 Uiso 1 1 calc R . . C24 C 0.8155(4) 0.8372(4) 0.6126(3) 0.0523(10) Uani 1 1 d . . . H24A H 0.8596 0.7849 0.6454 0.063 Uiso 1 1 calc R . . C25 C 0.8139(4) 0.8515(3) 0.5073(3) 0.0450(9) Uani 1 1 d . . . H25A H 0.8570 0.8084 0.4694 0.054 Uiso 1 1 calc R . . C30 C 0.9475(4) 0.7024(3) 0.2655(3) 0.0433(9) Uani 1 1 d . . . C31 C 0.9201(4) 0.5941(3) 0.2174(4) 0.0528(11) Uani 1 1 d . . . H31A H 0.8534 0.5747 0.1595 0.063 Uiso 1 1 calc R . . C32 C 0.9917(6) 0.5161(4) 0.2557(5) 0.0732(15) Uani 1 1 d . . . H32A H 0.9741 0.4448 0.2223 0.088 Uiso 1 1 calc R . . C33 C 1.0872(6) 0.5418(6) 0.3413(5) 0.089(2) Uani 1 1 d . . . H33A H 1.1330 0.4875 0.3676 0.107 Uiso 1 1 calc R . . C34 C 1.1162(6) 0.6472(6) 0.3889(4) 0.0865(19) Uani 1 1 d . . . H34A H 1.1824 0.6646 0.4475 0.104 Uiso 1 1 calc R . . C35 C 1.0486(4) 0.7282(4) 0.3512(3) 0.0615(12) Uani 1 1 d . . . H35A H 1.0708 0.8004 0.3833 0.074 Uiso 1 1 calc R . . C40 C 0.9152(4) 0.8157(3) 0.0844(3) 0.0392(8) Uani 1 1 d . . . C41 C 1.0397(4) 0.8800(3) 0.0789(3) 0.0497(10) Uani 1 1 d . . . H41A H 1.0887 0.9241 0.1370 0.060 Uiso 1 1 calc R . . C42 C 1.0927(5) 0.8788(4) -0.0145(4) 0.0615(13) Uani 1 1 d . . . H42A H 1.1760 0.9238 -0.0191 0.074 Uiso 1 1 calc R . . C43 C 1.0223(6) 0.8115(4) -0.0991(4) 0.0699(14) Uani 1 1 d . . . H43A H 1.0596 0.8086 -0.1600 0.084 Uiso 1 1 calc R . . C44 C 0.8994(6) 0.7495(4) -0.0951(4) 0.0718(14) Uani 1 1 d . . . H44A H 0.8512 0.7054 -0.1535 0.086 Uiso 1 1 calc R . . C45 C 0.8449(5) 0.7515(4) -0.0034(3) 0.0565(11) Uani 1 1 d . . . H45A H 0.7596 0.7089 -0.0012 0.068 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 0.0417(3) 0.0300(3) 0.0294(3) -0.0036(2) 0.0095(2) 0.0086(2) Fe2 0.0456(3) 0.0322(3) 0.0388(3) 0.0005(2) 0.0120(2) 0.0086(2) P1 0.0480(5) 0.0301(5) 0.0326(5) -0.0039(4) 0.0126(4) 0.0067(4) P2 0.0436(5) 0.0330(5) 0.0289(5) -0.0018(4) 0.0117(4) 0.0077(4) S1 0.0470(5) 0.0358(5) 0.0415(5) -0.0118(4) 0.0101(4) 0.0093(4) S2 0.0462(5) 0.0390(5) 0.0434(5) -0.0009(4) 0.0131(4) 0.0165(4) O1 0.093(2) 0.076(2) 0.0477(19) 0.0176(17) 0.0064(17) 0.0274(19) O2 0.081(2) 0.050(2) 0.134(4) 0.014(2) 0.018(2) -0.0076(19) O3 0.084(2) 0.111(3) 0.0447(19) -0.0093(18) 0.0252(17) 0.019(2) O4 0.067(2) 0.083(2) 0.071(2) 0.0205(19) 0.0122(17) 0.0345(19) C1 0.058(2) 0.046(2) 0.040(2) -0.0046(19) 0.0105(19) 0.017(2) C2 0.059(3) 0.048(3) 0.067(3) 0.012(2) 0.013(2) 0.012(2) C3 0.051(2) 0.054(3) 0.048(3) 0.004(2) 0.010(2) 0.009(2) C4 0.061(3) 0.040(2) 0.046(2) 0.0042(18) 0.019(2) 0.009(2) C5 0.057(3) 0.072(3) 0.053(3) -0.025(2) -0.001(2) 0.009(2) C6 0.116(6) 0.310(12) 0.194(9) -0.202(9) -0.104(6) 0.136(8) C7 0.051(3) 0.080(3) 0.062(3) 0.002(3) 0.002(2) 0.021(2) C8 0.047(2) 0.0334(19) 0.043(2) -0.0062(16) 0.0156(17) 0.0008(16) C10 0.064(2) 0.033(2) 0.038(2) -0.0015(16) 0.0228(19) 0.0072(18) C11 0.074(3) 0.039(2) 0.050(3) -0.0012(19) 0.010(2) 0.016(2) C12 0.107(4) 0.053(3) 0.058(3) 0.008(2) 0.011(3) 0.037(3) C13 0.133(5) 0.033(2) 0.061(3) 0.005(2) 0.033(3) 0.024(3) C14 0.108(4) 0.032(2) 0.053(3) -0.003(2) 0.032(3) -0.004(2) C15 0.069(3) 0.037(2) 0.047(2) -0.0019(18) 0.022(2) 0.002(2) C20 0.046(2) 0.0326(19) 0.0317(19) -0.0045(15) 0.0104(16) 0.0022(16) C21 0.064(3) 0.043(2) 0.041(2) 0.0004(18) 0.0196(19) 0.0142(19) C22 0.078(3) 0.055(3) 0.044(2) -0.006(2) 0.029(2) 0.016(2) C23 0.068(3) 0.062(3) 0.035(2) -0.005(2) 0.011(2) -0.004(2) C24 0.057(2) 0.051(3) 0.044(2) 0.004(2) 0.003(2) 0.005(2) C25 0.054(2) 0.041(2) 0.041(2) -0.0029(17) 0.0132(18) 0.0100(18) C30 0.046(2) 0.048(2) 0.039(2) 0.0080(18) 0.0162(18) 0.0107(18) C31 0.055(2) 0.045(2) 0.064(3) 0.006(2) 0.020(2) 0.014(2) C32 0.088(4) 0.055(3) 0.095(4) 0.029(3) 0.046(3) 0.034(3) C33 0.093(4) 0.118(5) 0.090(5) 0.061(4) 0.049(4) 0.070(4) C34 0.074(4) 0.147(6) 0.056(3) 0.033(4) 0.014(3) 0.059(4) C35 0.058(3) 0.089(4) 0.043(3) 0.004(2) 0.012(2) 0.026(3) C40 0.051(2) 0.040(2) 0.0332(19) 0.0025(16) 0.0164(17) 0.0166(17) C41 0.060(3) 0.046(2) 0.048(2) 0.0092(19) 0.020(2) 0.013(2) C42 0.069(3) 0.059(3) 0.071(3) 0.030(3) 0.035(3) 0.026(2) C43 0.108(4) 0.072(3) 0.050(3) 0.020(3) 0.046(3) 0.039(3) C44 0.108(4) 0.075(3) 0.038(2) -0.001(2) 0.027(3) 0.021(3) C45 0.075(3) 0.063(3) 0.035(2) 0.001(2) 0.019(2) 0.016(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 1.742(4) . ? Fe1 P1 2.2123(11) . ? Fe1 P2 2.2217(11) . ? Fe1 S1 2.2222(10) . ? Fe1 S2 2.2250(10) . ? Fe1 Fe2 2.5879(7) . ? Fe2 C2 1.775(5) . ? Fe2 C4 1.781(5) . ? Fe2 C3 1.785(4) . ? Fe2 S1 2.2614(11) . ? Fe2 S2 2.2650(11) . ? P1 C10 1.823(4) . ? P1 C20 1.830(4) . ? P1 C8 1.846(4) . ? P1 P2 2.6854(12) . ? P2 C30 1.821(4) . ? P2 C40 1.826(3) . ? P2 C8 1.840(4) . ? S1 C5 1.834(4) . ? S2 C7 1.818(5) . ? O1 C1 1.158(5) . ? O2 C2 1.149(5) . ? O3 C3 1.142(5) . ? O4 C4 1.146(5) . ? C5 C6 1.377(7) . ? C6 C7 1.365(7) . ? C10 C11 1.382(6) . ? C10 C15 1.397(6) . ? C11 C12 1.400(5) . ? C12 C13 1.361(7) . ? C13 C14 1.364(7) . ? C14 C15 1.378(6) . ? C20 C21 1.387(5) . ? C20 C25 1.388(5) . ? C21 C22 1.389(6) . ? C22 C23 1.364(6) . ? C23 C24 1.376(6) . ? C24 C25 1.373(5) . ? C30 C35 1.387(6) . ? C30 C31 1.398(5) . ? C31 C32 1.376(6) . ? C32 C33 1.353(8) . ? C33 C34 1.363(8) . ? C34 C35 1.380(7) . ? C40 C41 1.374(5) . ? C40 C45 1.381(6) . ? C41 C42 1.400(6) . ? C42 C43 1.369(7) . ? C43 C44 1.345(7) . ? C44 C45 1.389(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 P1 96.93(13) . . ? C1 Fe1 P2 92.58(14) . . ? P1 Fe1 P2 74.55(4) . . ? C1 Fe1 S1 105.05(13) . . ? P1 Fe1 S1 156.89(4) . . ? P2 Fe1 S1 97.07(4) . . ? C1 Fe1 S2 102.29(13) . . ? P1 Fe1 S2 95.97(4) . . ? P2 Fe1 S2 163.34(4) . . ? S1 Fe1 S2 86.40(4) . . ? C1 Fe1 Fe2 147.87(14) . . ? P1 Fe1 Fe2 107.51(3) . . ? P2 Fe1 Fe2 113.56(3) . . ? S1 Fe1 Fe2 55.46(3) . . ? S2 Fe1 Fe2 55.53(3) . . ? C2 Fe2 C4 99.08(19) . . ? C2 Fe2 C3 97.4(2) . . ? C4 Fe2 C3 90.85(19) . . ? C2 Fe2 S1 94.40(15) . . ? C4 Fe2 S1 94.05(13) . . ? C3 Fe2 S1 166.37(14) . . ? C2 Fe2 S2 113.36(15) . . ? C4 Fe2 S2 147.56(13) . . ? C3 Fe2 S2 84.51(14) . . ? S1 Fe2 S2 84.54(4) . . ? C2 Fe2 Fe1 144.30(15) . . ? C4 Fe2 Fe1 99.39(12) . . ? C3 Fe2 Fe1 112.59(13) . . ? S1 Fe2 Fe1 54.04(3) . . ? S2 Fe2 Fe1 54.08(3) . . ? C10 P1 C20 102.17(17) . . ? C10 P1 C8 105.84(17) . . ? C20 P1 C8 105.86(18) . . ? C10 P1 Fe1 122.97(14) . . ? C20 P1 Fe1 122.06(12) . . ? C8 P1 Fe1 95.39(12) . . ? C10 P1 P2 132.15(12) . . ? C20 P1 P2 119.33(13) . . ? C8 P1 P2 43.16(11) . . ? Fe1 P1 P2 52.88(3) . . ? C30 P2 C40 98.02(16) . . ? C30 P2 C8 108.68(19) . . ? C40 P2 C8 107.64(17) . . ? C30 P2 Fe1 126.53(12) . . ? C40 P2 Fe1 119.63(13) . . ? C8 P2 Fe1 95.23(12) . . ? C30 P2 P1 125.38(13) . . ? C40 P2 P1 131.56(12) . . ? C8 P2 P1 43.31(11) . . ? Fe1 P2 P1 52.57(3) . . ? C5 S1 Fe1 111.52(16) . . ? C5 S1 Fe2 109.40(15) . . ? Fe1 S1 Fe2 70.50(3) . . ? C7 S2 Fe1 111.45(15) . . ? C7 S2 Fe2 110.63(16) . . ? Fe1 S2 Fe2 70.39(3) . . ? O1 C1 Fe1 179.4(4) . . ? O2 C2 Fe2 176.5(4) . . ? O3 C3 Fe2 176.0(4) . . ? O4 C4 Fe2 174.7(4) . . ? C6 C5 S1 120.1(4) . . ? C7 C6 C5 134.6(6) . . ? C6 C7 S2 120.0(4) . . ? P2 C8 P1 93.53(17) . . ? C11 C10 C15 119.2(4) . . ? C11 C10 P1 120.5(3) . . ? C15 C10 P1 120.3(3) . . ? C10 C11 C12 119.9(4) . . ? C13 C12 C11 119.9(5) . . ? C12 C13 C14 120.5(4) . . ? C13 C14 C15 120.9(4) . . ? C14 C15 C10 119.6(5) . . ? C21 C20 C25 118.4(3) . . ? C21 C20 P1 121.6(3) . . ? C25 C20 P1 119.6(3) . . ? C20 C21 C22 120.0(4) . . ? C23 C22 C21 120.5(4) . . ? C22 C23 C24 120.0(4) . . ? C25 C24 C23 119.9(4) . . ? C24 C25 C20 121.1(4) . . ? C35 C30 C31 118.1(4) . . ? C35 C30 P2 125.3(3) . . ? C31 C30 P2 116.5(3) . . ? C32 C31 C30 120.2(5) . . ? C33 C32 C31 120.9(5) . . ? C32 C33 C34 119.9(5) . . ? C33 C34 C35 120.7(5) . . ? C34 C35 C30 120.2(5) . . ? C41 C40 C45 118.7(3) . . ? C41 C40 P2 122.1(3) . . ? C45 C40 P2 118.8(3) . . ? C40 C41 C42 119.8(4) . . ? C43 C42 C41 120.1(4) . . ? C44 C43 C42 120.6(4) . . ? C43 C44 C45 119.8(5) . . ? C40 C45 C44 121.0(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Fe1 Fe2 C2 27.7(3) . . . . ? P1 Fe1 Fe2 C2 165.4(2) . . . . ? P2 Fe1 Fe2 C2 -114.2(2) . . . . ? S1 Fe1 Fe2 C2 -32.1(2) . . . . ? S2 Fe1 Fe2 C2 80.3(2) . . . . ? C1 Fe1 Fe2 C4 148.0(3) . . . . ? P1 Fe1 Fe2 C4 -74.29(14) . . . . ? P2 Fe1 Fe2 C4 6.09(14) . . . . ? S1 Fe1 Fe2 C4 88.20(14) . . . . ? S2 Fe1 Fe2 C4 -159.46(14) . . . . ? C1 Fe1 Fe2 C3 -117.2(3) . . . . ? P1 Fe1 Fe2 C3 20.59(15) . . . . ? P2 Fe1 Fe2 C3 100.97(15) . . . . ? S1 Fe1 Fe2 C3 -176.92(15) . . . . ? S2 Fe1 Fe2 C3 -64.58(15) . . . . ? C1 Fe1 Fe2 S1 59.8(2) . . . . ? P1 Fe1 Fe2 S1 -162.49(5) . . . . ? P2 Fe1 Fe2 S1 -82.11(4) . . . . ? S2 Fe1 Fe2 S1 112.34(5) . . . . ? C1 Fe1 Fe2 S2 -52.6(2) . . . . ? P1 Fe1 Fe2 S2 85.17(5) . . . . ? P2 Fe1 Fe2 S2 165.54(5) . . . . ? S1 Fe1 Fe2 S2 -112.34(5) . . . . ? C1 Fe1 P1 C10 30.05(19) . . . . ? P2 Fe1 P1 C10 120.82(14) . . . . ? S1 Fe1 P1 C10 -167.99(15) . . . . ? S2 Fe1 P1 C10 -73.15(14) . . . . ? Fe2 Fe1 P1 C10 -128.84(14) . . . . ? C1 Fe1 P1 C20 164.7(2) . . . . ? P2 Fe1 P1 C20 -104.53(15) . . . . ? S1 Fe1 P1 C20 -33.33(19) . . . . ? S2 Fe1 P1 C20 61.51(15) . . . . ? Fe2 Fe1 P1 C20 5.82(15) . . . . ? C1 Fe1 P1 C8 -82.77(18) . . . . ? P2 Fe1 P1 C8 7.99(13) . . . . ? S1 Fe1 P1 C8 79.19(16) . . . . ? S2 Fe1 P1 C8 174.03(13) . . . . ? Fe2 Fe1 P1 C8 118.34(13) . . . . ? C1 Fe1 P1 P2 -90.77(13) . . . . ? S1 Fe1 P1 P2 71.20(10) . . . . ? S2 Fe1 P1 P2 166.03(4) . . . . ? Fe2 Fe1 P1 P2 110.35(3) . . . . ? C1 Fe1 P2 C30 -153.6(2) . . . . ? P1 Fe1 P2 C30 109.89(17) . . . . ? S1 Fe1 P2 C30 -48.11(17) . . . . ? S2 Fe1 P2 C30 53.1(2) . . . . ? Fe2 Fe1 P2 C30 7.19(17) . . . . ? C1 Fe1 P2 C40 -25.25(19) . . . . ? P1 Fe1 P2 C40 -121.73(14) . . . . ? S1 Fe1 P2 C40 80.26(14) . . . . ? S2 Fe1 P2 C40 -178.56(17) . . . . ? Fe2 Fe1 P2 C40 135.57(13) . . . . ? C1 Fe1 P2 C8 88.46(18) . . . . ? P1 Fe1 P2 C8 -8.01(13) . . . . ? S1 Fe1 P2 C8 -166.02(13) . . . . ? S2 Fe1 P2 C8 -64.85(19) . . . . ? Fe2 Fe1 P2 C8 -110.72(13) . . . . ? C1 Fe1 P2 P1 96.48(13) . . . . ? S1 Fe1 P2 P1 -158.01(4) . . . . ? S2 Fe1 P2 P1 -56.84(14) . . . . ? Fe2 Fe1 P2 P1 -102.71(4) . . . . ? C10 P1 P2 C30 144.3(2) . . . . ? C20 P1 P2 C30 -2.3(2) . . . . ? C8 P1 P2 C30 79.6(2) . . . . ? Fe1 P1 P2 C30 -112.07(16) . . . . ? C10 P1 P2 C40 -4.8(3) . . . . ? C20 P1 P2 C40 -151.4(2) . . . . ? C8 P1 P2 C40 -69.5(3) . . . . ? Fe1 P1 P2 C40 98.82(18) . . . . ? C10 P1 P2 C8 64.7(3) . . . . ? C20 P1 P2 C8 -81.9(2) . . . . ? Fe1 P1 P2 C8 168.32(19) . . . . ? C10 P1 P2 Fe1 -103.6(2) . . . . ? C20 P1 P2 Fe1 109.77(14) . . . . ? C8 P1 P2 Fe1 -168.32(19) . . . . ? C1 Fe1 S1 C5 -47.8(2) . . . . ? P1 Fe1 S1 C5 150.81(18) . . . . ? P2 Fe1 S1 C5 -142.35(17) . . . . ? S2 Fe1 S1 C5 54.02(17) . . . . ? Fe2 Fe1 S1 C5 103.84(17) . . . . ? C1 Fe1 S1 Fe2 -151.59(14) . . . . ? P1 Fe1 S1 Fe2 46.97(10) . . . . ? P2 Fe1 S1 Fe2 113.81(4) . . . . ? S2 Fe1 S1 Fe2 -49.82(3) . . . . ? C2 Fe2 S1 C5 55.2(2) . . . . ? C4 Fe2 S1 C5 154.6(2) . . . . ? C3 Fe2 S1 C5 -94.6(6) . . . . ? S2 Fe2 S1 C5 -57.93(17) . . . . ? Fe1 Fe2 S1 C5 -106.73(18) . . . . ? C2 Fe2 S1 Fe1 161.89(14) . . . . ? C4 Fe2 S1 Fe1 -98.66(13) . . . . ? C3 Fe2 S1 Fe1 12.1(6) . . . . ? S2 Fe2 S1 Fe1 48.81(3) . . . . ? C1 Fe1 S2 C7 49.2(2) . . . . ? P1 Fe1 S2 C7 147.66(18) . . . . ? P2 Fe1 S2 C7 -158.1(2) . . . . ? S1 Fe1 S2 C7 -55.42(18) . . . . ? Fe2 Fe1 S2 C7 -105.18(18) . . . . ? C1 Fe1 S2 Fe2 154.39(13) . . . . ? P1 Fe1 S2 Fe2 -107.16(4) . . . . ? P2 Fe1 S2 Fe2 -52.94(14) . . . . ? S1 Fe1 S2 Fe2 49.76(4) . . . . ? C2 Fe2 S2 C7 -34.9(2) . . . . ? C4 Fe2 S2 C7 146.5(3) . . . . ? C3 Fe2 S2 C7 -130.6(2) . . . . ? S1 Fe2 S2 C7 57.53(17) . . . . ? Fe1 Fe2 S2 C7 106.30(17) . . . . ? C2 Fe2 S2 Fe1 -141.21(17) . . . . ? C4 Fe2 S2 Fe1 40.2(2) . . . . ? C3 Fe2 S2 Fe1 123.10(13) . . . . ? S1 Fe2 S2 Fe1 -48.77(3) . . . . ? P1 Fe1 C1 O1 -159(40) . . . . ? P2 Fe1 C1 O1 126(40) . . . . ? S1 Fe1 C1 O1 28(40) . . . . ? S2 Fe1 C1 O1 -61(40) . . . . ? Fe2 Fe1 C1 O1 -19(40) . . . . ? C4 Fe2 C2 O2 -42(7) . . . . ? C3 Fe2 C2 O2 -134(7) . . . . ? S1 Fe2 C2 O2 53(7) . . . . ? S2 Fe2 C2 O2 139(7) . . . . ? Fe1 Fe2 C2 O2 78(7) . . . . ? C2 Fe2 C3 O3 -42(6) . . . . ? C4 Fe2 C3 O3 -141(6) . . . . ? S1 Fe2 C3 O3 108(6) . . . . ? S2 Fe2 C3 O3 71(6) . . . . ? Fe1 Fe2 C3 O3 118(6) . . . . ? C2 Fe2 C4 O4 -66(4) . . . . ? C3 Fe2 C4 O4 31(4) . . . . ? S1 Fe2 C4 O4 -161(4) . . . . ? S2 Fe2 C4 O4 112(4) . . . . ? Fe1 Fe2 C4 O4 144(4) . . . . ? Fe1 S1 C5 C6 -41.6(8) . . . . ? Fe2 S1 C5 C6 34.5(8) . . . . ? S1 C5 C6 C7 14.8(18) . . . . ? C5 C6 C7 S2 -16.3(18) . . . . ? Fe1 S2 C7 C6 44.4(8) . . . . ? Fe2 S2 C7 C6 -31.9(8) . . . . ? C30 P2 C8 P1 -122.16(17) . . . . ? C40 P2 C8 P1 132.66(17) . . . . ? Fe1 P2 C8 P1 9.29(15) . . . . ? C10 P1 C8 P2 -135.84(18) . . . . ? C20 P1 C8 P2 116.19(17) . . . . ? Fe1 P1 C8 P2 -9.33(15) . . . . ? C20 P1 C10 C11 -125.3(3) . . . . ? C8 P1 C10 C11 124.1(3) . . . . ? Fe1 P1 C10 C11 16.6(4) . . . . ? P2 P1 C10 C11 84.1(3) . . . . ? C20 P1 C10 C15 56.7(3) . . . . ? C8 P1 C10 C15 -53.9(3) . . . . ? Fe1 P1 C10 C15 -161.3(2) . . . . ? P2 P1 C10 C15 -93.9(3) . . . . ? C15 C10 C11 C12 -1.2(6) . . . . ? P1 C10 C11 C12 -179.1(3) . . . . ? C10 C11 C12 C13 0.6(7) . . . . ? C11 C12 C13 C14 -0.3(7) . . . . ? C12 C13 C14 C15 0.6(7) . . . . ? C13 C14 C15 C10 -1.2(6) . . . . ? C11 C10 C15 C14 1.5(6) . . . . ? P1 C10 C15 C14 179.4(3) . . . . ? C10 P1 C20 C21 29.0(4) . . . . ? C8 P1 C20 C21 139.5(3) . . . . ? Fe1 P1 C20 C21 -113.4(3) . . . . ? P2 P1 C20 C21 -175.7(3) . . . . ? C10 P1 C20 C25 -158.1(3) . . . . ? C8 P1 C20 C25 -47.5(3) . . . . ? Fe1 P1 C20 C25 59.5(3) . . . . ? P2 P1 C20 C25 -2.8(3) . . . . ? C25 C20 C21 C22 0.6(6) . . . . ? P1 C20 C21 C22 173.6(3) . . . . ? C20 C21 C22 C23 -0.4(7) . . . . ? C21 C22 C23 C24 0.0(7) . . . . ? C22 C23 C24 C25 0.1(7) . . . . ? C23 C24 C25 C20 0.1(6) . . . . ? C21 C20 C25 C24 -0.4(6) . . . . ? P1 C20 C25 C24 -173.6(3) . . . . ? C40 P2 C30 C35 110.7(3) . . . . ? C8 P2 C30 C35 -1.1(4) . . . . ? Fe1 P2 C30 C35 -112.8(3) . . . . ? P1 P2 C30 C35 -46.5(4) . . . . ? C40 P2 C30 C31 -67.9(3) . . . . ? C8 P2 C30 C31 -179.7(3) . . . . ? Fe1 P2 C30 C31 68.6(3) . . . . ? P1 P2 C30 C31 134.9(3) . . . . ? C35 C30 C31 C32 0.5(6) . . . . ? P2 C30 C31 C32 179.2(3) . . . . ? C30 C31 C32 C33 1.4(7) . . . . ? C31 C32 C33 C34 -1.9(8) . . . . ? C32 C33 C34 C35 0.4(8) . . . . ? C33 C34 C35 C30 1.6(7) . . . . ? C31 C30 C35 C34 -2.0(6) . . . . ? P2 C30 C35 C34 179.4(3) . . . . ? C30 P2 C40 C41 -75.1(3) . . . . ? C8 P2 C40 C41 37.5(4) . . . . ? Fe1 P2 C40 C41 144.4(3) . . . . ? P1 P2 C40 C41 79.9(3) . . . . ? C30 P2 C40 C45 97.4(3) . . . . ? C8 P2 C40 C45 -150.0(3) . . . . ? Fe1 P2 C40 C45 -43.0(3) . . . . ? P1 P2 C40 C45 -107.6(3) . . . . ? C45 C40 C41 C42 -0.2(6) . . . . ? P2 C40 C41 C42 172.3(3) . . . . ? C40 C41 C42 C43 -1.8(6) . . . . ? C41 C42 C43 C44 2.7(7) . . . . ? C42 C43 C44 C45 -1.6(7) . . . . ? C41 C40 C45 C44 1.4(6) . . . . ? P2 C40 C45 C44 -171.4(3) . . . . ? C43 C44 C45 C40 -0.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.633 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.074 data_str0432 _database_code_depnum_ccdc_archive 'CCDC 614638' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H41 Cl2 Fe2 O3 P3 S2' _chemical_formula_weight 921.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 9.4439(8) _cell_length_b 9.6258(9) _cell_length_c 22.437(2) _cell_angle_alpha 99.7830(10) _cell_angle_beta 95.331(2) _cell_angle_gamma 94.278(2) _cell_volume 1992.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 1.127 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8403 _exptl_absorpt_correction_T_max 0.9563 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17384 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9087 _reflns_number_gt 7520 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+0.9529P] 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 9087 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 0.13516(3) 0.76806(3) 0.319378(14) 0.01580(9) Uani 1 1 d . . . Fe2 Fe 0.08546(4) 0.89030(3) 0.229439(14) 0.01622(9) Uani 1 1 d . . . P1 P 0.08711(7) 0.68444(6) 0.40143(3) 0.01742(13) Uani 1 1 d . . . P2 P 0.15237(6) 0.54995(6) 0.27423(3) 0.01711(13) Uani 1 1 d . . . P3 P 0.03901(6) 0.73007(6) 0.14534(3) 0.01703(13) Uani 1 1 d . . . S1 S -0.08223(6) 0.75661(6) 0.26652(3) 0.01738(12) Uani 1 1 d . . . S2 S 0.12665(7) 1.00513(6) 0.32849(3) 0.02051(13) Uani 1 1 d . . . O1 O 0.43955(19) 0.8259(2) 0.35641(9) 0.0306(4) Uani 1 1 d . . . O2 O 0.3926(2) 0.9232(2) 0.22207(9) 0.0348(5) Uani 1 1 d . . . O3 O -0.0007(2) 1.1229(2) 0.17081(9) 0.0398(5) Uani 1 1 d . . . C1 C 0.3189(3) 0.8001(2) 0.34176(11) 0.0204(5) Uani 1 1 d . . . C2 C 0.2709(3) 0.9086(3) 0.22498(11) 0.0223(5) Uani 1 1 d . . . C3 C 0.0273(3) 1.0285(3) 0.19386(11) 0.0230(5) Uani 1 1 d . . . C4 C -0.2142(3) 0.8682(3) 0.29942(12) 0.0251(5) Uani 1 1 d . . . H4A H -0.3039 0.8493 0.2716 0.030 Uiso 1 1 calc R . . H4B H -0.2349 0.8397 0.3383 0.030 Uiso 1 1 calc R . . C5 C -0.1709(3) 1.0259(3) 0.31130(12) 0.0272(6) Uani 1 1 d . . . H5A H -0.1530 1.0561 0.2724 0.033 Uiso 1 1 calc R . . H5B H -0.2505 1.0768 0.3273 0.033 Uiso 1 1 calc R . . C6 C -0.0390(3) 1.0665(3) 0.35590(11) 0.0266(6) Uani 1 1 d . . . H6A H -0.0547 1.0280 0.3932 0.032 Uiso 1 1 calc R . . H6B H -0.0263 1.1710 0.3673 0.032 Uiso 1 1 calc R . . C7 C 0.1040(3) 0.4903(2) 0.38567(11) 0.0217(5) Uani 1 1 d . . . H7A H 0.2039 0.4717 0.3966 0.026 Uiso 1 1 calc R . . H7B H 0.0419 0.4419 0.4105 0.026 Uiso 1 1 calc R . . C8 C 0.0600(3) 0.4335(2) 0.31817(11) 0.0204(5) Uani 1 1 d . . . H8A H -0.0447 0.4323 0.3090 0.024 Uiso 1 1 calc R . . H8B H 0.0868 0.3356 0.3074 0.024 Uiso 1 1 calc R . . C9 C 0.0676(3) 0.4818(3) 0.19608(11) 0.0206(5) Uani 1 1 d . . . H9A H 0.0862 0.3813 0.1850 0.025 Uiso 1 1 calc R . . H9B H -0.0369 0.4848 0.1960 0.025 Uiso 1 1 calc R . . C10 C 0.1172(3) 0.5612(3) 0.14687(11) 0.0201(5) Uani 1 1 d . . . H10A H 0.0925 0.4994 0.1067 0.024 Uiso 1 1 calc R . . H10B H 0.2225 0.5799 0.1535 0.024 Uiso 1 1 calc R . . C11 C 0.2066(2) 0.7478(3) 0.47113(10) 0.0188(5) Uani 1 1 d . . . C12 C 0.2650(3) 0.8881(3) 0.48240(11) 0.0242(5) Uani 1 1 d . . . H12A H 0.2416 0.9476 0.4539 0.029 Uiso 1 1 calc R . . C13 C 0.3562(3) 0.9422(3) 0.53420(11) 0.0254(5) Uani 1 1 d . . . H13A H 0.3937 1.0386 0.5415 0.030 Uiso 1 1 calc R . . C14 C 0.3927(3) 0.8562(3) 0.57547(11) 0.0222(5) Uani 1 1 d . . . H14A H 0.4577 0.8925 0.6105 0.027 Uiso 1 1 calc R . . C15 C 0.3343(3) 0.7169(3) 0.56554(11) 0.0248(5) Uani 1 1 d . . . H15A H 0.3584 0.6580 0.5942 0.030 Uiso 1 1 calc R . . C16 C 0.2411(3) 0.6628(3) 0.51406(11) 0.0223(5) Uani 1 1 d . . . H16A H 0.2005 0.5675 0.5079 0.027 Uiso 1 1 calc R . . C17 C -0.0896(3) 0.6876(2) 0.42977(11) 0.0195(5) Uani 1 1 d . . . C18 C -0.2103(3) 0.6263(3) 0.39049(11) 0.0217(5) Uani 1 1 d . . . H18A H -0.1998 0.5861 0.3496 0.026 Uiso 1 1 calc R . . C19 C -0.3446(3) 0.6236(3) 0.41050(12) 0.0246(5) Uani 1 1 d . . . H19A H -0.4255 0.5819 0.3833 0.030 Uiso 1 1 calc R . . C20 C -0.3616(3) 0.6814(3) 0.46998(12) 0.0265(6) Uani 1 1 d . . . H20A H -0.4538 0.6790 0.4837 0.032 Uiso 1 1 calc R . . C21 C -0.2434(3) 0.7427(3) 0.50926(12) 0.0272(6) Uani 1 1 d . . . H21A H -0.2545 0.7820 0.5502 0.033 Uiso 1 1 calc R . . C22 C -0.1086(3) 0.7471(3) 0.48931(11) 0.0234(5) Uani 1 1 d . . . H22A H -0.0284 0.7911 0.5165 0.028 Uiso 1 1 calc R . . C23 C 0.3291(3) 0.4837(3) 0.26948(10) 0.0204(5) Uani 1 1 d . . . C24 C 0.4356(3) 0.5627(3) 0.24687(11) 0.0241(5) Uani 1 1 d . . . H24A H 0.4171 0.6520 0.2367 0.029 Uiso 1 1 calc R . . C25 C 0.5676(3) 0.5126(3) 0.23905(12) 0.0298(6) Uani 1 1 d . . . H25A H 0.6380 0.5667 0.2228 0.036 Uiso 1 1 calc R . . C26 C 0.5973(3) 0.3846(3) 0.25468(13) 0.0331(6) Uani 1 1 d . . . H26A H 0.6881 0.3507 0.2493 0.040 Uiso 1 1 calc R . . C27 C 0.4947(3) 0.3053(3) 0.27820(13) 0.0334(6) Uani 1 1 d . . . H27A H 0.5154 0.2176 0.2895 0.040 Uiso 1 1 calc R . . C28 C 0.3610(3) 0.3544(3) 0.28529(11) 0.0257(5) Uani 1 1 d . . . H28A H 0.2907 0.2992 0.3011 0.031 Uiso 1 1 calc R . . C29 C 0.0984(3) 0.7788(3) 0.07578(10) 0.0200(5) Uani 1 1 d . . . C30 C 0.0038(4) 0.7926(6) 0.02752(16) 0.0719(15) Uani 1 1 d . . . H30A H -0.0957 0.7739 0.0294 0.086 Uiso 1 1 calc R . . C31 C 0.0516(4) 0.8337(7) -0.02416(19) 0.0904(19) Uani 1 1 d . . . H31A H -0.0159 0.8419 -0.0572 0.108 Uiso 1 1 calc R . . C32 C 0.1923(3) 0.8623(4) -0.02822(13) 0.0389(7) Uani 1 1 d . . . H32A H 0.2239 0.8913 -0.0636 0.047 Uiso 1 1 calc R . . C33 C 0.2881(3) 0.8487(4) 0.01921(13) 0.0395(7) Uani 1 1 d . . . H33A H 0.3875 0.8670 0.0169 0.047 Uiso 1 1 calc R . . C34 C 0.2406(3) 0.8082(4) 0.07094(13) 0.0397(8) Uani 1 1 d . . . H34A H 0.3086 0.8007 0.1039 0.048 Uiso 1 1 calc R . . C35 C -0.1510(3) 0.6762(3) 0.12117(10) 0.0196(5) Uani 1 1 d . . . C36 C -0.2490(3) 0.7756(3) 0.13237(12) 0.0254(5) Uani 1 1 d . . . H36A H -0.2172 0.8682 0.1536 0.030 Uiso 1 1 calc R . . C37 C -0.3931(3) 0.7406(3) 0.11272(13) 0.0312(6) Uani 1 1 d . . . H37A H -0.4590 0.8099 0.1198 0.037 Uiso 1 1 calc R . . C38 C -0.4406(3) 0.6062(3) 0.08309(13) 0.0336(6) Uani 1 1 d . . . H38A H -0.5393 0.5822 0.0701 0.040 Uiso 1 1 calc R . . C39 C -0.3451(3) 0.5065(3) 0.07225(13) 0.0352(7) Uani 1 1 d . . . H39A H -0.3784 0.4132 0.0522 0.042 Uiso 1 1 calc R . . C40 C -0.2004(3) 0.5408(3) 0.09038(12) 0.0282(6) Uani 1 1 d . . . H40A H -0.1349 0.4717 0.0818 0.034 Uiso 1 1 calc R . . C41 C 0.3661(4) 0.1912(5) 0.12401(17) 0.0640(11) Uani 1 1 d . . . H41A H 0.2905 0.1144 0.1244 0.077 Uiso 1 1 calc R . . H41B H 0.3658 0.2624 0.1614 0.077 Uiso 1 1 calc R . . Cl1 Cl 0.53156(9) 0.12141(10) 0.12418(4) 0.0513(2) Uani 1 1 d . . . Cl2 Cl 0.32746(11) 0.27003(12) 0.06063(6) 0.0759(3) 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 0.01918(18) 0.01477(16) 0.01276(16) 0.00378(12) -0.00172(12) -0.00167(12) Fe2 0.01958(18) 0.01635(17) 0.01244(16) 0.00408(13) -0.00026(12) -0.00116(13) P1 0.0217(3) 0.0163(3) 0.0136(3) 0.0043(2) -0.0016(2) -0.0021(2) P2 0.0202(3) 0.0156(3) 0.0150(3) 0.0038(2) -0.0012(2) -0.0003(2) P3 0.0177(3) 0.0197(3) 0.0135(3) 0.0036(2) -0.0003(2) 0.0007(2) S1 0.0189(3) 0.0181(3) 0.0150(3) 0.0044(2) -0.0001(2) -0.0003(2) S2 0.0294(3) 0.0159(3) 0.0150(3) 0.0027(2) -0.0005(2) -0.0020(2) O1 0.0238(10) 0.0319(10) 0.0325(10) 0.0022(8) -0.0053(8) -0.0024(8) O2 0.0251(11) 0.0463(12) 0.0343(11) 0.0128(9) 0.0051(8) -0.0040(9) O3 0.0633(15) 0.0262(10) 0.0316(11) 0.0150(9) -0.0034(10) 0.0026(10) C1 0.0270(13) 0.0163(11) 0.0175(11) 0.0039(9) 0.0004(10) 0.0003(9) C2 0.0290(14) 0.0213(12) 0.0152(11) 0.0026(9) 0.0000(10) -0.0026(10) C3 0.0302(14) 0.0206(12) 0.0170(11) 0.0028(10) -0.0002(10) -0.0008(10) C4 0.0216(13) 0.0293(14) 0.0269(13) 0.0076(11) 0.0068(10) 0.0072(10) C5 0.0343(15) 0.0268(14) 0.0243(13) 0.0072(11) 0.0104(11) 0.0114(11) C6 0.0429(16) 0.0202(12) 0.0179(12) 0.0014(10) 0.0103(11) 0.0058(11) C7 0.0271(13) 0.0185(12) 0.0203(12) 0.0074(10) 0.0013(10) -0.0001(10) C8 0.0250(13) 0.0165(11) 0.0190(11) 0.0032(9) 0.0016(9) -0.0017(9) C9 0.0241(13) 0.0173(12) 0.0182(11) 0.0009(9) -0.0035(9) -0.0001(9) C10 0.0212(12) 0.0232(12) 0.0157(11) 0.0029(9) -0.0005(9) 0.0038(10) C11 0.0194(12) 0.0215(12) 0.0147(11) 0.0039(9) -0.0007(9) -0.0010(9) C12 0.0329(14) 0.0211(12) 0.0181(12) 0.0057(10) -0.0020(10) -0.0012(10) C13 0.0321(14) 0.0205(13) 0.0211(12) 0.0011(10) -0.0003(10) -0.0042(10) C14 0.0216(12) 0.0282(13) 0.0147(11) 0.0016(10) -0.0015(9) -0.0023(10) C15 0.0297(14) 0.0268(13) 0.0186(12) 0.0086(10) -0.0032(10) 0.0034(11) C16 0.0275(13) 0.0200(12) 0.0195(12) 0.0065(10) 0.0001(10) -0.0016(10) C17 0.0238(12) 0.0172(11) 0.0186(11) 0.0080(9) 0.0006(9) 0.0007(9) C18 0.0260(13) 0.0223(12) 0.0171(11) 0.0069(10) 0.0001(10) -0.0016(10) C19 0.0234(13) 0.0227(13) 0.0277(13) 0.0081(11) -0.0014(10) -0.0005(10) C20 0.0253(13) 0.0253(13) 0.0322(14) 0.0100(11) 0.0076(11) 0.0073(10) C21 0.0350(15) 0.0243(13) 0.0235(13) 0.0043(10) 0.0056(11) 0.0075(11) C22 0.0300(14) 0.0197(12) 0.0193(12) 0.0023(10) -0.0012(10) 0.0024(10) C23 0.0231(12) 0.0214(12) 0.0154(11) 0.0015(9) -0.0025(9) 0.0028(10) C24 0.0252(13) 0.0242(13) 0.0211(12) 0.0029(10) -0.0036(10) 0.0013(10) C25 0.0232(13) 0.0358(15) 0.0271(14) -0.0004(12) -0.0004(11) -0.0018(11) C26 0.0283(15) 0.0365(16) 0.0306(15) -0.0036(12) -0.0052(11) 0.0094(12) C27 0.0378(16) 0.0302(15) 0.0315(15) 0.0048(12) -0.0059(12) 0.0123(12) C28 0.0302(14) 0.0241(13) 0.0229(13) 0.0056(10) 0.0000(10) 0.0033(11) C29 0.0230(12) 0.0218(12) 0.0157(11) 0.0039(9) 0.0034(9) 0.0028(10) C30 0.0240(17) 0.162(5) 0.045(2) 0.068(3) 0.0006(14) 0.000(2) C31 0.038(2) 0.202(6) 0.055(2) 0.089(3) 0.0029(18) 0.013(3) C32 0.0383(17) 0.057(2) 0.0284(15) 0.0212(14) 0.0129(13) 0.0085(15) C33 0.0270(15) 0.065(2) 0.0263(14) 0.0104(14) 0.0076(12) -0.0067(14) C34 0.0226(14) 0.076(2) 0.0210(14) 0.0140(14) -0.0016(11) -0.0015(14) C35 0.0200(12) 0.0253(13) 0.0133(11) 0.0052(9) 0.0002(9) -0.0017(9) C36 0.0250(13) 0.0239(13) 0.0252(13) 0.0031(10) -0.0037(10) 0.0003(10) C37 0.0231(14) 0.0373(16) 0.0330(15) 0.0058(12) -0.0012(11) 0.0074(11) C38 0.0222(14) 0.0424(17) 0.0337(15) 0.0068(13) -0.0052(11) -0.0036(12) C39 0.0316(15) 0.0313(15) 0.0367(16) -0.0005(13) -0.0082(12) -0.0069(12) C40 0.0272(14) 0.0266(14) 0.0279(14) 0.0004(11) -0.0026(11) 0.0004(11) C41 0.045(2) 0.107(4) 0.041(2) 0.009(2) 0.0106(16) 0.016(2) Cl1 0.0481(5) 0.0584(5) 0.0507(5) 0.0115(4) 0.0149(4) 0.0103(4) Cl2 0.0570(6) 0.0723(7) 0.0973(9) 0.0368(6) -0.0205(6) -0.0151(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 1.750(3) . ? Fe1 P2 2.1953(7) . ? Fe1 P1 2.2016(7) . ? Fe1 S1 2.2589(7) . ? Fe1 S2 2.2644(7) . ? Fe1 Fe2 2.5279(5) . ? Fe2 C3 1.760(3) . ? Fe2 C2 1.761(3) . ? Fe2 P3 2.2109(7) . ? Fe2 S1 2.2718(7) . ? Fe2 S2 2.2918(7) . ? P1 C11 1.827(2) . ? P1 C17 1.841(3) . ? P1 C7 1.863(2) . ? P2 C23 1.836(2) . ? P2 C8 1.838(2) . ? P2 C9 1.848(2) . ? P3 C29 1.828(2) . ? P3 C35 1.835(2) . ? P3 C10 1.839(2) . ? S1 C4 1.831(2) . ? S2 C6 1.835(3) . ? O1 C1 1.153(3) . ? O2 C2 1.156(3) . ? O3 C3 1.155(3) . ? C4 C5 1.515(4) . ? C5 C6 1.506(4) . ? C7 C8 1.528(3) . ? C9 C10 1.534(3) . ? C11 C12 1.392(3) . ? C11 C16 1.397(3) . ? C12 C13 1.380(3) . ? C13 C14 1.380(4) . ? C14 C15 1.385(4) . ? C15 C16 1.385(3) . ? C17 C22 1.394(3) . ? C17 C18 1.400(3) . ? C18 C19 1.384(4) . ? C19 C20 1.385(4) . ? C20 C21 1.383(4) . ? C21 C22 1.388(4) . ? C23 C28 1.397(3) . ? C23 C24 1.400(4) . ? C24 C25 1.385(4) . ? C25 C26 1.378(4) . ? C26 C27 1.386(4) . ? C27 C28 1.394(4) . ? C29 C30 1.369(4) . ? C29 C34 1.370(4) . ? C30 C31 1.390(4) . ? C31 C32 1.351(5) . ? C32 C33 1.361(4) . ? C33 C34 1.387(4) . ? C35 C36 1.388(4) . ? C35 C40 1.392(4) . ? C36 C37 1.390(4) . ? C37 C38 1.371(4) . ? C38 C39 1.373(4) . ? C39 C40 1.388(4) . ? C41 Cl2 1.744(4) . ? C41 Cl1 1.747(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 P2 93.26(8) . . ? C1 Fe1 P1 94.47(8) . . ? P2 Fe1 P1 88.37(3) . . ? C1 Fe1 S1 162.54(8) . . ? P2 Fe1 S1 88.13(2) . . ? P1 Fe1 S1 102.97(3) . . ? C1 Fe1 S2 87.99(8) . . ? P2 Fe1 S2 157.61(3) . . ? P1 Fe1 S2 113.84(3) . . ? S1 Fe1 S2 84.24(2) . . ? C1 Fe1 Fe2 106.46(8) . . ? P2 Fe1 Fe2 101.66(2) . . ? P1 Fe1 Fe2 156.05(2) . . ? S1 Fe1 Fe2 56.328(18) . . ? S2 Fe1 Fe2 56.820(18) . . ? C3 Fe2 C2 101.97(12) . . ? C3 Fe2 P3 93.47(8) . . ? C2 Fe2 P3 94.58(8) . . ? C3 Fe2 S1 117.39(9) . . ? C2 Fe2 S1 140.62(8) . . ? P3 Fe2 S1 84.90(2) . . ? C3 Fe2 S2 100.30(8) . . ? C2 Fe2 S2 88.60(8) . . ? P3 Fe2 S2 164.92(3) . . ? S1 Fe2 S2 83.33(2) . . ? C3 Fe2 Fe1 154.24(8) . . ? C2 Fe2 Fe1 88.00(8) . . ? P3 Fe2 Fe1 109.52(2) . . ? S1 Fe2 Fe1 55.846(18) . . ? S2 Fe2 Fe1 55.787(19) . . ? C11 P1 C17 101.93(11) . . ? C11 P1 C7 103.86(11) . . ? C17 P1 C7 100.77(11) . . ? C11 P1 Fe1 117.57(8) . . ? C17 P1 Fe1 122.77(8) . . ? C7 P1 Fe1 107.32(8) . . ? C23 P2 C8 104.10(11) . . ? C23 P2 C9 100.61(11) . . ? C8 P2 C9 101.86(11) . . ? C23 P2 Fe1 119.72(8) . . ? C8 P2 Fe1 106.59(8) . . ? C9 P2 Fe1 121.47(8) . . ? C29 P3 C35 101.09(11) . . ? C29 P3 C10 101.80(11) . . ? C35 P3 C10 103.61(11) . . ? C29 P3 Fe2 116.95(8) . . ? C35 P3 Fe2 115.42(8) . . ? C10 P3 Fe2 115.78(8) . . ? C4 S1 Fe1 118.18(9) . . ? C4 S1 Fe2 110.07(9) . . ? Fe1 S1 Fe2 67.83(2) . . ? C6 S2 Fe1 113.31(9) . . ? C6 S2 Fe2 110.68(9) . . ? Fe1 S2 Fe2 67.39(2) . . ? O1 C1 Fe1 177.7(2) . . ? O2 C2 Fe2 178.8(2) . . ? O3 C3 Fe2 175.1(2) . . ? C5 C4 S1 115.39(18) . . ? C6 C5 C4 112.5(2) . . ? C5 C6 S2 115.23(17) . . ? C8 C7 P1 109.18(16) . . ? C7 C8 P2 108.04(16) . . ? C10 C9 P2 115.67(17) . . ? C9 C10 P3 114.16(16) . . ? C12 C11 C16 118.3(2) . . ? C12 C11 P1 118.42(18) . . ? C16 C11 P1 123.24(18) . . ? C13 C12 C11 121.2(2) . . ? C12 C13 C14 120.0(2) . . ? C13 C14 C15 119.7(2) . . ? C14 C15 C16 120.4(2) . . ? C15 C16 C11 120.3(2) . . ? C22 C17 C18 118.3(2) . . ? C22 C17 P1 122.67(19) . . ? C18 C17 P1 119.04(18) . . ? C19 C18 C17 120.8(2) . . ? C18 C19 C20 120.3(2) . . ? C21 C20 C19 119.5(2) . . ? C20 C21 C22 120.4(2) . . ? C21 C22 C17 120.6(2) . . ? C28 C23 C24 118.0(2) . . ? C28 C23 P2 122.9(2) . . ? C24 C23 P2 119.05(18) . . ? C25 C24 C23 121.0(2) . . ? C26 C25 C24 120.3(3) . . ? C25 C26 C27 120.0(3) . . ? C26 C27 C28 119.9(3) . . ? C27 C28 C23 120.8(3) . . ? C30 C29 C34 117.2(2) . . ? C30 C29 P3 122.0(2) . . ? C34 C29 P3 120.77(19) . . ? C29 C30 C31 120.8(3) . . ? C32 C31 C30 121.2(3) . . ? C31 C32 C33 118.9(3) . . ? C32 C33 C34 120.0(3) . . ? C29 C34 C33 121.8(3) . . ? C36 C35 C40 118.6(2) . . ? C36 C35 P3 118.75(19) . . ? C40 C35 P3 122.6(2) . . ? C35 C36 C37 120.5(2) . . ? C38 C37 C36 120.2(3) . . ? C37 C38 C39 119.9(3) . . ? C38 C39 C40 120.6(3) . . ? C39 C40 C35 120.2(3) . . ? Cl2 C41 Cl1 112.1(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Fe1 Fe2 C3 -100.5(2) . . . . ? P2 Fe1 Fe2 C3 162.5(2) . . . . ? P1 Fe1 Fe2 C3 49.4(2) . . . . ? S1 Fe1 Fe2 C3 82.7(2) . . . . ? S2 Fe1 Fe2 C3 -24.2(2) . . . . ? C1 Fe1 Fe2 C2 13.37(11) . . . . ? P2 Fe1 Fe2 C2 -83.61(8) . . . . ? P1 Fe1 Fe2 C2 163.26(10) . . . . ? S1 Fe1 Fe2 C2 -163.39(8) . . . . ? S2 Fe1 Fe2 C2 89.66(8) . . . . ? C1 Fe1 Fe2 P3 107.52(8) . . . . ? P2 Fe1 Fe2 P3 10.55(3) . . . . ? P1 Fe1 Fe2 P3 -102.58(6) . . . . ? S1 Fe1 Fe2 P3 -69.23(3) . . . . ? S2 Fe1 Fe2 P3 -176.18(3) . . . . ? C1 Fe1 Fe2 S1 176.76(8) . . . . ? P2 Fe1 Fe2 S1 79.78(3) . . . . ? P1 Fe1 Fe2 S1 -33.35(6) . . . . ? S2 Fe1 Fe2 S1 -106.94(3) . . . . ? C1 Fe1 Fe2 S2 -76.30(8) . . . . ? P2 Fe1 Fe2 S2 -173.27(3) . . . . ? P1 Fe1 Fe2 S2 73.59(6) . . . . ? S1 Fe1 Fe2 S2 106.94(3) . . . . ? C1 Fe1 P1 C11 27.65(12) . . . . ? P2 Fe1 P1 C11 120.79(9) . . . . ? S1 Fe1 P1 C11 -151.50(9) . . . . ? S2 Fe1 P1 C11 -62.12(10) . . . . ? Fe2 Fe1 P1 C11 -123.50(10) . . . . ? C1 Fe1 P1 C17 155.49(12) . . . . ? P2 Fe1 P1 C17 -111.37(10) . . . . ? S1 Fe1 P1 C17 -23.66(10) . . . . ? S2 Fe1 P1 C17 65.71(10) . . . . ? Fe2 Fe1 P1 C17 4.34(12) . . . . ? C1 Fe1 P1 C7 -88.82(12) . . . . ? P2 Fe1 P1 C7 4.32(9) . . . . ? S1 Fe1 P1 C7 92.03(9) . . . . ? S2 Fe1 P1 C7 -178.59(9) . . . . ? Fe2 Fe1 P1 C7 120.03(10) . . . . ? C1 Fe1 P2 C23 -4.19(12) . . . . ? P1 Fe1 P2 C23 -98.57(9) . . . . ? S1 Fe1 P2 C23 158.39(9) . . . . ? S2 Fe1 P2 C23 88.44(11) . . . . ? Fe2 Fe1 P2 C23 103.36(9) . . . . ? C1 Fe1 P2 C8 113.37(12) . . . . ? P1 Fe1 P2 C8 18.99(9) . . . . ? S1 Fe1 P2 C8 -84.05(9) . . . . ? S2 Fe1 P2 C8 -154.00(10) . . . . ? Fe2 Fe1 P2 C8 -139.08(8) . . . . ? C1 Fe1 P2 C9 -130.92(12) . . . . ? P1 Fe1 P2 C9 134.70(10) . . . . ? S1 Fe1 P2 C9 31.66(10) . . . . ? S2 Fe1 P2 C9 -38.29(13) . . . . ? Fe2 Fe1 P2 C9 -23.37(10) . . . . ? C3 Fe2 P3 C29 45.92(12) . . . . ? C2 Fe2 P3 C29 -56.39(12) . . . . ? S1 Fe2 P3 C29 163.13(9) . . . . ? S2 Fe2 P3 C29 -158.12(12) . . . . ? Fe1 Fe2 P3 C29 -145.89(9) . . . . ? C3 Fe2 P3 C35 -72.79(12) . . . . ? C2 Fe2 P3 C35 -175.11(12) . . . . ? S1 Fe2 P3 C35 44.42(9) . . . . ? S2 Fe2 P3 C35 83.16(14) . . . . ? Fe1 Fe2 P3 C35 95.39(9) . . . . ? C3 Fe2 P3 C10 165.94(12) . . . . ? C2 Fe2 P3 C10 63.63(12) . . . . ? S1 Fe2 P3 C10 -76.85(9) . . . . ? S2 Fe2 P3 C10 -38.10(15) . . . . ? Fe1 Fe2 P3 C10 -25.87(9) . . . . ? C1 Fe1 S1 C4 -112.1(3) . . . . ? P2 Fe1 S1 C4 152.99(10) . . . . ? P1 Fe1 S1 C4 65.10(10) . . . . ? S2 Fe1 S1 C4 -48.08(10) . . . . ? Fe2 Fe1 S1 C4 -101.66(10) . . . . ? C1 Fe1 S1 Fe2 -10.4(3) . . . . ? P2 Fe1 S1 Fe2 -105.34(2) . . . . ? P1 Fe1 S1 Fe2 166.76(2) . . . . ? S2 Fe1 S1 Fe2 53.58(2) . . . . ? C3 Fe2 S1 C4 -37.76(13) . . . . ? C2 Fe2 S1 C4 139.96(15) . . . . ? P3 Fe2 S1 C4 -129.03(9) . . . . ? S2 Fe2 S1 C4 60.41(9) . . . . ? Fe1 Fe2 S1 C4 113.20(9) . . . . ? C3 Fe2 S1 Fe1 -150.96(9) . . . . ? C2 Fe2 S1 Fe1 26.76(13) . . . . ? P3 Fe2 S1 Fe1 117.77(2) . . . . ? S2 Fe2 S1 Fe1 -52.79(2) . . . . ? C1 Fe1 S2 C6 -145.08(12) . . . . ? P2 Fe1 S2 C6 121.25(11) . . . . ? P1 Fe1 S2 C6 -51.09(10) . . . . ? S1 Fe1 S2 C6 50.57(9) . . . . ? Fe2 Fe1 S2 C6 103.72(9) . . . . ? C1 Fe1 S2 Fe2 111.20(8) . . . . ? P2 Fe1 S2 Fe2 17.53(8) . . . . ? P1 Fe1 S2 Fe2 -154.80(3) . . . . ? S1 Fe1 S2 Fe2 -53.14(2) . . . . ? C3 Fe2 S2 C6 62.04(13) . . . . ? C2 Fe2 S2 C6 163.94(12) . . . . ? P3 Fe2 S2 C6 -93.55(14) . . . . ? S1 Fe2 S2 C6 -54.67(9) . . . . ? Fe1 Fe2 S2 C6 -107.52(9) . . . . ? C3 Fe2 S2 Fe1 169.56(9) . . . . ? C2 Fe2 S2 Fe1 -88.54(8) . . . . ? P3 Fe2 S2 Fe1 13.97(11) . . . . ? S1 Fe2 S2 Fe1 52.85(2) . . . . ? P2 Fe1 C1 O1 151(6) . . . . ? P1 Fe1 C1 O1 -120(6) . . . . ? S1 Fe1 C1 O1 57(6) . . . . ? S2 Fe1 C1 O1 -7(6) . . . . ? Fe2 Fe1 C1 O1 48(6) . . . . ? C3 Fe2 C2 O2 29(10) . . . . ? P3 Fe2 C2 O2 123(10) . . . . ? S1 Fe2 C2 O2 -149(10) . . . . ? S2 Fe2 C2 O2 -71(10) . . . . ? Fe1 Fe2 C2 O2 -127(10) . . . . ? C2 Fe2 C3 O3 -13(3) . . . . ? P3 Fe2 C3 O3 -108(3) . . . . ? S1 Fe2 C3 O3 166(3) . . . . ? S2 Fe2 C3 O3 78(3) . . . . ? Fe1 Fe2 C3 O3 98(3) . . . . ? Fe1 S1 C4 C5 59.7(2) . . . . ? Fe2 S1 C4 C5 -15.2(2) . . . . ? S1 C4 C5 C6 -61.2(3) . . . . ? C4 C5 C6 S2 68.2(3) . . . . ? Fe1 S2 C6 C5 -70.5(2) . . . . ? Fe2 S2 C6 C5 2.9(2) . . . . ? C11 P1 C7 C8 -157.57(17) . . . . ? C17 P1 C7 C8 97.14(18) . . . . ? Fe1 P1 C7 C8 -32.39(18) . . . . ? P1 C7 C8 P2 48.2(2) . . . . ? C23 P2 C8 C7 83.58(18) . . . . ? C9 P2 C8 C7 -172.14(17) . . . . ? Fe1 P2 C8 C7 -43.88(18) . . . . ? C23 P2 C9 C10 -75.29(19) . . . . ? C8 P2 C9 C10 177.70(18) . . . . ? Fe1 P2 C9 C10 59.6(2) . . . . ? P2 C9 C10 P3 -77.6(2) . . . . ? C29 P3 C10 C9 -171.62(17) . . . . ? C35 P3 C10 C9 -66.98(19) . . . . ? Fe2 P3 C10 C9 60.42(19) . . . . ? C17 P1 C11 C12 -101.5(2) . . . . ? C7 P1 C11 C12 154.1(2) . . . . ? Fe1 P1 C11 C12 35.8(2) . . . . ? C17 P1 C11 C16 77.8(2) . . . . ? C7 P1 C11 C16 -26.6(2) . . . . ? Fe1 P1 C11 C16 -144.97(19) . . . . ? C16 C11 C12 C13 0.8(4) . . . . ? P1 C11 C12 C13 -179.9(2) . . . . ? C11 C12 C13 C14 1.0(4) . . . . ? C12 C13 C14 C15 -1.9(4) . . . . ? C13 C14 C15 C16 0.9(4) . . . . ? C14 C15 C16 C11 0.9(4) . . . . ? C12 C11 C16 C15 -1.8(4) . . . . ? P1 C11 C16 C15 179.0(2) . . . . ? C11 P1 C17 C22 8.2(2) . . . . ? C7 P1 C17 C22 115.0(2) . . . . ? Fe1 P1 C17 C22 -126.13(18) . . . . ? C11 P1 C17 C18 -170.94(19) . . . . ? C7 P1 C17 C18 -64.1(2) . . . . ? Fe1 P1 C17 C18 54.7(2) . . . . ? C22 C17 C18 C19 -0.7(4) . . . . ? P1 C17 C18 C19 178.49(18) . . . . ? C17 C18 C19 C20 -0.2(4) . . . . ? C18 C19 C20 C21 0.4(4) . . . . ? C19 C20 C21 C22 0.3(4) . . . . ? C20 C21 C22 C17 -1.2(4) . . . . ? C18 C17 C22 C21 1.4(4) . . . . ? P1 C17 C22 C21 -177.76(19) . . . . ? C8 P2 C23 C28 12.4(2) . . . . ? C9 P2 C23 C28 -92.8(2) . . . . ? Fe1 P2 C23 C28 131.25(19) . . . . ? C8 P2 C23 C24 -170.14(19) . . . . ? C9 P2 C23 C24 84.6(2) . . . . ? Fe1 P2 C23 C24 -51.3(2) . . . . ? C28 C23 C24 C25 1.5(4) . . . . ? P2 C23 C24 C25 -176.07(19) . . . . ? C23 C24 C25 C26 -1.3(4) . . . . ? C24 C25 C26 C27 0.2(4) . . . . ? C25 C26 C27 C28 0.8(4) . . . . ? C26 C27 C28 C23 -0.6(4) . . . . ? C24 C23 C28 C27 -0.5(4) . . . . ? P2 C23 C28 C27 176.9(2) . . . . ? C35 P3 C29 C30 11.3(3) . . . . ? C10 P3 C29 C30 117.9(3) . . . . ? Fe2 P3 C29 C30 -114.9(3) . . . . ? C35 P3 C29 C34 -171.2(2) . . . . ? C10 P3 C29 C34 -64.6(3) . . . . ? Fe2 P3 C29 C34 62.6(3) . . . . ? C34 C29 C30 C31 0.5(7) . . . . ? P3 C29 C30 C31 178.1(4) . . . . ? C29 C30 C31 C32 -0.5(9) . . . . ? C30 C31 C32 C33 0.7(8) . . . . ? C31 C32 C33 C34 -0.9(6) . . . . ? C30 C29 C34 C33 -0.8(5) . . . . ? P3 C29 C34 C33 -178.4(3) . . . . ? C32 C33 C34 C29 1.0(5) . . . . ? C29 P3 C35 C36 -93.9(2) . . . . ? C10 P3 C35 C36 160.90(19) . . . . ? Fe2 P3 C35 C36 33.3(2) . . . . ? C29 P3 C35 C40 84.1(2) . . . . ? C10 P3 C35 C40 -21.1(2) . . . . ? Fe2 P3 C35 C40 -148.74(19) . . . . ? C40 C35 C36 C37 -0.6(4) . . . . ? P3 C35 C36 C37 177.5(2) . . . . ? C35 C36 C37 C38 1.4(4) . . . . ? C36 C37 C38 C39 -0.7(4) . . . . ? C37 C38 C39 C40 -0.8(5) . . . . ? C38 C39 C40 C35 1.6(4) . . . . ? C36 C35 C40 C39 -0.9(4) . . . . ? P3 C35 C40 C39 -178.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.659 _refine_diff_density_min -1.013 _refine_diff_density_rms 0.081 #===END data_str0540 _database_code_depnum_ccdc_archive 'CCDC 639866' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H33 Fe2 N O4 P2 S2' _chemical_formula_weight 757.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p_-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7227(10) _cell_length_b 10.3859(11) _cell_length_c 18.5263(19) _cell_angle_alpha 84.913(2) _cell_angle_beta 80.645(2) _cell_angle_gamma 63.569(2) _cell_volume 1652.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 1.141 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7714 _exptl_absorpt_correction_T_max 0.8566 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14333 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 28.31 _reflns_number_total 7563 _reflns_number_gt 6917 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+2.8501P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7563 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.1095 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.51744(4) 0.36202(3) 0.272386(17) 0.01089(9) Uani 1 1 d . . . Fe2 Fe 0.44438(4) 0.27286(4) 0.403438(18) 0.01320(9) Uani 1 1 d . . . P1 P 0.77021(7) 0.29495(6) 0.24932(3) 0.01170(12) Uani 1 1 d . . . P2 P 0.62387(7) 0.17397(6) 0.19995(3) 0.01232(13) Uani 1 1 d . . . S1 S 0.29936(7) 0.34150(6) 0.31094(3) 0.01587(13) Uani 1 1 d . . . S2 S 0.47348(7) 0.47571(6) 0.37575(3) 0.01588(13) Uani 1 1 d . . . N1 N 0.8103(2) 0.1518(2) 0.19667(11) 0.0148(4) Uani 1 1 d . . . O1 O 0.3750(2) 0.6158(2) 0.18172(10) 0.0232(4) Uani 1 1 d . . . O2 O 0.2227(2) 0.3484(2) 0.53867(11) 0.0288(4) Uani 1 1 d . . . O3 O 0.7204(3) 0.1534(3) 0.47764(13) 0.0345(5) Uani 1 1 d . . . O4 O 0.4666(3) -0.0185(2) 0.40865(11) 0.0270(4) Uani 1 1 d . . . C1 C 0.4404(3) 0.5110(3) 0.21455(13) 0.0146(4) Uani 1 1 d . . . C2 C 0.3075(3) 0.3215(3) 0.48557(13) 0.0178(5) Uani 1 1 d . . . C3 C 0.6167(3) 0.2016(3) 0.44650(14) 0.0212(5) Uani 1 1 d . . . C4 C 0.4596(3) 0.0941(3) 0.40197(13) 0.0174(5) Uani 1 1 d . . . C5 C 0.1388(3) 0.5205(3) 0.3247(2) 0.0318(7) Uani 1 1 d . . . H5A H 0.1364 0.5759 0.2782 0.038 Uiso 1 1 calc R . . H5B H 0.0411 0.5098 0.3345 0.038 Uiso 1 1 calc R . . C6 C 0.1392(4) 0.6052(4) 0.3825(2) 0.0379(7) Uani 1 1 d . . . H6A H 0.1224 0.5580 0.4296 0.045 Uiso 1 1 calc R . . H6B H 0.0484 0.7002 0.3811 0.045 Uiso 1 1 calc R . . C7 C 0.2825(3) 0.6322(3) 0.38309(17) 0.0287(6) Uani 1 1 d . . . H7A H 0.2677 0.6816 0.4290 0.034 Uiso 1 1 calc R . . H7B H 0.2849 0.6996 0.3422 0.034 Uiso 1 1 calc R . . C8 C 0.9547(3) 0.0757(3) 0.14429(15) 0.0287(6) Uani 1 1 d . . . H8A H 1.0362 0.0888 0.1651 0.034 Uiso 1 1 calc R . . C9 C 0.9512(3) 0.1483(3) 0.06958(14) 0.0222(5) Uani 1 1 d . . . H9A H 1.0488 0.0939 0.0381 0.033 Uiso 1 1 calc R . . H9B H 0.9381 0.2464 0.0746 0.033 Uiso 1 1 calc R . . H9C H 0.8645 0.1517 0.0476 0.033 Uiso 1 1 calc R . . C10 C 1.0131(4) -0.0809(4) 0.1419(2) 0.0435(8) Uani 1 1 d . . . H10A H 1.0128 -0.1205 0.1919 0.065 Uiso 1 1 calc R . . H10B H 1.1192 -0.1229 0.1160 0.065 Uiso 1 1 calc R . . H10C H 0.9464 -0.1038 0.1163 0.065 Uiso 1 1 calc R . . C11 C 0.8607(3) 0.3998(3) 0.19396(13) 0.0152(4) Uani 1 1 d . . . C12 C 1.0157(3) 0.3696(3) 0.19598(15) 0.0228(5) Uani 1 1 d . . . H12A H 1.0729 0.2993 0.2297 0.027 Uiso 1 1 calc R . . C13 C 1.0862(3) 0.4415(4) 0.14912(16) 0.0307(7) Uani 1 1 d . . . H13A H 1.1915 0.4194 0.1507 0.037 Uiso 1 1 calc R . . C14 C 1.0040(4) 0.5451(4) 0.10003(16) 0.0303(6) Uani 1 1 d . . . H14A H 1.0526 0.5944 0.0683 0.036 Uiso 1 1 calc R . . C15 C 0.8503(4) 0.5766(3) 0.09744(16) 0.0276(6) Uani 1 1 d . . . H15A H 0.7934 0.6473 0.0638 0.033 Uiso 1 1 calc R . . C16 C 0.7800(3) 0.5044(3) 0.14412(14) 0.0208(5) Uani 1 1 d . . . H16A H 0.6747 0.5266 0.1421 0.025 Uiso 1 1 calc R . . C17 C 0.8908(3) 0.2296(3) 0.32218(13) 0.0146(4) Uani 1 1 d . . . C18 C 0.9848(4) 0.0857(3) 0.33491(17) 0.0285(6) Uani 1 1 d . . . H18A H 0.9889 0.0149 0.3044 0.034 Uiso 1 1 calc R . . C19 C 1.0729(4) 0.0444(3) 0.39202(18) 0.0335(7) Uani 1 1 d . . . H19A H 1.1375 -0.0546 0.4002 0.040 Uiso 1 1 calc R . . C20 C 1.0675(3) 0.1466(3) 0.43731(15) 0.0226(5) Uani 1 1 d . . . H20A H 1.1277 0.1180 0.4765 0.027 Uiso 1 1 calc R . . C21 C 0.9739(3) 0.2904(3) 0.42483(13) 0.0171(5) Uani 1 1 d . . . H21A H 0.9701 0.3608 0.4555 0.020 Uiso 1 1 calc R . . C22 C 0.8852(3) 0.3326(3) 0.36783(13) 0.0147(4) Uani 1 1 d . . . H22A H 0.8207 0.4317 0.3598 0.018 Uiso 1 1 calc R . . C23 C 0.5890(3) 0.1809(3) 0.10479(13) 0.0155(5) Uani 1 1 d . . . C24 C 0.6396(3) 0.0560(3) 0.06480(14) 0.0195(5) Uani 1 1 d . . . H24A H 0.6860 -0.0355 0.0881 0.023 Uiso 1 1 calc R . . C25 C 0.6225(3) 0.0646(3) -0.00891(14) 0.0220(5) Uani 1 1 d . . . H25A H 0.6591 -0.0210 -0.0357 0.026 Uiso 1 1 calc R . . C26 C 0.5525(4) 0.1969(3) -0.04319(14) 0.0258(6) Uani 1 1 d . . . H26A H 0.5407 0.2025 -0.0934 0.031 Uiso 1 1 calc R . . C27 C 0.4997(4) 0.3210(3) -0.00392(15) 0.0278(6) Uani 1 1 d . . . H27A H 0.4507 0.4121 -0.0273 0.033 Uiso 1 1 calc R . . C28 C 0.5178(3) 0.3137(3) 0.06962(14) 0.0211(5) Uani 1 1 d . . . H28A H 0.4813 0.3998 0.0960 0.025 Uiso 1 1 calc R . . C29 C 0.6148(3) 0.0063(3) 0.23047(13) 0.0160(5) Uani 1 1 d . . . C30 C 0.4810(3) -0.0069(3) 0.22290(14) 0.0204(5) Uani 1 1 d . . . H30A H 0.4001 0.0695 0.2011 0.024 Uiso 1 1 calc R . . C31 C 0.4654(4) -0.1306(3) 0.24701(15) 0.0250(6) Uani 1 1 d . . . H31A H 0.3738 -0.1386 0.2420 0.030 Uiso 1 1 calc R . . C32 C 0.5835(4) -0.2424(3) 0.27833(16) 0.0268(6) Uani 1 1 d . . . H32A H 0.5741 -0.3282 0.2939 0.032 Uiso 1 1 calc R . . C33 C 0.7155(3) -0.2293(3) 0.28700(17) 0.0299(6) Uani 1 1 d . . . H33A H 0.7961 -0.3057 0.3089 0.036 Uiso 1 1 calc R . . C34 C 0.7304(3) -0.1047(3) 0.26377(15) 0.0235(5) Uani 1 1 d . . . H34A H 0.8203 -0.0956 0.2707 0.028 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01041(16) 0.01068(16) 0.01018(16) 0.00089(11) -0.00100(12) -0.00368(13) Fe2 0.01536(17) 0.01292(17) 0.01098(17) 0.00079(12) -0.00041(12) -0.00654(14) P1 0.0107(3) 0.0125(3) 0.0105(3) -0.0007(2) -0.0011(2) -0.0038(2) P2 0.0139(3) 0.0121(3) 0.0110(3) 0.0002(2) -0.0024(2) -0.0055(2) S1 0.0113(3) 0.0157(3) 0.0191(3) 0.0035(2) -0.0024(2) -0.0051(2) S2 0.0195(3) 0.0136(3) 0.0139(3) -0.0026(2) 0.0025(2) -0.0079(2) N1 0.0143(9) 0.0142(9) 0.0134(9) -0.0031(7) -0.0002(7) -0.0041(8) O1 0.0250(10) 0.0168(9) 0.0234(10) 0.0056(7) -0.0064(8) -0.0054(8) O2 0.0281(11) 0.0318(11) 0.0188(10) -0.0004(8) 0.0038(8) -0.0087(9) O3 0.0322(11) 0.0435(13) 0.0381(12) 0.0191(10) -0.0175(10) -0.0251(10) O4 0.0393(12) 0.0197(10) 0.0230(10) 0.0003(7) 0.0004(8) -0.0154(9) C1 0.0139(11) 0.0144(11) 0.0143(11) -0.0013(8) -0.0014(8) -0.0053(9) C2 0.0199(12) 0.0164(11) 0.0152(11) 0.0009(9) -0.0022(9) -0.0067(10) C3 0.0258(13) 0.0239(13) 0.0191(12) 0.0058(10) -0.0045(10) -0.0163(11) C4 0.0187(12) 0.0198(12) 0.0127(11) -0.0005(9) -0.0005(9) -0.0080(10) C5 0.0112(12) 0.0193(13) 0.057(2) 0.0061(13) -0.0018(12) -0.0016(10) C6 0.0307(16) 0.0303(16) 0.0410(18) -0.0075(13) -0.0082(14) -0.0005(13) C7 0.0261(14) 0.0122(12) 0.0383(16) -0.0062(11) 0.0126(12) -0.0046(11) C8 0.0229(14) 0.0267(14) 0.0192(13) -0.0046(10) 0.0059(11) 0.0023(11) C9 0.0213(13) 0.0253(13) 0.0185(12) -0.0065(10) 0.0059(10) -0.0108(11) C10 0.0384(19) 0.0377(19) 0.044(2) -0.0084(15) 0.0050(15) -0.0095(16) C11 0.0164(11) 0.0194(12) 0.0114(10) -0.0013(8) 0.0000(8) -0.0096(10) C12 0.0197(12) 0.0322(15) 0.0191(12) 0.0028(10) -0.0037(10) -0.0139(11) C13 0.0225(14) 0.0492(19) 0.0270(15) 0.0048(13) -0.0026(11) -0.0229(14) C14 0.0332(16) 0.0440(18) 0.0221(14) 0.0063(12) 0.0002(12) -0.0270(14) C15 0.0293(15) 0.0323(15) 0.0216(13) 0.0075(11) -0.0032(11) -0.0153(13) C16 0.0179(12) 0.0252(13) 0.0195(12) 0.0036(10) -0.0032(10) -0.0100(10) C17 0.0140(11) 0.0164(11) 0.0126(10) 0.0001(8) -0.0029(8) -0.0056(9) C18 0.0346(16) 0.0159(13) 0.0338(16) -0.0031(11) -0.0188(13) -0.0049(12) C19 0.0409(18) 0.0169(13) 0.0403(17) 0.0035(12) -0.0268(14) -0.0042(12) C20 0.0238(13) 0.0243(13) 0.0210(13) 0.0035(10) -0.0107(10) -0.0099(11) C21 0.0176(11) 0.0217(12) 0.0147(11) -0.0018(9) -0.0013(9) -0.0112(10) C22 0.0143(11) 0.0141(11) 0.0142(11) -0.0004(8) 0.0003(8) -0.0055(9) C23 0.0168(11) 0.0216(12) 0.0109(10) 0.0000(9) -0.0027(8) -0.0107(10) C24 0.0210(12) 0.0213(12) 0.0172(12) -0.0012(9) -0.0029(9) -0.0100(10) C25 0.0221(13) 0.0297(14) 0.0181(12) -0.0053(10) -0.0021(10) -0.0141(11) C26 0.0349(15) 0.0378(16) 0.0135(12) 0.0025(10) -0.0059(11) -0.0233(13) C27 0.0422(17) 0.0265(14) 0.0185(13) 0.0067(10) -0.0123(12) -0.0171(13) C28 0.0294(14) 0.0197(12) 0.0168(12) 0.0013(9) -0.0066(10) -0.0123(11) C29 0.0216(12) 0.0123(11) 0.0148(11) -0.0006(8) 0.0000(9) -0.0089(9) C30 0.0267(13) 0.0200(12) 0.0181(12) 0.0015(9) -0.0063(10) -0.0129(11) C31 0.0341(15) 0.0260(14) 0.0216(13) -0.0048(10) 0.0005(11) -0.0197(12) C32 0.0348(15) 0.0167(12) 0.0268(14) -0.0011(10) 0.0076(12) -0.0133(12) C33 0.0254(14) 0.0163(13) 0.0377(16) 0.0094(11) 0.0002(12) -0.0033(11) C34 0.0177(12) 0.0196(13) 0.0293(14) 0.0047(10) 0.0000(10) -0.0067(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 1.743(2) . ? Fe1 P1 2.2124(7) . ? Fe1 P2 2.2137(7) . ? Fe1 S2 2.2203(7) . ? Fe1 S1 2.2214(7) . ? Fe1 Fe2 2.6236(5) . ? Fe2 C3 1.793(3) . ? Fe2 C2 1.794(3) . ? Fe2 C4 1.798(3) . ? Fe2 S2 2.2524(7) . ? Fe2 S1 2.2598(7) . ? P1 N1 1.712(2) . ? P1 C17 1.817(2) . ? P1 C11 1.837(2) . ? P1 P2 2.5803(8) . ? P2 N1 1.714(2) . ? P2 C29 1.818(2) . ? P2 C23 1.838(2) . ? S1 C5 1.825(3) . ? S2 C7 1.838(3) . ? N1 C8 1.498(3) . ? O1 C1 1.163(3) . ? O2 C2 1.143(3) . ? O3 C3 1.136(3) . ? O4 C4 1.138(3) . ? C5 C6 1.446(5) . ? C6 C7 1.540(5) . ? C8 C10 1.466(5) . ? C8 C9 1.514(4) . ? C11 C16 1.395(3) . ? C11 C12 1.401(3) . ? C12 C13 1.389(4) . ? C13 C14 1.386(4) . ? C14 C15 1.389(4) . ? C15 C16 1.388(4) . ? C17 C18 1.384(4) . ? C17 C22 1.399(3) . ? C18 C19 1.388(4) . ? C19 C20 1.389(4) . ? C20 C21 1.382(4) . ? C21 C22 1.388(3) . ? C23 C28 1.394(3) . ? C23 C24 1.399(3) . ? C24 C25 1.393(4) . ? C25 C26 1.381(4) . ? C26 C27 1.382(4) . ? C27 C28 1.393(4) . ? C29 C34 1.386(4) . ? C29 C30 1.397(4) . ? C30 C31 1.388(4) . ? C31 C32 1.383(4) . ? C32 C33 1.385(4) . ? C33 C34 1.388(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 P1 103.57(8) . . ? C1 Fe1 P2 105.18(8) . . ? P1 Fe1 P2 71.32(2) . . ? C1 Fe1 S2 98.94(8) . . ? P1 Fe1 S2 97.43(2) . . ? P2 Fe1 S2 155.14(3) . . ? C1 Fe1 S1 97.35(8) . . ? P1 Fe1 S1 157.69(3) . . ? P2 Fe1 S1 95.92(3) . . ? S2 Fe1 S1 86.77(3) . . ? C1 Fe1 Fe2 138.66(8) . . ? P1 Fe1 Fe2 110.44(2) . . ? P2 Fe1 Fe2 107.44(2) . . ? S2 Fe1 Fe2 54.656(19) . . ? S1 Fe1 Fe2 54.848(18) . . ? C3 Fe2 C2 97.06(12) . . ? C3 Fe2 C4 89.11(12) . . ? C2 Fe2 C4 94.50(11) . . ? C3 Fe2 S2 89.11(8) . . ? C2 Fe2 S2 101.91(8) . . ? C4 Fe2 S2 163.59(8) . . ? C3 Fe2 S1 157.61(9) . . ? C2 Fe2 S1 105.29(8) . . ? C4 Fe2 S1 90.40(8) . . ? S2 Fe2 S1 85.09(2) . . ? C3 Fe2 Fe1 106.30(8) . . ? C2 Fe2 Fe1 144.71(8) . . ? C4 Fe2 Fe1 111.62(8) . . ? S2 Fe2 Fe1 53.519(18) . . ? S1 Fe2 Fe1 53.488(18) . . ? N1 P1 C17 108.07(11) . . ? N1 P1 C11 105.35(10) . . ? C17 P1 C11 100.33(11) . . ? N1 P1 Fe1 95.50(7) . . ? C17 P1 Fe1 121.02(8) . . ? C11 P1 Fe1 124.68(8) . . ? N1 P1 P2 41.16(7) . . ? C17 P1 P2 127.57(8) . . ? C11 P1 P2 125.21(8) . . ? Fe1 P1 P2 54.36(2) . . ? N1 P2 C29 109.20(11) . . ? N1 P2 C23 106.81(10) . . ? C29 P2 C23 99.69(11) . . ? N1 P2 Fe1 95.40(7) . . ? C29 P2 Fe1 120.60(8) . . ? C23 P2 Fe1 124.02(8) . . ? N1 P2 P1 41.10(7) . . ? C29 P2 P1 128.33(8) . . ? C23 P2 P1 126.14(8) . . ? Fe1 P2 P1 54.32(2) . . ? C5 S1 Fe1 109.21(10) . . ? C5 S1 Fe2 111.89(12) . . ? Fe1 S1 Fe2 71.66(2) . . ? C7 S2 Fe1 109.92(11) . . ? C7 S2 Fe2 109.84(9) . . ? Fe1 S2 Fe2 71.83(2) . . ? C8 N1 P1 126.24(19) . . ? C8 N1 P2 132.32(19) . . ? P1 N1 P2 97.74(10) . . ? O1 C1 Fe1 172.6(2) . . ? O2 C2 Fe2 177.9(2) . . ? O3 C3 Fe2 175.3(2) . . ? O4 C4 Fe2 173.0(2) . . ? C6 C5 S1 117.5(2) . . ? C5 C6 C7 119.0(3) . . ? C6 C7 S2 117.8(2) . . ? C10 C8 N1 115.7(3) . . ? C10 C8 C9 113.9(3) . . ? N1 C8 C9 113.5(2) . . ? C16 C11 C12 118.1(2) . . ? C16 C11 P1 120.32(18) . . ? C12 C11 P1 121.3(2) . . ? C13 C12 C11 120.5(3) . . ? C14 C13 C12 120.5(3) . . ? C13 C14 C15 119.7(3) . . ? C16 C15 C14 119.8(3) . . ? C15 C16 C11 121.4(2) . . ? C18 C17 C22 119.2(2) . . ? C18 C17 P1 123.82(19) . . ? C22 C17 P1 116.99(18) . . ? C17 C18 C19 120.4(3) . . ? C18 C19 C20 120.5(3) . . ? C21 C20 C19 119.4(2) . . ? C20 C21 C22 120.5(2) . . ? C21 C22 C17 120.1(2) . . ? C28 C23 C24 118.5(2) . . ? C28 C23 P2 119.63(19) . . ? C24 C23 P2 121.82(19) . . ? C25 C24 C23 120.6(2) . . ? C26 C25 C24 120.3(2) . . ? C25 C26 C27 119.6(2) . . ? C26 C27 C28 120.6(3) . . ? C27 C28 C23 120.4(2) . . ? C34 C29 C30 119.1(2) . . ? C34 C29 P2 123.0(2) . . ? C30 C29 P2 117.81(19) . . ? C31 C30 C29 120.5(3) . . ? C32 C31 C30 119.9(3) . . ? C31 C32 C33 119.9(3) . . ? C32 C33 C34 120.3(3) . . ? C29 C34 C33 120.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Fe1 Fe2 C3 -135.15(15) . . . . ? P1 Fe1 Fe2 C3 8.22(9) . . . . ? P2 Fe1 Fe2 C3 84.26(9) . . . . ? S2 Fe1 Fe2 C3 -76.33(9) . . . . ? S1 Fe1 Fe2 C3 169.15(9) . . . . ? C1 Fe1 Fe2 C2 -5.74(19) . . . . ? P1 Fe1 Fe2 C2 137.64(15) . . . . ? P2 Fe1 Fe2 C2 -146.32(15) . . . . ? S2 Fe1 Fe2 C2 53.09(15) . . . . ? S1 Fe1 Fe2 C2 -61.43(15) . . . . ? C1 Fe1 Fe2 C4 129.20(15) . . . . ? P1 Fe1 Fe2 C4 -87.43(9) . . . . ? P2 Fe1 Fe2 C4 -11.39(9) . . . . ? S2 Fe1 Fe2 C4 -171.98(9) . . . . ? S1 Fe1 Fe2 C4 73.50(9) . . . . ? C1 Fe1 Fe2 S2 -58.82(12) . . . . ? P1 Fe1 Fe2 S2 84.55(3) . . . . ? P2 Fe1 Fe2 S2 160.59(3) . . . . ? S1 Fe1 Fe2 S2 -114.52(3) . . . . ? C1 Fe1 Fe2 S1 55.70(12) . . . . ? P1 Fe1 Fe2 S1 -160.93(3) . . . . ? P2 Fe1 Fe2 S1 -84.89(3) . . . . ? S2 Fe1 Fe2 S1 114.52(3) . . . . ? C1 Fe1 P1 N1 -103.15(11) . . . . ? P2 Fe1 P1 N1 -1.45(7) . . . . ? S2 Fe1 P1 N1 155.74(7) . . . . ? S1 Fe1 P1 N1 56.04(10) . . . . ? Fe2 Fe1 P1 N1 100.76(7) . . . . ? C1 Fe1 P1 C17 141.92(12) . . . . ? P2 Fe1 P1 C17 -116.38(10) . . . . ? S2 Fe1 P1 C17 40.81(10) . . . . ? S1 Fe1 P1 C17 -58.89(12) . . . . ? Fe2 Fe1 P1 C17 -14.16(10) . . . . ? C1 Fe1 P1 C11 9.81(13) . . . . ? P2 Fe1 P1 C11 111.51(10) . . . . ? S2 Fe1 P1 C11 -91.30(10) . . . . ? S1 Fe1 P1 C11 169.00(10) . . . . ? Fe2 Fe1 P1 C11 -146.28(9) . . . . ? C1 Fe1 P1 P2 -101.70(8) . . . . ? S2 Fe1 P1 P2 157.19(3) . . . . ? S1 Fe1 P1 P2 57.49(7) . . . . ? Fe2 Fe1 P1 P2 102.22(2) . . . . ? C1 Fe1 P2 N1 100.94(11) . . . . ? P1 Fe1 P2 N1 1.45(7) . . . . ? S2 Fe1 P2 N1 -64.67(10) . . . . ? S1 Fe1 P2 N1 -159.77(7) . . . . ? Fe2 Fe1 P2 N1 -104.82(7) . . . . ? C1 Fe1 P2 C29 -142.98(13) . . . . ? P1 Fe1 P2 C29 117.54(10) . . . . ? S2 Fe1 P2 C29 51.42(12) . . . . ? S1 Fe1 P2 C29 -43.69(10) . . . . ? Fe2 Fe1 P2 C29 11.27(10) . . . . ? C1 Fe1 P2 C23 -13.54(13) . . . . ? P1 Fe1 P2 C23 -113.03(10) . . . . ? S2 Fe1 P2 C23 -179.15(10) . . . . ? S1 Fe1 P2 C23 85.74(10) . . . . ? Fe2 Fe1 P2 C23 140.70(9) . . . . ? C1 Fe1 P2 P1 99.49(8) . . . . ? S2 Fe1 P2 P1 -66.12(6) . . . . ? S1 Fe1 P2 P1 -161.23(3) . . . . ? Fe2 Fe1 P2 P1 -106.27(2) . . . . ? C17 P1 P2 N1 -73.41(14) . . . . ? C11 P1 P2 N1 71.65(14) . . . . ? Fe1 P1 P2 N1 -177.80(11) . . . . ? N1 P1 P2 C29 74.43(15) . . . . ? C17 P1 P2 C29 1.02(15) . . . . ? C11 P1 P2 C29 146.08(14) . . . . ? Fe1 P1 P2 C29 -103.37(10) . . . . ? N1 P1 P2 C23 -73.01(15) . . . . ? C17 P1 P2 C23 -146.43(14) . . . . ? C11 P1 P2 C23 -1.36(15) . . . . ? Fe1 P1 P2 C23 109.18(10) . . . . ? N1 P1 P2 Fe1 177.80(11) . . . . ? C17 P1 P2 Fe1 104.39(10) . . . . ? C11 P1 P2 Fe1 -110.55(10) . . . . ? C1 Fe1 S1 C5 -39.13(15) . . . . ? P1 Fe1 S1 C5 161.25(13) . . . . ? P2 Fe1 S1 C5 -145.32(12) . . . . ? S2 Fe1 S1 C5 59.48(12) . . . . ? Fe2 Fe1 S1 C5 107.49(12) . . . . ? C1 Fe1 S1 Fe2 -146.62(8) . . . . ? P1 Fe1 S1 Fe2 53.76(7) . . . . ? P2 Fe1 S1 Fe2 107.19(2) . . . . ? S2 Fe1 S1 Fe2 -48.01(2) . . . . ? C3 Fe2 S1 C5 -132.2(2) . . . . ? C2 Fe2 S1 C5 44.36(13) . . . . ? C4 Fe2 S1 C5 139.14(13) . . . . ? S2 Fe2 S1 C5 -56.66(11) . . . . ? Fe1 Fe2 S1 C5 -103.91(11) . . . . ? C3 Fe2 S1 Fe1 -28.3(2) . . . . ? C2 Fe2 S1 Fe1 148.27(8) . . . . ? C4 Fe2 S1 Fe1 -116.95(8) . . . . ? S2 Fe2 S1 Fe1 47.24(2) . . . . ? C1 Fe1 S2 C7 39.98(13) . . . . ? P1 Fe1 S2 C7 145.05(10) . . . . ? P2 Fe1 S2 C7 -154.08(11) . . . . ? S1 Fe1 S2 C7 -56.96(10) . . . . ? Fe2 Fe1 S2 C7 -105.13(10) . . . . ? C1 Fe1 S2 Fe2 145.11(8) . . . . ? P1 Fe1 S2 Fe2 -109.82(2) . . . . ? P2 Fe1 S2 Fe2 -48.95(7) . . . . ? S1 Fe1 S2 Fe2 48.17(2) . . . . ? C3 Fe2 S2 C7 -143.63(14) . . . . ? C2 Fe2 S2 C7 -46.60(14) . . . . ? C4 Fe2 S2 C7 132.6(3) . . . . ? S1 Fe2 S2 C7 58.02(11) . . . . ? Fe1 Fe2 S2 C7 105.24(11) . . . . ? C3 Fe2 S2 Fe1 111.13(9) . . . . ? C2 Fe2 S2 Fe1 -151.83(8) . . . . ? C4 Fe2 S2 Fe1 27.3(3) . . . . ? S1 Fe2 S2 Fe1 -47.22(2) . . . . ? C17 P1 N1 C8 -72.7(2) . . . . ? C11 P1 N1 C8 33.9(2) . . . . ? Fe1 P1 N1 C8 162.2(2) . . . . ? P2 P1 N1 C8 160.4(3) . . . . ? C17 P1 N1 P2 126.96(11) . . . . ? C11 P1 N1 P2 -126.46(11) . . . . ? Fe1 P1 N1 P2 1.79(9) . . . . ? C29 P2 N1 C8 74.6(2) . . . . ? C23 P2 N1 C8 -32.3(3) . . . . ? Fe1 P2 N1 C8 -160.3(2) . . . . ? P1 P2 N1 C8 -158.5(3) . . . . ? C29 P2 N1 P1 -126.85(11) . . . . ? C23 P2 N1 P1 126.21(11) . . . . ? Fe1 P2 N1 P1 -1.79(9) . . . . ? P1 Fe1 C1 O1 -149.4(17) . . . . ? P2 Fe1 C1 O1 136.7(17) . . . . ? S2 Fe1 C1 O1 -49.4(17) . . . . ? S1 Fe1 C1 O1 38.4(17) . . . . ? Fe2 Fe1 C1 O1 -4.5(18) . . . . ? C3 Fe2 C2 O2 -53(7) . . . . ? C4 Fe2 C2 O2 37(7) . . . . ? S2 Fe2 C2 O2 -143(7) . . . . ? S1 Fe2 C2 O2 129(7) . . . . ? Fe1 Fe2 C2 O2 176(100) . . . . ? C2 Fe2 C3 O3 34(3) . . . . ? C4 Fe2 C3 O3 -61(3) . . . . ? S2 Fe2 C3 O3 135(3) . . . . ? S1 Fe2 C3 O3 -150(3) . . . . ? Fe1 Fe2 C3 O3 -173(3) . . . . ? C3 Fe2 C4 O4 65.6(19) . . . . ? C2 Fe2 C4 O4 -31.4(19) . . . . ? S2 Fe2 C4 O4 149.4(17) . . . . ? S1 Fe2 C4 O4 -136.8(19) . . . . ? Fe1 Fe2 C4 O4 172.8(19) . . . . ? Fe1 S1 C5 C6 -66.2(3) . . . . ? Fe2 S1 C5 C6 11.1(3) . . . . ? S1 C5 C6 C7 54.7(4) . . . . ? C5 C6 C7 S2 -51.2(4) . . . . ? Fe1 S2 C7 C6 59.1(3) . . . . ? Fe2 S2 C7 C6 -18.1(3) . . . . ? P1 N1 C8 C10 141.7(3) . . . . ? P2 N1 C8 C10 -65.0(4) . . . . ? P1 N1 C8 C9 -83.8(3) . . . . ? P2 N1 C8 C9 69.5(3) . . . . ? N1 P1 C11 C16 87.1(2) . . . . ? C17 P1 C11 C16 -160.8(2) . . . . ? Fe1 P1 C11 C16 -21.0(2) . . . . ? P2 P1 C11 C16 46.7(2) . . . . ? N1 P1 C11 C12 -87.6(2) . . . . ? C17 P1 C11 C12 24.5(2) . . . . ? Fe1 P1 C11 C12 164.28(18) . . . . ? P2 P1 C11 C12 -127.98(19) . . . . ? C16 C11 C12 C13 -0.5(4) . . . . ? P1 C11 C12 C13 174.3(2) . . . . ? C11 C12 C13 C14 0.5(5) . . . . ? C12 C13 C14 C15 -0.4(5) . . . . ? C13 C14 C15 C16 0.2(5) . . . . ? C14 C15 C16 C11 -0.1(4) . . . . ? C12 C11 C16 C15 0.3(4) . . . . ? P1 C11 C16 C15 -174.6(2) . . . . ? N1 P1 C17 C18 -6.1(3) . . . . ? C11 P1 C17 C18 -116.1(2) . . . . ? Fe1 P1 C17 C18 102.2(2) . . . . ? P2 P1 C17 C18 35.5(3) . . . . ? N1 P1 C17 C22 174.62(18) . . . . ? C11 P1 C17 C22 64.6(2) . . . . ? Fe1 P1 C17 C22 -77.1(2) . . . . ? P2 P1 C17 C22 -143.81(15) . . . . ? C22 C17 C18 C19 -0.4(4) . . . . ? P1 C17 C18 C19 -179.7(3) . . . . ? C17 C18 C19 C20 0.3(5) . . . . ? C18 C19 C20 C21 -0.3(5) . . . . ? C19 C20 C21 C22 0.3(4) . . . . ? C20 C21 C22 C17 -0.4(4) . . . . ? C18 C17 C22 C21 0.4(4) . . . . ? P1 C17 C22 C21 179.74(18) . . . . ? N1 P2 C23 C28 -95.4(2) . . . . ? C29 P2 C23 C28 151.0(2) . . . . ? Fe1 P2 C23 C28 13.4(2) . . . . ? P1 P2 C23 C28 -54.3(2) . . . . ? N1 P2 C23 C24 81.1(2) . . . . ? C29 P2 C23 C24 -32.5(2) . . . . ? Fe1 P2 C23 C24 -170.09(17) . . . . ? P1 P2 C23 C24 122.15(19) . . . . ? C28 C23 C24 C25 1.6(4) . . . . ? P2 C23 C24 C25 -174.9(2) . . . . ? C23 C24 C25 C26 -1.3(4) . . . . ? C24 C25 C26 C27 0.2(4) . . . . ? C25 C26 C27 C28 0.6(5) . . . . ? C26 C27 C28 C23 -0.2(4) . . . . ? C24 C23 C28 C27 -0.9(4) . . . . ? P2 C23 C28 C27 175.7(2) . . . . ? N1 P2 C29 C34 15.7(2) . . . . ? C23 P2 C29 C34 127.5(2) . . . . ? Fe1 P2 C29 C34 -93.0(2) . . . . ? P1 P2 C29 C34 -26.4(3) . . . . ? N1 P2 C29 C30 -167.48(19) . . . . ? C23 P2 C29 C30 -55.8(2) . . . . ? Fe1 P2 C29 C30 83.7(2) . . . . ? P1 P2 C29 C30 150.40(16) . . . . ? C34 C29 C30 C31 -1.3(4) . . . . ? P2 C29 C30 C31 -178.2(2) . . . . ? C29 C30 C31 C32 -0.5(4) . . . . ? C30 C31 C32 C33 1.4(4) . . . . ? C31 C32 C33 C34 -0.6(5) . . . . ? C30 C29 C34 C33 2.2(4) . . . . ? P2 C29 C34 C33 178.9(2) . . . . ? C32 C33 C34 C29 -1.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.451 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.099 #===END #===END data_str0539 _database_code_depnum_ccdc_archive 'CCDC 639867' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 Cl2 Fe2 O4 P2 S2' _chemical_formula_weight 861.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 10.1181(13) _cell_length_b 10.9537(14) _cell_length_c 17.301(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.262(2) _cell_angle_gamma 90.00 _cell_volume 1840.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.174 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7658 _exptl_absorpt_correction_T_max 0.9223 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15525 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8372 _reflns_number_gt 7769 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.033(11) _refine_ls_number_reflns 8372 _refine_ls_number_parameters 451 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0874 _refine_ls_wR_factor_gt 0.0856 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 0.28103(4) 0.41919(4) 0.55572(3) 0.01450(10) Uani 1 1 d . . . Fe2 Fe 0.44441(4) 0.25199(4) 0.62611(3) 0.01047(9) Uani 1 1 d . . . P1 P 0.65070(8) 0.27367(7) 0.60909(5) 0.01068(15) Uani 1 1 d . . . P2 P 0.53735(8) 0.11958(7) 0.72000(5) 0.01198(16) Uani 1 1 d . . . S1 S 0.44215(8) 0.44259(7) 0.67597(5) 0.01322(15) Uani 1 1 d . . . S2 S 0.21640(8) 0.25219(7) 0.61441(5) 0.01490(16) Uani 1 1 d . . . O1 O 0.0555(3) 0.5894(2) 0.55448(17) 0.0314(6) Uani 1 1 d . . . O2 O 0.1833(3) 0.2955(3) 0.40062(15) 0.0321(6) Uani 1 1 d . . . O3 O 0.4469(3) 0.5822(3) 0.48601(17) 0.0392(7) Uani 1 1 d . . . O4 O 0.3844(3) 0.0601(2) 0.50497(14) 0.0207(5) Uani 1 1 d . . . C1 C 0.1441(3) 0.5238(3) 0.5567(2) 0.0187(7) Uani 1 1 d . . . C2 C 0.2181(3) 0.3432(3) 0.4615(2) 0.0213(7) Uani 1 1 d . . . C3 C 0.3834(4) 0.5184(3) 0.5131(2) 0.0234(8) Uani 1 1 d . . . C4 C 0.4101(3) 0.1366(3) 0.55303(19) 0.0141(6) Uani 1 1 d . . . C5 C 0.3577(3) 0.4551(3) 0.75663(19) 0.0175(7) Uani 1 1 d . . . H5A H 0.4279 0.4798 0.8066 0.021 Uiso 1 1 calc R . . H5B H 0.2889 0.5216 0.7425 0.021 Uiso 1 1 calc R . . C6 C 0.2867(3) 0.3420(3) 0.77440(19) 0.0167(7) Uani 1 1 d . . . H6A H 0.2505 0.3588 0.8209 0.020 Uiso 1 1 calc R . . H6B H 0.3556 0.2758 0.7903 0.020 Uiso 1 1 calc R . . C7 C 0.1696(3) 0.2978(3) 0.70481(19) 0.0185(7) Uani 1 1 d . . . H7A H 0.1000 0.3637 0.6900 0.022 Uiso 1 1 calc R . . H7B H 0.1255 0.2273 0.7235 0.022 Uiso 1 1 calc R . . C8 C 0.7447(3) 0.1325(3) 0.64530(18) 0.0131(6) Uani 1 1 d . . . C9 C 0.6917(3) 0.0611(3) 0.69702(18) 0.0135(6) Uani 1 1 d . . . C10 C 0.7642(3) -0.0424(3) 0.7325(2) 0.0188(7) Uani 1 1 d . . . H10A H 0.7296 -0.0908 0.7681 0.023 Uiso 1 1 calc R . . C11 C 0.8848(4) -0.0752(3) 0.7166(2) 0.0197(7) Uani 1 1 d . . . H11A H 0.9334 -0.1454 0.7417 0.024 Uiso 1 1 calc R . . C12 C 0.9363(3) -0.0061(3) 0.6641(2) 0.0189(7) Uani 1 1 d . . . H12A H 1.0189 -0.0303 0.6525 0.023 Uiso 1 1 calc R . . C13 C 0.8673(3) 0.0978(3) 0.62851(18) 0.0151(6) Uani 1 1 d . . . H13A H 0.9029 0.1453 0.5929 0.018 Uiso 1 1 calc R . . C14 C 0.7696(3) 0.3878(3) 0.66841(18) 0.0126(6) Uani 1 1 d . . . C15 C 0.8567(3) 0.3604(3) 0.74345(19) 0.0146(6) Uani 1 1 d . . . H15A H 0.8571 0.2804 0.7648 0.017 Uiso 1 1 calc R . . C16 C 0.9440(3) 0.4495(3) 0.78809(19) 0.0173(7) Uani 1 1 d . . . H16A H 1.0030 0.4299 0.8398 0.021 Uiso 1 1 calc R . . C17 C 0.9455(4) 0.5648(3) 0.7580(2) 0.0204(7) Uani 1 1 d . . . H17A H 1.0068 0.6247 0.7879 0.024 Uiso 1 1 calc R . . C18 C 0.8563(4) 0.5938(3) 0.6830(2) 0.0227(7) Uani 1 1 d . . . H18A H 0.8573 0.6737 0.6619 0.027 Uiso 1 1 calc R . . C19 C 0.7661(3) 0.5072(3) 0.63873(19) 0.0185(7) Uani 1 1 d . . . H19A H 0.7027 0.5287 0.5888 0.022 Uiso 1 1 calc R . . C20 C 0.6743(3) 0.2964(3) 0.50880(18) 0.0136(6) Uani 1 1 d . . . C21 C 0.8010(3) 0.3307(3) 0.49844(18) 0.0153(6) Uani 1 1 d . . . H21A H 0.8777 0.3423 0.5443 0.018 Uiso 1 1 calc R . . C22 C 0.8166(3) 0.3482(3) 0.42212(19) 0.0189(7) Uani 1 1 d . . . H22A H 0.9032 0.3725 0.4159 0.023 Uiso 1 1 calc R . . C23 C 0.7056(4) 0.3301(3) 0.35475(19) 0.0199(7) Uani 1 1 d . . . H23A H 0.7161 0.3418 0.3024 0.024 Uiso 1 1 calc R . . C24 C 0.5806(3) 0.2953(3) 0.36397(19) 0.0176(6) Uani 1 1 d . . . H24A H 0.5050 0.2821 0.3178 0.021 Uiso 1 1 calc R . . C25 C 0.5642(3) 0.2792(3) 0.44013(19) 0.0148(6) Uani 1 1 d . . . H25A H 0.4767 0.2563 0.4457 0.018 Uiso 1 1 calc R . . C26 C 0.6073(3) 0.1580(3) 0.82705(18) 0.0158(6) Uani 1 1 d . . . C27 C 0.6269(4) 0.0688(3) 0.8873(2) 0.0215(7) Uani 1 1 d . . . H27A H 0.5997 -0.0133 0.8738 0.026 Uiso 1 1 calc R . . C28 C 0.6864(4) 0.1020(4) 0.9669(2) 0.0300(9) Uani 1 1 d . . . H28A H 0.6988 0.0423 1.0081 0.036 Uiso 1 1 calc R . . C29 C 0.7276(4) 0.2200(4) 0.9868(2) 0.0324(9) Uani 1 1 d . . . H29A H 0.7685 0.2410 1.0415 0.039 Uiso 1 1 calc R . . C30 C 0.7099(4) 0.3086(3) 0.9278(2) 0.0245(8) Uani 1 1 d . . . H30A H 0.7403 0.3899 0.9415 0.029 Uiso 1 1 calc R . . C31 C 0.6472(3) 0.2770(3) 0.84831(19) 0.0162(6) Uani 1 1 d . . . H31A H 0.6314 0.3381 0.8078 0.019 Uiso 1 1 calc R . . C32 C 0.4313(3) -0.0149(3) 0.72156(18) 0.0136(6) Uani 1 1 d . . . C33 C 0.3439(3) -0.0174(3) 0.7707(2) 0.0192(7) Uani 1 1 d . . . H33A H 0.3462 0.0479 0.8072 0.023 Uiso 1 1 calc R . . C34 C 0.2529(3) -0.1138(3) 0.7673(2) 0.0234(8) Uani 1 1 d . . . H34A H 0.1948 -0.1152 0.8019 0.028 Uiso 1 1 calc R . . C35 C 0.2479(3) -0.2078(3) 0.7130(2) 0.0235(8) Uani 1 1 d . . . H35A H 0.1857 -0.2737 0.7102 0.028 Uiso 1 1 calc R . . C36 C 0.3331(4) -0.2064(3) 0.6624(2) 0.0220(7) Uani 1 1 d . . . H36A H 0.3285 -0.2708 0.6250 0.026 Uiso 1 1 calc R . . C37 C 0.4249(3) -0.1110(3) 0.66673(19) 0.0183(7) Uani 1 1 d . . . H37A H 0.4837 -0.1106 0.6325 0.022 Uiso 1 1 calc R . . C38 C 0.0770(5) 0.0877(5) 0.9760(3) 0.0528(13) Uani 1 1 d . . . H38A H 0.0125 0.1390 0.9955 0.063 Uiso 1 1 calc R . . H38B H 0.1580 0.0709 1.0223 0.063 Uiso 1 1 calc R . . Cl1 Cl -0.00460(13) -0.05167(12) 0.93989(8) 0.0543(3) Uani 1 1 d . . . Cl2 Cl 0.1304(2) 0.16855(16) 0.90311(12) 0.0966(7) 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 0.0124(2) 0.0179(2) 0.0134(2) 0.00149(18) 0.00391(16) 0.00290(18) Fe2 0.00930(19) 0.0112(2) 0.0110(2) -0.00074(15) 0.00310(16) -0.00038(15) P1 0.0095(4) 0.0120(4) 0.0102(4) -0.0008(3) 0.0023(3) -0.0008(3) P2 0.0116(4) 0.0126(4) 0.0119(4) 0.0003(3) 0.0036(3) -0.0008(3) S1 0.0135(4) 0.0130(4) 0.0143(4) -0.0007(3) 0.0056(3) 0.0000(3) S2 0.0110(4) 0.0199(4) 0.0144(4) -0.0020(3) 0.0046(3) -0.0015(3) O1 0.0248(14) 0.0286(15) 0.0413(17) -0.0014(12) 0.0103(12) 0.0082(11) O2 0.0341(16) 0.0414(16) 0.0168(13) -0.0048(11) 0.0004(11) 0.0120(13) O3 0.0320(16) 0.0510(19) 0.0377(17) 0.0186(14) 0.0149(13) -0.0083(13) O4 0.0250(13) 0.0188(12) 0.0181(12) -0.0055(9) 0.0056(10) -0.0032(10) C1 0.0168(16) 0.0188(16) 0.0210(17) 0.0007(13) 0.0063(13) 0.0013(13) C2 0.0176(17) 0.0254(19) 0.0208(18) 0.0062(14) 0.0051(14) 0.0093(14) C3 0.0182(17) 0.031(2) 0.0201(18) 0.0040(15) 0.0036(14) 0.0045(15) C4 0.0095(14) 0.0169(16) 0.0170(16) 0.0036(12) 0.0055(12) -0.0011(12) C5 0.0167(16) 0.0221(17) 0.0155(16) -0.0028(13) 0.0075(13) 0.0019(13) C6 0.0164(16) 0.0185(16) 0.0179(16) -0.0015(12) 0.0096(13) -0.0002(12) C7 0.0148(16) 0.0234(17) 0.0204(17) -0.0005(13) 0.0099(13) -0.0022(13) C8 0.0124(15) 0.0132(15) 0.0124(14) -0.0018(11) 0.0016(12) 0.0002(12) C9 0.0133(15) 0.0105(15) 0.0162(15) 0.0009(11) 0.0034(12) -0.0022(11) C10 0.0206(17) 0.0165(16) 0.0186(16) 0.0026(13) 0.0040(13) 0.0011(13) C11 0.0187(17) 0.0122(15) 0.0246(18) -0.0027(13) 0.0004(14) 0.0033(13) C12 0.0164(16) 0.0182(16) 0.0210(17) -0.0061(13) 0.0034(13) 0.0038(13) C13 0.0141(15) 0.0172(16) 0.0128(16) -0.0023(12) 0.0019(12) 0.0013(12) C14 0.0090(14) 0.0177(16) 0.0123(14) -0.0031(12) 0.0051(11) -0.0017(11) C15 0.0123(15) 0.0142(15) 0.0192(16) -0.0005(12) 0.0076(12) 0.0021(12) C16 0.0106(15) 0.0264(18) 0.0142(15) -0.0056(13) 0.0023(12) -0.0002(13) C17 0.0195(17) 0.0259(18) 0.0170(17) -0.0091(13) 0.0071(14) -0.0088(14) C18 0.033(2) 0.0196(17) 0.0160(16) -0.0005(13) 0.0082(15) -0.0093(14) C19 0.0226(17) 0.0185(17) 0.0135(16) -0.0003(12) 0.0034(13) -0.0042(13) C20 0.0171(16) 0.0117(15) 0.0125(14) 0.0006(11) 0.0051(12) 0.0006(12) C21 0.0127(15) 0.0187(16) 0.0134(16) -0.0020(12) 0.0017(12) 0.0005(12) C22 0.0186(17) 0.0208(17) 0.0209(17) 0.0001(13) 0.0114(13) -0.0025(13) C23 0.0254(18) 0.0236(18) 0.0123(15) 0.0000(13) 0.0079(13) 0.0002(14) C24 0.0205(16) 0.0170(16) 0.0137(15) -0.0015(12) 0.0024(13) -0.0023(13) C25 0.0125(15) 0.0140(15) 0.0173(15) -0.0014(12) 0.0032(12) -0.0007(12) C26 0.0124(15) 0.0222(17) 0.0114(14) 0.0014(12) 0.0011(12) 0.0010(12) C27 0.0189(17) 0.0245(19) 0.0208(17) 0.0029(13) 0.0051(14) 0.0006(14) C28 0.036(2) 0.033(2) 0.0163(18) 0.0094(15) 0.0006(16) 0.0054(17) C29 0.035(2) 0.043(2) 0.0143(18) -0.0041(16) -0.0008(16) 0.0014(18) C30 0.0256(19) 0.0229(19) 0.0244(18) -0.0062(14) 0.0062(15) 0.0009(15) C31 0.0126(15) 0.0215(17) 0.0158(16) 0.0003(13) 0.0061(12) -0.0001(12) C32 0.0109(14) 0.0122(15) 0.0161(15) 0.0055(11) 0.0010(12) -0.0003(11) C33 0.0174(16) 0.0167(16) 0.0226(17) 0.0048(13) 0.0040(14) 0.0006(13) C34 0.0164(16) 0.0196(18) 0.034(2) 0.0121(15) 0.0072(15) 0.0008(13) C35 0.0114(16) 0.0169(17) 0.037(2) 0.0098(15) -0.0008(15) -0.0032(13) C36 0.0202(17) 0.0150(17) 0.0255(18) 0.0030(13) -0.0024(14) -0.0026(13) C37 0.0194(17) 0.0180(16) 0.0155(16) 0.0035(12) 0.0015(13) -0.0022(13) C38 0.051(3) 0.061(3) 0.054(3) 0.003(3) 0.027(3) 0.007(2) Cl1 0.0479(7) 0.0623(8) 0.0498(7) 0.0000(6) 0.0089(6) 0.0084(6) Cl2 0.1280(16) 0.0729(10) 0.1279(15) 0.0615(11) 0.0999(14) 0.0455(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 1.781(4) . ? Fe1 C3 1.796(4) . ? Fe1 C1 1.801(3) . ? Fe1 S1 2.2698(9) . ? Fe1 S2 2.2752(9) . ? Fe1 Fe2 2.5382(6) . ? Fe2 C4 1.753(3) . ? Fe2 P2 2.1843(9) . ? Fe2 P1 2.2008(9) . ? Fe2 S2 2.2587(9) . ? Fe2 S1 2.2616(9) . ? P1 C8 1.831(3) . ? P1 C20 1.834(3) . ? P1 C14 1.836(3) . ? P2 C32 1.827(3) . ? P2 C9 1.831(3) . ? P2 C26 1.837(3) . ? S1 C5 1.834(3) . ? S2 C7 1.826(3) . ? O1 C1 1.141(4) . ? O2 C2 1.140(4) . ? O3 C3 1.136(4) . ? O4 C4 1.157(4) . ? C5 C6 1.506(4) . ? C6 C7 1.513(4) . ? C8 C9 1.403(4) . ? C8 C13 1.403(4) . ? C9 C10 1.396(4) . ? C10 C11 1.371(5) . ? C11 C12 1.391(5) . ? C12 C13 1.386(5) . ? C14 C15 1.383(4) . ? C14 C19 1.403(5) . ? C15 C16 1.396(4) . ? C16 C17 1.368(5) . ? C17 C18 1.394(5) . ? C18 C19 1.388(5) . ? C20 C21 1.395(4) . ? C20 C25 1.396(4) . ? C21 C22 1.386(4) . ? C22 C23 1.388(5) . ? C23 C24 1.372(5) . ? C24 C25 1.385(4) . ? C26 C31 1.383(4) . ? C26 C27 1.402(4) . ? C27 C28 1.389(5) . ? C28 C29 1.371(6) . ? C29 C30 1.384(5) . ? C30 C31 1.387(5) . ? C32 C33 1.388(4) . ? C32 C37 1.406(5) . ? C33 C34 1.392(5) . ? C34 C35 1.385(5) . ? C35 C36 1.389(5) . ? C36 C37 1.386(5) . ? C38 Cl2 1.746(5) . ? C38 Cl1 1.764(6) . ? 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 90.40(16) . . ? C2 Fe1 C1 103.13(15) . . ? C3 Fe1 C1 98.78(16) . . ? C2 Fe1 S1 150.72(11) . . ? C3 Fe1 S1 87.65(11) . . ? C1 Fe1 S1 106.03(11) . . ? C2 Fe1 S2 87.63(12) . . ? C3 Fe1 S2 160.14(12) . . ? C1 Fe1 S2 100.91(11) . . ? S1 Fe1 S2 84.50(3) . . ? C2 Fe1 Fe2 96.87(11) . . ? C3 Fe1 Fe2 105.09(11) . . ? C1 Fe1 Fe2 148.61(11) . . ? S1 Fe1 Fe2 55.78(2) . . ? S2 Fe1 Fe2 55.65(2) . . ? C4 Fe2 P2 90.84(10) . . ? C4 Fe2 P1 89.14(10) . . ? P2 Fe2 P1 86.80(3) . . ? C4 Fe2 S2 86.85(10) . . ? P2 Fe2 S2 106.47(3) . . ? P1 Fe2 S2 166.17(3) . . ? C4 Fe2 S1 156.92(10) . . ? P2 Fe2 S1 112.18(3) . . ? P1 Fe2 S1 93.59(3) . . ? S2 Fe2 S1 85.07(3) . . ? C4 Fe2 Fe1 101.74(10) . . ? P2 Fe2 Fe1 157.34(3) . . ? P1 Fe2 Fe1 111.88(3) . . ? S2 Fe2 Fe1 56.26(3) . . ? S1 Fe2 Fe1 56.09(2) . . ? C8 P1 C20 104.20(14) . . ? C8 P1 C14 100.78(14) . . ? C20 P1 C14 101.43(14) . . ? C8 P1 Fe2 106.53(10) . . ? C20 P1 Fe2 121.40(11) . . ? C14 P1 Fe2 119.74(10) . . ? C32 P2 C9 105.15(14) . . ? C32 P2 C26 103.42(14) . . ? C9 P2 C26 100.82(14) . . ? C32 P2 Fe2 114.45(10) . . ? C9 P2 Fe2 106.64(10) . . ? C26 P2 Fe2 124.17(11) . . ? C5 S1 Fe2 114.58(11) . . ? C5 S1 Fe1 109.75(11) . . ? Fe2 S1 Fe1 68.13(3) . . ? C7 S2 Fe2 115.27(11) . . ? C7 S2 Fe1 109.75(11) . . ? Fe2 S2 Fe1 68.09(3) . . ? O1 C1 Fe1 177.6(3) . . ? O2 C2 Fe1 176.9(3) . . ? O3 C3 Fe1 179.1(3) . . ? O4 C4 Fe2 178.4(3) . . ? C6 C5 S1 116.4(2) . . ? C5 C6 C7 114.4(3) . . ? C6 C7 S2 115.8(2) . . ? C9 C8 C13 119.9(3) . . ? C9 C8 P1 115.7(2) . . ? C13 C8 P1 124.2(2) . . ? C10 C9 C8 119.0(3) . . ? C10 C9 P2 124.3(2) . . ? C8 C9 P2 116.4(2) . . ? C11 C10 C9 120.8(3) . . ? C10 C11 C12 120.4(3) . . ? C13 C12 C11 120.2(3) . . ? C12 C13 C8 119.6(3) . . ? C15 C14 C19 119.3(3) . . ? C15 C14 P1 121.5(2) . . ? C19 C14 P1 119.0(2) . . ? C14 C15 C16 120.4(3) . . ? C17 C16 C15 120.5(3) . . ? C16 C17 C18 119.4(3) . . ? C19 C18 C17 120.8(3) . . ? C18 C19 C14 119.3(3) . . ? C21 C20 C25 118.1(3) . . ? C21 C20 P1 121.8(2) . . ? C25 C20 P1 120.2(2) . . ? C22 C21 C20 120.9(3) . . ? C21 C22 C23 119.9(3) . . ? C24 C23 C22 119.8(3) . . ? C23 C24 C25 120.4(3) . . ? C24 C25 C20 120.8(3) . . ? C31 C26 C27 119.3(3) . . ? C31 C26 P2 119.1(2) . . ? C27 C26 P2 121.6(3) . . ? C28 C27 C26 119.1(3) . . ? C29 C28 C27 120.8(3) . . ? C28 C29 C30 120.6(3) . . ? C29 C30 C31 119.0(3) . . ? C26 C31 C30 121.2(3) . . ? C33 C32 C37 118.8(3) . . ? C33 C32 P2 120.1(2) . . ? C37 C32 P2 120.7(2) . . ? C32 C33 C34 121.1(3) . . ? C35 C34 C33 119.4(3) . . ? C34 C35 C36 120.5(3) . . ? C37 C36 C35 119.9(3) . . ? C36 C37 C32 120.3(3) . . ? Cl2 C38 Cl1 113.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Fe1 Fe2 C4 -4.28(15) . . . . ? C3 Fe1 Fe2 C4 -96.55(16) . . . . ? C1 Fe1 Fe2 C4 125.3(2) . . . . ? S1 Fe1 Fe2 C4 -172.98(11) . . . . ? S2 Fe1 Fe2 C4 78.09(10) . . . . ? C2 Fe1 Fe2 P2 -126.74(14) . . . . ? C3 Fe1 Fe2 P2 140.98(14) . . . . ? C1 Fe1 Fe2 P2 2.8(2) . . . . ? S1 Fe1 Fe2 P2 64.56(8) . . . . ? S2 Fe1 Fe2 P2 -44.37(8) . . . . ? C2 Fe1 Fe2 P1 89.56(12) . . . . ? C3 Fe1 Fe2 P1 -2.71(12) . . . . ? C1 Fe1 Fe2 P1 -140.9(2) . . . . ? S1 Fe1 Fe2 P1 -79.13(4) . . . . ? S2 Fe1 Fe2 P1 171.93(4) . . . . ? C2 Fe1 Fe2 S2 -82.37(12) . . . . ? C3 Fe1 Fe2 S2 -174.64(12) . . . . ? C1 Fe1 Fe2 S2 47.2(2) . . . . ? S1 Fe1 Fe2 S2 108.93(4) . . . . ? C2 Fe1 Fe2 S1 168.70(12) . . . . ? C3 Fe1 Fe2 S1 76.42(12) . . . . ? C1 Fe1 Fe2 S1 -61.8(2) . . . . ? S2 Fe1 Fe2 S1 -108.93(4) . . . . ? C4 Fe2 P1 C8 -66.72(14) . . . . ? P2 Fe2 P1 C8 24.17(10) . . . . ? S2 Fe2 P1 C8 -139.81(17) . . . . ? S1 Fe2 P1 C8 136.22(10) . . . . ? Fe1 Fe2 P1 C8 -169.03(10) . . . . ? C4 Fe2 P1 C20 52.03(16) . . . . ? P2 Fe2 P1 C20 142.92(12) . . . . ? S2 Fe2 P1 C20 -21.1(2) . . . . ? S1 Fe2 P1 C20 -105.04(12) . . . . ? Fe1 Fe2 P1 C20 -50.29(12) . . . . ? C4 Fe2 P1 C14 -179.94(15) . . . . ? P2 Fe2 P1 C14 -89.05(12) . . . . ? S2 Fe2 P1 C14 106.96(18) . . . . ? S1 Fe2 P1 C14 22.99(12) . . . . ? Fe1 Fe2 P1 C14 77.74(12) . . . . ? C4 Fe2 P2 C32 -50.78(15) . . . . ? P1 Fe2 P2 C32 -139.88(12) . . . . ? S2 Fe2 P2 C32 36.18(12) . . . . ? S1 Fe2 P2 C32 127.54(12) . . . . ? Fe1 Fe2 P2 C32 73.51(14) . . . . ? C4 Fe2 P2 C9 65.04(14) . . . . ? P1 Fe2 P2 C9 -24.06(11) . . . . ? S2 Fe2 P2 C9 152.00(10) . . . . ? S1 Fe2 P2 C9 -116.64(11) . . . . ? Fe1 Fe2 P2 C9 -170.67(11) . . . . ? C4 Fe2 P2 C26 -178.87(16) . . . . ? P1 Fe2 P2 C26 92.03(13) . . . . ? S2 Fe2 P2 C26 -91.91(13) . . . . ? S1 Fe2 P2 C26 -0.55(13) . . . . ? Fe1 Fe2 P2 C26 -54.58(16) . . . . ? C4 Fe2 S1 C5 120.3(3) . . . . ? P2 Fe2 S1 C5 -55.41(13) . . . . ? P1 Fe2 S1 C5 -143.42(12) . . . . ? S2 Fe2 S1 C5 50.38(12) . . . . ? Fe1 Fe2 S1 C5 102.52(12) . . . . ? C4 Fe2 S1 Fe1 17.8(3) . . . . ? P2 Fe2 S1 Fe1 -157.94(3) . . . . ? P1 Fe2 S1 Fe1 114.06(3) . . . . ? S2 Fe2 S1 Fe1 -52.14(3) . . . . ? C2 Fe1 S1 C5 -132.8(3) . . . . ? C3 Fe1 S1 C5 140.54(16) . . . . ? C1 Fe1 S1 C5 42.08(16) . . . . ? S2 Fe1 S1 C5 -57.72(12) . . . . ? Fe2 Fe1 S1 C5 -109.40(12) . . . . ? C2 Fe1 S1 Fe2 -23.4(2) . . . . ? C3 Fe1 S1 Fe2 -110.06(12) . . . . ? C1 Fe1 S1 Fe2 151.48(11) . . . . ? S2 Fe1 S1 Fe2 51.68(3) . . . . ? C4 Fe2 S2 C7 151.33(16) . . . . ? P2 Fe2 S2 C7 61.39(13) . . . . ? P1 Fe2 S2 C7 -135.31(18) . . . . ? S1 Fe2 S2 C7 -50.30(13) . . . . ? Fe1 Fe2 S2 C7 -102.30(13) . . . . ? C4 Fe2 S2 Fe1 -106.37(10) . . . . ? P2 Fe2 S2 Fe1 163.69(3) . . . . ? P1 Fe2 S2 Fe1 -33.01(15) . . . . ? S1 Fe2 S2 Fe1 51.99(3) . . . . ? C2 Fe1 S2 C7 -149.88(15) . . . . ? C3 Fe1 S2 C7 125.5(4) . . . . ? C1 Fe1 S2 C7 -46.96(16) . . . . ? S1 Fe1 S2 C7 58.35(12) . . . . ? Fe2 Fe1 S2 C7 110.14(12) . . . . ? C2 Fe1 S2 Fe2 99.98(11) . . . . ? C3 Fe1 S2 Fe2 15.4(3) . . . . ? C1 Fe1 S2 Fe2 -157.10(11) . . . . ? S1 Fe1 S2 Fe2 -51.79(3) . . . . ? C2 Fe1 C1 O1 -15(8) . . . . ? C3 Fe1 C1 O1 78(7) . . . . ? S1 Fe1 C1 O1 168(7) . . . . ? S2 Fe1 C1 O1 -105(7) . . . . ? Fe2 Fe1 C1 O1 -143(7) . . . . ? C3 Fe1 C2 O2 33(6) . . . . ? C1 Fe1 C2 O2 132(6) . . . . ? S1 Fe1 C2 O2 -53(6) . . . . ? S2 Fe1 C2 O2 -128(6) . . . . ? Fe2 Fe1 C2 O2 -73(6) . . . . ? C2 Fe1 C3 O3 95(23) . . . . ? C1 Fe1 C3 O3 -8(23) . . . . ? S1 Fe1 C3 O3 -114(23) . . . . ? S2 Fe1 C3 O3 180(100) . . . . ? Fe2 Fe1 C3 O3 -167(100) . . . . ? P2 Fe2 C4 O4 95(11) . . . . ? P1 Fe2 C4 O4 -178(100) . . . . ? S2 Fe2 C4 O4 -11(10) . . . . ? S1 Fe2 C4 O4 -81(11) . . . . ? Fe1 Fe2 C4 O4 -66(11) . . . . ? Fe2 S1 C5 C6 -6.4(3) . . . . ? Fe1 S1 C5 C6 67.9(3) . . . . ? S1 C5 C6 C7 -61.8(3) . . . . ? C5 C6 C7 S2 62.2(3) . . . . ? Fe2 S2 C7 C6 5.8(3) . . . . ? Fe1 S2 C7 C6 -68.6(3) . . . . ? C20 P1 C8 C9 -148.8(2) . . . . ? C14 P1 C8 C9 106.4(2) . . . . ? Fe2 P1 C8 C9 -19.3(2) . . . . ? C20 P1 C8 C13 35.3(3) . . . . ? C14 P1 C8 C13 -69.6(3) . . . . ? Fe2 P1 C8 C13 164.8(2) . . . . ? C13 C8 C9 C10 1.5(5) . . . . ? P1 C8 C9 C10 -174.6(2) . . . . ? C13 C8 C9 P2 176.2(2) . . . . ? P1 C8 C9 P2 0.1(3) . . . . ? C32 P2 C9 C10 -44.3(3) . . . . ? C26 P2 C9 C10 62.9(3) . . . . ? Fe2 P2 C9 C10 -166.3(3) . . . . ? C32 P2 C9 C8 141.2(2) . . . . ? C26 P2 C9 C8 -111.6(2) . . . . ? Fe2 P2 C9 C8 19.3(3) . . . . ? C8 C9 C10 C11 -0.7(5) . . . . ? P2 C9 C10 C11 -175.1(3) . . . . ? C9 C10 C11 C12 -0.6(5) . . . . ? C10 C11 C12 C13 1.2(5) . . . . ? C11 C12 C13 C8 -0.5(5) . . . . ? C9 C8 C13 C12 -0.9(4) . . . . ? P1 C8 C13 C12 174.9(2) . . . . ? C8 P1 C14 C15 -28.5(3) . . . . ? C20 P1 C14 C15 -135.6(3) . . . . ? Fe2 P1 C14 C15 87.7(3) . . . . ? C8 P1 C14 C19 155.1(3) . . . . ? C20 P1 C14 C19 48.1(3) . . . . ? Fe2 P1 C14 C19 -88.6(3) . . . . ? C19 C14 C15 C16 -2.3(5) . . . . ? P1 C14 C15 C16 -178.6(2) . . . . ? C14 C15 C16 C17 -0.5(5) . . . . ? C15 C16 C17 C18 1.6(5) . . . . ? C16 C17 C18 C19 0.1(5) . . . . ? C17 C18 C19 C14 -2.9(5) . . . . ? C15 C14 C19 C18 4.0(5) . . . . ? P1 C14 C19 C18 -179.6(3) . . . . ? C8 P1 C20 C21 -71.2(3) . . . . ? C14 P1 C20 C21 33.2(3) . . . . ? Fe2 P1 C20 C21 168.9(2) . . . . ? C8 P1 C20 C25 108.7(3) . . . . ? C14 P1 C20 C25 -146.9(3) . . . . ? Fe2 P1 C20 C25 -11.2(3) . . . . ? C25 C20 C21 C22 0.5(5) . . . . ? P1 C20 C21 C22 -179.6(3) . . . . ? C20 C21 C22 C23 -0.8(5) . . . . ? C21 C22 C23 C24 0.2(5) . . . . ? C22 C23 C24 C25 0.7(5) . . . . ? C23 C24 C25 C20 -0.9(5) . . . . ? C21 C20 C25 C24 0.3(5) . . . . ? P1 C20 C25 C24 -179.6(2) . . . . ? C32 P2 C26 C31 -155.2(3) . . . . ? C9 P2 C26 C31 96.2(3) . . . . ? Fe2 P2 C26 C31 -22.6(3) . . . . ? C32 P2 C26 C27 27.7(3) . . . . ? C9 P2 C26 C27 -80.9(3) . . . . ? Fe2 P2 C26 C27 160.3(2) . . . . ? C31 C26 C27 C28 -0.3(5) . . . . ? P2 C26 C27 C28 176.8(3) . . . . ? C26 C27 C28 C29 -0.9(6) . . . . ? C27 C28 C29 C30 0.3(6) . . . . ? C28 C29 C30 C31 1.4(6) . . . . ? C27 C26 C31 C30 2.0(5) . . . . ? P2 C26 C31 C30 -175.2(3) . . . . ? C29 C30 C31 C26 -2.5(5) . . . . ? C9 P2 C32 C33 150.0(2) . . . . ? C26 P2 C32 C33 44.7(3) . . . . ? Fe2 P2 C32 C33 -93.3(2) . . . . ? C9 P2 C32 C37 -37.3(3) . . . . ? C26 P2 C32 C37 -142.7(3) . . . . ? Fe2 P2 C32 C37 79.4(3) . . . . ? C37 C32 C33 C34 1.2(5) . . . . ? P2 C32 C33 C34 173.9(2) . . . . ? C32 C33 C34 C35 -1.2(5) . . . . ? C33 C34 C35 C36 0.3(5) . . . . ? C34 C35 C36 C37 0.6(5) . . . . ? C35 C36 C37 C32 -0.6(5) . . . . ? C33 C32 C37 C36 -0.3(5) . . . . ? P2 C32 C37 C36 -173.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.050 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.084 #===END data_str0505 _database_code_depnum_ccdc_archive 'CCDC 639868' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H32 Fe2 O4 P2 S2' _chemical_formula_weight 742.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p_-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4973(8) _cell_length_b 11.1050(8) _cell_length_c 16.5294(12) _cell_angle_alpha 73.689(1) _cell_angle_beta 84.670(1) _cell_angle_gamma 61.833(1) _cell_volume 1628.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 1.155 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7380 _exptl_absorpt_correction_T_max 0.8738 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14343 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.25 _reflns_number_total 7449 _reflns_number_gt 6774 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+0.6386P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7449 _refine_ls_number_parameters 525 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0694 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.71273(2) 0.92035(2) 0.279747(13) 0.01408(6) Uani 1 1 d . . . Fe2 Fe 0.89726(2) 1.01297(2) 0.233344(14) 0.01762(6) Uani 1 1 d . . . P1 P 0.49330(4) 1.10008(4) 0.28071(2) 0.01654(8) Uani 1 1 d . . . P2 P 0.63563(4) 0.76251(4) 0.29228(2) 0.01578(8) Uani 1 1 d . . . S1 S 0.74493(4) 1.01504(4) 0.14410(2) 0.01700(8) Uani 1 1 d . . . S2 S 0.95412(4) 0.78146(4) 0.28651(2) 0.01840(8) Uani 1 1 d . . . O1 O 0.72757(14) 0.87317(14) 0.46108(7) 0.0297(3) Uani 1 1 d . . . O2 O 1.14660(16) 0.98837(17) 0.13056(10) 0.0410(3) Uani 1 1 d . . . O3 O 0.74143(16) 1.32333(14) 0.17591(10) 0.0410(4) Uani 1 1 d . . . O4 O 0.99277(15) 0.99178(15) 0.40064(8) 0.0350(3) Uani 1 1 d . . . C1 C 0.72145(17) 0.89163(16) 0.38882(10) 0.0194(3) Uani 1 1 d . . . C2 C 1.05082(18) 0.99651(18) 0.17097(11) 0.0243(3) Uani 1 1 d . . . C3 C 0.80060(19) 1.20244(19) 0.20094(11) 0.0261(4) Uani 1 1 d . . . C4 C 0.95526(18) 1.00173(18) 0.33500(11) 0.0235(3) Uani 1 1 d . . . C5 C 0.85479(19) 0.88779(18) 0.08363(10) 0.0229(3) Uani 1 1 d . . . C6 C 0.91771(19) 0.73300(18) 0.13227(11) 0.0243(3) Uani 1 1 d . . . C7 C 1.02379(18) 0.68854(18) 0.20412(12) 0.0253(3) Uani 1 1 d . . . C8 C 0.36853(18) 1.04701(18) 0.34912(11) 0.0228(3) Uani 1 1 d . . . C9 C 0.35689(18) 0.91716(19) 0.34450(12) 0.0248(3) Uani 1 1 d . . . C10 C 0.49652(18) 0.77725(18) 0.37045(10) 0.0212(3) Uani 1 1 d . . . C11 C 0.38571(17) 1.21380(16) 0.18208(10) 0.0201(3) Uani 1 1 d . . . C12 C 0.41371(19) 1.32251(19) 0.13305(11) 0.0259(4) Uani 1 1 d . . . C13 C 0.3305(2) 1.4145(2) 0.05986(12) 0.0319(4) Uani 1 1 d . . . C14 C 0.2188(2) 1.3984(2) 0.03425(12) 0.0360(5) Uani 1 1 d . . . C15 C 0.1919(2) 1.2902(2) 0.08140(14) 0.0391(5) Uani 1 1 d . . . C16 C 0.2747(2) 1.1982(2) 0.15511(12) 0.0317(4) Uani 1 1 d . . . C17 C 0.47420(17) 1.23826(16) 0.32966(10) 0.0196(3) Uani 1 1 d . . . C18 C 0.58999(18) 1.22890(18) 0.37005(10) 0.0222(3) Uani 1 1 d . . . C19 C 0.5697(2) 1.32956(19) 0.41168(11) 0.0246(3) Uani 1 1 d . . . C20 C 0.4325(2) 1.43923(18) 0.41353(10) 0.0250(4) Uani 1 1 d . . . C21 C 0.3163(2) 1.45093(18) 0.37281(11) 0.0267(4) Uani 1 1 d . . . C22 C 0.33687(19) 1.35136(18) 0.33091(11) 0.0246(3) Uani 1 1 d . . . C23 C 0.77357(17) 0.57806(16) 0.33552(10) 0.0186(3) Uani 1 1 d . . . C24 C 0.83194(19) 0.48039(18) 0.28786(10) 0.0226(3) Uani 1 1 d . . . C25 C 0.93796(19) 0.34205(18) 0.32331(12) 0.0259(4) Uani 1 1 d . . . C26 C 0.98571(19) 0.29994(18) 0.40675(12) 0.0273(4) Uani 1 1 d . . . C27 C 0.92950(19) 0.39673(19) 0.45442(11) 0.0269(4) Uani 1 1 d . . . C28 C 0.82518(18) 0.53486(18) 0.41920(11) 0.0233(3) Uani 1 1 d . . . C29 C 0.55036(16) 0.75253(16) 0.20429(10) 0.0182(3) Uani 1 1 d . . . C30 C 0.49697(19) 0.65487(18) 0.21677(11) 0.0237(3) Uani 1 1 d . . . C31 C 0.42906(19) 0.64971(18) 0.15067(12) 0.0256(3) Uani 1 1 d . . . C32 C 0.41549(19) 0.74013(19) 0.07107(11) 0.0255(3) Uani 1 1 d . . . C33 C 0.46891(19) 0.83627(19) 0.05782(11) 0.0248(3) Uani 1 1 d . . . C34 C 0.53378(17) 0.84409(17) 0.12432(10) 0.0200(3) Uani 1 1 d . . . H5A H 0.931(2) 0.915(2) 0.0595(13) 0.027(5) Uiso 1 1 d . . . H5B H 0.790(2) 0.909(2) 0.0371(13) 0.026(5) Uiso 1 1 d . . . H6A H 0.966(2) 0.675(2) 0.0945(14) 0.035(6) Uiso 1 1 d . . . H6B H 0.841(2) 0.711(2) 0.1531(13) 0.026(5) Uiso 1 1 d . . . H7A H 1.108(2) 0.701(2) 0.1842(14) 0.032(6) Uiso 1 1 d . . . H7B H 1.056(2) 0.588(2) 0.2343(14) 0.038(6) Uiso 1 1 d . . . H8A H 0.273(2) 1.127(2) 0.3396(13) 0.030(5) Uiso 1 1 d . . . H8B H 0.400(2) 1.031(2) 0.4071(14) 0.029(5) Uiso 1 1 d . . . H9A H 0.324(2) 0.926(2) 0.2910(13) 0.021(5) Uiso 1 1 d . . . H9B H 0.284(2) 0.908(2) 0.3813(14) 0.034(6) Uiso 1 1 d . . . H10A H 0.535(2) 0.772(2) 0.4216(13) 0.025(5) Uiso 1 1 d . . . H10B H 0.477(2) 0.697(2) 0.3774(12) 0.024(5) Uiso 1 1 d . . . H12 H 0.489(2) 1.334(2) 0.1481(14) 0.035(6) Uiso 1 1 d . . . H13 H 0.346(3) 1.486(3) 0.0274(15) 0.039(6) Uiso 1 1 d . . . H14 H 0.160(3) 1.461(3) -0.0136(15) 0.044(6) Uiso 1 1 d . . . H15 H 0.118(3) 1.278(3) 0.0638(16) 0.054(7) Uiso 1 1 d . . . H16 H 0.252(2) 1.128(3) 0.1871(15) 0.039(6) Uiso 1 1 d . . . H18 H 0.681(2) 1.154(2) 0.3679(13) 0.026(5) Uiso 1 1 d . . . H19 H 0.648(2) 1.323(2) 0.4364(13) 0.025(5) Uiso 1 1 d . . . H20 H 0.423(2) 1.501(2) 0.4439(14) 0.036(6) Uiso 1 1 d . . . H21 H 0.226(2) 1.525(2) 0.3733(13) 0.033(6) Uiso 1 1 d . . . H22 H 0.257(2) 1.358(2) 0.3040(13) 0.026(5) Uiso 1 1 d . . . H24 H 0.800(2) 0.502(2) 0.2335(14) 0.029(5) Uiso 1 1 d . . . H25 H 0.974(2) 0.279(2) 0.2904(13) 0.030(5) Uiso 1 1 d . . . H26 H 1.055(3) 0.204(3) 0.4313(14) 0.040(6) Uiso 1 1 d . . . H27 H 0.959(2) 0.371(2) 0.5107(14) 0.033(6) Uiso 1 1 d . . . H28 H 0.788(2) 0.603(2) 0.4511(12) 0.021(5) Uiso 1 1 d . . . H30 H 0.508(2) 0.591(2) 0.2687(13) 0.027(5) Uiso 1 1 d . . . H31 H 0.394(2) 0.586(2) 0.1597(13) 0.029(5) Uiso 1 1 d . . . H32 H 0.371(2) 0.737(2) 0.0266(14) 0.035(6) Uiso 1 1 d . . . H33 H 0.464(2) 0.897(2) 0.0033(14) 0.030(5) Uiso 1 1 d . . . H34 H 0.569(2) 0.912(2) 0.1158(13) 0.029(5) 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 0.01345(10) 0.01375(11) 0.01284(10) -0.00310(8) -0.00083(8) -0.00462(8) Fe2 0.01589(11) 0.01835(11) 0.01919(12) -0.00556(9) 0.00012(8) -0.00806(9) P1 0.01437(18) 0.01581(18) 0.01647(18) -0.00516(15) -0.00119(14) -0.00392(15) P2 0.01744(18) 0.01470(18) 0.01317(17) -0.00164(14) -0.00100(14) -0.00674(15) S1 0.01715(17) 0.01730(18) 0.01477(17) -0.00340(14) -0.00041(13) -0.00694(14) S2 0.01477(17) 0.01693(18) 0.01933(18) -0.00433(14) -0.00209(14) -0.00390(14) O1 0.0332(7) 0.0329(7) 0.0170(6) -0.0063(5) -0.0022(5) -0.0103(6) O2 0.0356(8) 0.0522(9) 0.0442(8) -0.0181(7) 0.0177(7) -0.0277(7) O3 0.0436(8) 0.0204(7) 0.0554(9) -0.0064(6) -0.0155(7) -0.0109(6) O4 0.0379(7) 0.0423(8) 0.0287(7) -0.0123(6) -0.0054(6) -0.0191(6) C1 0.0172(7) 0.0166(7) 0.0212(8) -0.0051(6) -0.0009(6) -0.0049(6) C2 0.0236(8) 0.0246(8) 0.0273(8) -0.0082(7) 0.0005(7) -0.0126(7) C3 0.0247(8) 0.0277(9) 0.0305(9) -0.0111(7) -0.0032(7) -0.0133(7) C4 0.0201(8) 0.0221(8) 0.0288(9) -0.0079(7) 0.0006(6) -0.0096(6) C5 0.0236(8) 0.0271(8) 0.0179(8) -0.0096(7) 0.0039(6) -0.0103(7) C6 0.0232(8) 0.0245(8) 0.0247(8) -0.0130(7) 0.0029(7) -0.0076(7) C7 0.0200(8) 0.0207(8) 0.0301(9) -0.0117(7) 0.0005(7) -0.0028(6) C8 0.0172(7) 0.0250(8) 0.0233(8) -0.0091(7) 0.0052(6) -0.0069(7) C9 0.0185(8) 0.0286(9) 0.0267(9) -0.0069(7) 0.0041(7) -0.0115(7) C10 0.0224(8) 0.0233(8) 0.0181(8) -0.0039(6) 0.0032(6) -0.0122(7) C11 0.0183(7) 0.0166(7) 0.0196(7) -0.0060(6) -0.0030(6) -0.0022(6) C12 0.0239(8) 0.0248(8) 0.0245(8) -0.0053(7) -0.0030(7) -0.0079(7) C13 0.0375(10) 0.0230(9) 0.0248(9) -0.0004(7) -0.0039(8) -0.0083(8) C14 0.0382(11) 0.0281(10) 0.0268(9) -0.0036(8) -0.0152(8) -0.0029(8) C15 0.0385(11) 0.0367(11) 0.0390(11) -0.0040(9) -0.0205(9) -0.0146(9) C16 0.0347(10) 0.0270(9) 0.0320(10) -0.0025(8) -0.0125(8) -0.0137(8) C17 0.0221(8) 0.0158(7) 0.0170(7) -0.0050(6) -0.0001(6) -0.0054(6) C18 0.0218(8) 0.0217(8) 0.0211(8) -0.0070(6) 0.0023(6) -0.0082(7) C19 0.0302(9) 0.0278(9) 0.0204(8) -0.0070(7) 0.0015(7) -0.0169(7) C20 0.0396(10) 0.0197(8) 0.0175(8) -0.0066(6) 0.0057(7) -0.0152(7) C21 0.0286(9) 0.0172(8) 0.0244(8) -0.0064(7) 0.0012(7) -0.0024(7) C22 0.0219(8) 0.0211(8) 0.0238(8) -0.0071(7) -0.0032(6) -0.0032(7) C23 0.0186(7) 0.0161(7) 0.0193(7) -0.0012(6) -0.0015(6) -0.0083(6) C24 0.0266(8) 0.0220(8) 0.0184(8) -0.0044(6) -0.0021(6) -0.0109(7) C25 0.0263(8) 0.0202(8) 0.0293(9) -0.0092(7) -0.0009(7) -0.0077(7) C26 0.0239(8) 0.0192(8) 0.0303(9) -0.0024(7) -0.0062(7) -0.0043(7) C27 0.0271(9) 0.0249(9) 0.0212(8) -0.0011(7) -0.0068(7) -0.0076(7) C28 0.0252(8) 0.0215(8) 0.0198(8) -0.0042(6) -0.0024(6) -0.0084(7) C29 0.0184(7) 0.0175(7) 0.0173(7) -0.0041(6) -0.0009(6) -0.0073(6) C30 0.0270(8) 0.0221(8) 0.0211(8) -0.0003(7) -0.0029(6) -0.0131(7) C31 0.0259(8) 0.0235(8) 0.0311(9) -0.0077(7) -0.0017(7) -0.0137(7) C32 0.0246(8) 0.0280(9) 0.0245(8) -0.0095(7) -0.0040(7) -0.0107(7) C33 0.0258(8) 0.0272(9) 0.0180(8) -0.0016(7) -0.0039(6) -0.0113(7) C34 0.0197(7) 0.0201(8) 0.0189(7) -0.0019(6) -0.0006(6) -0.0098(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 1.7438(16) . ? Fe1 P2 2.2077(5) . ? Fe1 P1 2.2272(4) . ? Fe1 S2 2.2535(4) . ? Fe1 S1 2.2622(4) . ? Fe1 Fe2 2.5614(3) . ? Fe2 C3 1.7877(18) . ? Fe2 C4 1.7917(18) . ? Fe2 C2 1.7927(17) . ? Fe2 S1 2.2623(4) . ? Fe2 S2 2.2623(5) . ? P1 C11 1.8351(16) . ? P1 C8 1.8495(17) . ? P1 C17 1.8509(16) . ? P2 C29 1.8317(16) . ? P2 C10 1.8362(16) . ? P2 C23 1.8365(16) . ? S1 C5 1.8349(17) . ? S2 C7 1.8292(17) . ? O1 C1 1.156(2) . ? O2 C2 1.135(2) . ? O3 C3 1.144(2) . ? O4 C4 1.147(2) . ? C5 C6 1.513(2) . ? C6 C7 1.514(2) . ? C8 C9 1.526(2) . ? C9 C10 1.529(2) . ? C11 C16 1.385(2) . ? C11 C12 1.393(2) . ? C12 C13 1.389(2) . ? C13 C14 1.385(3) . ? C14 C15 1.373(3) . ? C15 C16 1.394(3) . ? C17 C18 1.388(2) . ? C17 C22 1.398(2) . ? C18 C19 1.396(2) . ? C19 C20 1.384(3) . ? C20 C21 1.382(3) . ? C21 C22 1.388(2) . ? C23 C24 1.391(2) . ? C23 C28 1.399(2) . ? C24 C25 1.394(2) . ? C25 C26 1.385(2) . ? C26 C27 1.384(3) . ? C27 C28 1.386(2) . ? C29 C34 1.390(2) . ? C29 C30 1.400(2) . ? C30 C31 1.387(2) . ? C31 C32 1.385(3) . ? C32 C33 1.383(2) . ? C33 C34 1.389(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 P2 92.01(5) . . ? C1 Fe1 P1 86.49(5) . . ? P2 Fe1 P1 94.959(18) . . ? C1 Fe1 S2 88.37(5) . . ? P2 Fe1 S2 100.840(17) . . ? P1 Fe1 S2 163.544(18) . . ? C1 Fe1 S1 155.21(6) . . ? P2 Fe1 S1 112.642(17) . . ? P1 Fe1 S1 93.554(16) . . ? S2 Fe1 S1 84.645(15) . . ? C1 Fe1 Fe2 101.27(5) . . ? P2 Fe1 Fe2 151.996(15) . . ? P1 Fe1 Fe2 110.233(15) . . ? S2 Fe1 Fe2 55.608(13) . . ? S1 Fe1 Fe2 55.522(12) . . ? C3 Fe2 C4 95.25(8) . . ? C3 Fe2 C2 96.17(8) . . ? C4 Fe2 C2 103.18(8) . . ? C3 Fe2 S1 87.09(5) . . ? C4 Fe2 S1 153.41(6) . . ? C2 Fe2 S1 102.88(6) . . ? C3 Fe2 S2 163.02(6) . . ? C4 Fe2 S2 85.96(5) . . ? C2 Fe2 S2 100.05(6) . . ? S1 Fe2 S2 84.440(15) . . ? C3 Fe2 Fe1 107.92(6) . . ? C4 Fe2 Fe1 98.96(5) . . ? C2 Fe2 Fe1 145.45(6) . . ? S1 Fe2 Fe1 55.519(12) . . ? S2 Fe2 Fe1 55.283(12) . . ? C11 P1 C8 104.06(8) . . ? C11 P1 C17 99.53(7) . . ? C8 P1 C17 96.48(8) . . ? C11 P1 Fe1 120.88(5) . . ? C8 P1 Fe1 113.65(6) . . ? C17 P1 Fe1 118.50(5) . . ? C29 P2 C10 100.28(8) . . ? C29 P2 C23 103.05(7) . . ? C10 P2 C23 100.87(7) . . ? C29 P2 Fe1 122.99(5) . . ? C10 P2 Fe1 112.58(6) . . ? C23 P2 Fe1 114.08(5) . . ? C5 S1 Fe2 107.47(6) . . ? C5 S1 Fe1 115.93(6) . . ? Fe2 S1 Fe1 68.959(14) . . ? C7 S2 Fe1 115.44(6) . . ? C7 S2 Fe2 110.17(6) . . ? Fe1 S2 Fe2 69.110(13) . . ? O1 C1 Fe1 179.58(16) . . ? O2 C2 Fe2 178.80(18) . . ? O3 C3 Fe2 176.27(18) . . ? O4 C4 Fe2 178.61(15) . . ? C6 C5 S1 115.59(12) . . ? C5 C6 C7 114.59(15) . . ? C6 C7 S2 116.18(12) . . ? C9 C8 P1 119.74(12) . . ? C8 C9 C10 114.41(14) . . ? C9 C10 P2 112.68(11) . . ? C16 C11 C12 118.30(16) . . ? C16 C11 P1 122.52(13) . . ? C12 C11 P1 119.16(13) . . ? C13 C12 C11 120.78(17) . . ? C14 C13 C12 120.18(19) . . ? C15 C14 C13 119.46(17) . . ? C14 C15 C16 120.49(19) . . ? C11 C16 C15 120.78(19) . . ? C18 C17 C22 118.62(15) . . ? C18 C17 P1 122.24(12) . . ? C22 C17 P1 119.01(13) . . ? C17 C18 C19 120.73(16) . . ? C20 C19 C18 119.77(17) . . ? C21 C20 C19 120.19(16) . . ? C20 C21 C22 119.97(16) . . ? C21 C22 C17 120.70(16) . . ? C24 C23 C28 118.52(14) . . ? C24 C23 P2 122.75(12) . . ? C28 C23 P2 118.70(12) . . ? C23 C24 C25 120.55(15) . . ? C26 C25 C24 120.28(16) . . ? C27 C26 C25 119.62(16) . . ? C26 C27 C28 120.33(16) . . ? C27 C28 C23 120.68(16) . . ? C34 C29 C30 118.58(15) . . ? C34 C29 P2 120.81(12) . . ? C30 C29 P2 120.59(12) . . ? C31 C30 C29 120.63(16) . . ? C32 C31 C30 120.07(16) . . ? C33 C32 C31 119.82(16) . . ? C32 C33 C34 120.25(16) . . ? C33 C34 C29 120.62(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Fe1 Fe2 C3 -97.10(8) . . . . ? P2 Fe1 Fe2 C3 146.08(7) . . . . ? P1 Fe1 Fe2 C3 -6.70(6) . . . . ? S2 Fe1 Fe2 C3 -177.22(6) . . . . ? S1 Fe1 Fe2 C3 73.34(6) . . . . ? C1 Fe1 Fe2 C4 1.43(7) . . . . ? P2 Fe1 Fe2 C4 -115.39(6) . . . . ? P1 Fe1 Fe2 C4 91.82(6) . . . . ? S2 Fe1 Fe2 C4 -78.69(6) . . . . ? S1 Fe1 Fe2 C4 171.86(6) . . . . ? C1 Fe1 Fe2 C2 130.94(11) . . . . ? P2 Fe1 Fe2 C2 14.11(11) . . . . ? P1 Fe1 Fe2 C2 -138.67(10) . . . . ? S2 Fe1 Fe2 C2 50.82(10) . . . . ? S1 Fe1 Fe2 C2 -58.63(10) . . . . ? C1 Fe1 Fe2 S1 -170.44(5) . . . . ? P2 Fe1 Fe2 S1 72.74(3) . . . . ? P1 Fe1 Fe2 S1 -80.040(18) . . . . ? S2 Fe1 Fe2 S1 109.444(18) . . . . ? C1 Fe1 Fe2 S2 80.12(5) . . . . ? P2 Fe1 Fe2 S2 -36.70(3) . . . . ? P1 Fe1 Fe2 S2 170.516(19) . . . . ? S1 Fe1 Fe2 S2 -109.444(18) . . . . ? C1 Fe1 P1 C11 177.80(8) . . . . ? P2 Fe1 P1 C11 -90.48(7) . . . . ? S2 Fe1 P1 C11 105.76(9) . . . . ? S1 Fe1 P1 C11 22.64(7) . . . . ? Fe2 Fe1 P1 C11 77.08(7) . . . . ? C1 Fe1 P1 C8 -57.38(8) . . . . ? P2 Fe1 P1 C8 34.34(6) . . . . ? S2 Fe1 P1 C8 -129.42(8) . . . . ? S1 Fe1 P1 C8 147.45(6) . . . . ? Fe2 Fe1 P1 C8 -158.11(6) . . . . ? C1 Fe1 P1 C17 54.83(8) . . . . ? P2 Fe1 P1 C17 146.55(6) . . . . ? S2 Fe1 P1 C17 -17.22(9) . . . . ? S1 Fe1 P1 C17 -100.34(6) . . . . ? Fe2 Fe1 P1 C17 -45.90(6) . . . . ? C1 Fe1 P2 C29 163.41(8) . . . . ? P1 Fe1 P2 C29 76.76(6) . . . . ? S2 Fe1 P2 C29 -107.86(6) . . . . ? S1 Fe1 P2 C29 -19.19(6) . . . . ? Fe2 Fe1 P2 C29 -77.72(7) . . . . ? C1 Fe1 P2 C10 43.38(8) . . . . ? P1 Fe1 P2 C10 -43.26(6) . . . . ? S2 Fe1 P2 C10 132.11(6) . . . . ? S1 Fe1 P2 C10 -139.21(6) . . . . ? Fe2 Fe1 P2 C10 162.25(6) . . . . ? C1 Fe1 P2 C23 -70.80(8) . . . . ? P1 Fe1 P2 C23 -157.44(6) . . . . ? S2 Fe1 P2 C23 17.93(6) . . . . ? S1 Fe1 P2 C23 106.61(6) . . . . ? Fe2 Fe1 P2 C23 48.07(7) . . . . ? C3 Fe2 S1 C5 134.16(8) . . . . ? C4 Fe2 S1 C5 -129.93(13) . . . . ? C2 Fe2 S1 C5 38.50(8) . . . . ? S2 Fe2 S1 C5 -60.58(6) . . . . ? Fe1 Fe2 S1 C5 -111.72(6) . . . . ? C3 Fe2 S1 Fe1 -114.12(6) . . . . ? C4 Fe2 S1 Fe1 -18.20(12) . . . . ? C2 Fe2 S1 Fe1 150.22(6) . . . . ? S2 Fe2 S1 Fe1 51.147(13) . . . . ? C1 Fe1 S1 C5 122.70(14) . . . . ? P2 Fe1 S1 C5 -51.10(7) . . . . ? P1 Fe1 S1 C5 -147.98(7) . . . . ? S2 Fe1 S1 C5 48.43(7) . . . . ? Fe2 Fe1 S1 C5 99.83(7) . . . . ? C1 Fe1 S1 Fe2 22.87(12) . . . . ? P2 Fe1 S1 Fe2 -150.932(16) . . . . ? P1 Fe1 S1 Fe2 112.190(16) . . . . ? S2 Fe1 S1 Fe2 -51.402(14) . . . . ? C1 Fe1 S2 C7 152.01(9) . . . . ? P2 Fe1 S2 C7 60.27(7) . . . . ? P1 Fe1 S2 C7 -136.21(9) . . . . ? S1 Fe1 S2 C7 -51.80(7) . . . . ? Fe2 Fe1 S2 C7 -103.13(7) . . . . ? C1 Fe1 S2 Fe2 -104.86(5) . . . . ? P2 Fe1 S2 Fe2 163.398(15) . . . . ? P1 Fe1 S2 Fe2 -33.08(6) . . . . ? S1 Fe1 S2 Fe2 51.328(13) . . . . ? C3 Fe2 S2 C7 119.5(2) . . . . ? C4 Fe2 S2 C7 -145.72(8) . . . . ? C2 Fe2 S2 C7 -43.03(8) . . . . ? S1 Fe2 S2 C7 59.11(6) . . . . ? Fe1 Fe2 S2 C7 110.46(6) . . . . ? C3 Fe2 S2 Fe1 9.1(2) . . . . ? C4 Fe2 S2 Fe1 103.82(5) . . . . ? C2 Fe2 S2 Fe1 -153.49(6) . . . . ? S1 Fe2 S2 Fe1 -51.350(14) . . . . ? P2 Fe1 C1 O1 177(100) . . . . ? P1 Fe1 C1 O1 -88(30) . . . . ? S2 Fe1 C1 O1 76(30) . . . . ? S1 Fe1 C1 O1 3(30) . . . . ? Fe2 Fe1 C1 O1 22(30) . . . . ? C3 Fe2 C2 O2 -23(8) . . . . ? C4 Fe2 C2 O2 -120(8) . . . . ? S1 Fe2 C2 O2 66(8) . . . . ? S2 Fe2 C2 O2 152(8) . . . . ? Fe1 Fe2 C2 O2 112(8) . . . . ? C4 Fe2 C3 O3 142(2) . . . . ? C2 Fe2 C3 O3 38(2) . . . . ? S1 Fe2 C3 O3 -65(2) . . . . ? S2 Fe2 C3 O3 -125(2) . . . . ? Fe1 Fe2 C3 O3 -117(2) . . . . ? C3 Fe2 C4 O4 158(7) . . . . ? C2 Fe2 C4 O4 -104(7) . . . . ? S1 Fe2 C4 O4 64(7) . . . . ? S2 Fe2 C4 O4 -5(7) . . . . ? Fe1 Fe2 C4 O4 49(7) . . . . ? Fe2 S1 C5 C6 71.92(13) . . . . ? Fe1 S1 C5 C6 -2.68(15) . . . . ? S1 C5 C6 C7 -63.26(18) . . . . ? C5 C6 C7 S2 59.38(19) . . . . ? Fe1 S2 C7 C6 10.03(16) . . . . ? Fe2 S2 C7 C6 -65.73(15) . . . . ? C11 P1 C8 C9 86.73(14) . . . . ? C17 P1 C8 C9 -171.72(14) . . . . ? Fe1 P1 C8 C9 -46.69(15) . . . . ? P1 C8 C9 C10 63.19(19) . . . . ? C8 C9 C10 P2 -71.59(17) . . . . ? C29 P2 C10 C9 -67.11(13) . . . . ? C23 P2 C10 C9 -172.69(12) . . . . ? Fe1 P2 C10 C9 65.32(13) . . . . ? C8 P1 C11 C16 -28.49(17) . . . . ? C17 P1 C11 C16 -127.70(16) . . . . ? Fe1 P1 C11 C16 100.68(15) . . . . ? C8 P1 C11 C12 149.91(13) . . . . ? C17 P1 C11 C12 50.70(14) . . . . ? Fe1 P1 C11 C12 -80.92(14) . . . . ? C16 C11 C12 C13 1.2(3) . . . . ? P1 C11 C12 C13 -177.25(14) . . . . ? C11 C12 C13 C14 -0.5(3) . . . . ? C12 C13 C14 C15 -0.5(3) . . . . ? C13 C14 C15 C16 0.9(3) . . . . ? C12 C11 C16 C15 -0.9(3) . . . . ? P1 C11 C16 C15 177.55(16) . . . . ? C14 C15 C16 C11 -0.2(3) . . . . ? C11 P1 C17 C18 -137.14(14) . . . . ? C8 P1 C17 C18 117.38(14) . . . . ? Fe1 P1 C17 C18 -4.03(16) . . . . ? C11 P1 C17 C22 47.12(15) . . . . ? C8 P1 C17 C22 -58.37(14) . . . . ? Fe1 P1 C17 C22 -179.77(11) . . . . ? C22 C17 C18 C19 0.5(2) . . . . ? P1 C17 C18 C19 -175.23(13) . . . . ? C17 C18 C19 C20 0.7(3) . . . . ? C18 C19 C20 C21 -1.4(3) . . . . ? C19 C20 C21 C22 0.9(3) . . . . ? C20 C21 C22 C17 0.3(3) . . . . ? C18 C17 C22 C21 -1.0(3) . . . . ? P1 C17 C22 C21 174.88(14) . . . . ? C29 P2 C23 C24 24.13(15) . . . . ? C10 P2 C23 C24 127.49(14) . . . . ? Fe1 P2 C23 C24 -111.58(13) . . . . ? C29 P2 C23 C28 -157.72(13) . . . . ? C10 P2 C23 C28 -54.36(14) . . . . ? Fe1 P2 C23 C28 66.58(14) . . . . ? C28 C23 C24 C25 0.9(2) . . . . ? P2 C23 C24 C25 179.08(13) . . . . ? C23 C24 C25 C26 0.5(3) . . . . ? C24 C25 C26 C27 -1.2(3) . . . . ? C25 C26 C27 C28 0.5(3) . . . . ? C26 C27 C28 C23 1.0(3) . . . . ? C24 C23 C28 C27 -1.6(3) . . . . ? P2 C23 C28 C27 -179.87(14) . . . . ? C10 P2 C29 C34 127.13(14) . . . . ? C23 P2 C29 C34 -129.06(13) . . . . ? Fe1 P2 C29 C34 1.46(16) . . . . ? C10 P2 C29 C30 -51.15(15) . . . . ? C23 P2 C29 C30 52.67(15) . . . . ? Fe1 P2 C29 C30 -176.81(11) . . . . ? C34 C29 C30 C31 0.0(2) . . . . ? P2 C29 C30 C31 178.34(13) . . . . ? C29 C30 C31 C32 1.0(3) . . . . ? C30 C31 C32 C33 -0.5(3) . . . . ? C31 C32 C33 C34 -1.1(3) . . . . ? C32 C33 C34 C29 2.2(3) . . . . ? C30 C29 C34 C33 -1.6(2) . . . . ? P2 C29 C34 C33 -179.92(13) . . . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.454 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.061 #===END data_str0484 _database_code_depnum_ccdc_archive 'CCDC 639869' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H22.50 Fe O2 P1.50 S' _chemical_formula_weight 477.28 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' 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 orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 23.707(2) _cell_length_b 16.7698(14) _cell_length_c 11.2147(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4458.5(7) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7749 _exptl_absorpt_correction_T_max 0.9823 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36380 _diffrn_reflns_av_R_equivalents 0.0904 _diffrn_reflns_av_sigmaI/netI 0.0937 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.26 _reflns_number_total 10394 _reflns_number_gt 7859 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.002(11) _refine_ls_number_reflns 10394 _refine_ls_number_parameters 532 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _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 0.281217(18) 0.08125(3) 0.31540(4) 0.02306(11) Uani 1 1 d . . . Fe2 Fe 0.355138(16) 0.10869(2) 0.47891(4) 0.01598(10) Uani 1 1 d . . . P1 P 0.38141(3) 0.11483(5) 0.66824(7) 0.01780(18) Uani 1 1 d . . . P2 P 0.41926(3) 0.19988(5) 0.43028(7) 0.01731(17) Uani 1 1 d . . . P3 P 0.58429(4) 0.27422(6) 0.68327(8) 0.0291(2) Uani 1 1 d . . . S1 S 0.28823(3) 0.01392(4) 0.48910(7) 0.02065(17) Uani 1 1 d . . . S2 S 0.28271(3) 0.19135(5) 0.43279(7) 0.02146(18) Uani 1 1 d . . . O1 O 0.15957(11) 0.05940(17) 0.2831(3) 0.0556(8) Uani 1 1 d . . . O2 O 0.33069(14) -0.05674(18) 0.1950(2) 0.0629(9) Uani 1 1 d . . . O3 O 0.31229(11) 0.17535(16) 0.1060(2) 0.0434(7) Uani 1 1 d . . . O4 O 0.43173(9) -0.01974(13) 0.4162(2) 0.0287(5) Uani 1 1 d . . . C1 C 0.20707(15) 0.0684(2) 0.2924(3) 0.0333(9) Uani 1 1 d . . . C2 C 0.31132(17) -0.0033(2) 0.2433(3) 0.0379(10) Uani 1 1 d . . . C3 C 0.30033(14) 0.1402(2) 0.1898(3) 0.0287(8) Uani 1 1 d . . . C4 C 0.40198(13) 0.03287(19) 0.4427(3) 0.0199(7) Uani 1 1 d . . . C5 C 0.22986(13) 0.03865(19) 0.5886(3) 0.0252(8) Uani 1 1 d . . . H5A H 0.1942 0.0256 0.5472 0.030 Uiso 1 1 calc R . . H5B H 0.2324 0.0037 0.6595 0.030 Uiso 1 1 calc R . . C6 C 0.22637(14) 0.12389(19) 0.6312(3) 0.0261(8) Uani 1 1 d . . . H6A H 0.2602 0.1356 0.6797 0.031 Uiso 1 1 calc R . . H6B H 0.1930 0.1292 0.6838 0.031 Uiso 1 1 calc R . . C7 C 0.22210(12) 0.1857(2) 0.5331(3) 0.0288(8) Uani 1 1 d . . . H7A H 0.2167 0.2387 0.5704 0.035 Uiso 1 1 calc R . . H7B H 0.1881 0.1742 0.4850 0.035 Uiso 1 1 calc R . . C8 C 0.45760(12) 0.09610(18) 0.6829(3) 0.0210(7) Uani 1 1 d . . . H8A H 0.4667 0.0947 0.7691 0.025 Uiso 1 1 calc R . . H8B H 0.4653 0.0422 0.6507 0.025 Uiso 1 1 calc R . . C9 C 0.49945(12) 0.15550(18) 0.6219(3) 0.0194(7) Uani 1 1 d . . . C10 C 0.46990(12) 0.22254(18) 0.5506(3) 0.0196(7) Uani 1 1 d . . . H10A H 0.5000 0.2559 0.5151 0.023 Uiso 1 1 calc R . . H10B H 0.4499 0.2565 0.6092 0.023 Uiso 1 1 calc R . . C11 C 0.53229(13) 0.1974(2) 0.7247(3) 0.0256(8) Uani 1 1 d . . . H11A H 0.5521 0.1558 0.7711 0.031 Uiso 1 1 calc R . . H11B H 0.5043 0.2224 0.7786 0.031 Uiso 1 1 calc R . . C12 C 0.54014(14) 0.10909(19) 0.5422(3) 0.0287(8) Uani 1 1 d . . . H12A H 0.5582 0.0667 0.5888 0.043 Uiso 1 1 calc R . . H12B H 0.5691 0.1453 0.5112 0.043 Uiso 1 1 calc R . . H12C H 0.5193 0.0855 0.4756 0.043 Uiso 1 1 calc R . . C13 C 0.35227(13) 0.0369(2) 0.7640(3) 0.0225(7) Uani 1 1 d . . . C14 C 0.36373(14) -0.0438(2) 0.7358(3) 0.0292(8) Uani 1 1 d . . . H14A H 0.3893 -0.0563 0.6733 0.035 Uiso 1 1 calc R . . C15 C 0.33782(16) -0.1042(2) 0.7988(4) 0.0390(10) Uani 1 1 d . . . H15A H 0.3459 -0.1581 0.7793 0.047 Uiso 1 1 calc R . . C16 C 0.30063(16) -0.0878(2) 0.8890(3) 0.0425(10) Uani 1 1 d . . . H16A H 0.2826 -0.1300 0.9308 0.051 Uiso 1 1 calc R . . C17 C 0.28970(14) -0.0094(2) 0.9185(3) 0.0338(9) Uani 1 1 d . . . H17A H 0.2643 0.0024 0.9815 0.041 Uiso 1 1 calc R . . C18 C 0.31546(14) 0.0520(2) 0.8569(3) 0.0282(8) Uani 1 1 d . . . H18A H 0.3077 0.1056 0.8788 0.034 Uiso 1 1 calc R . . C19 C 0.37004(13) 0.2054(2) 0.7585(3) 0.0238(8) Uani 1 1 d . . . C20 C 0.33704(14) 0.2675(2) 0.7139(3) 0.0295(8) Uani 1 1 d . . . H20A H 0.3203 0.2630 0.6372 0.035 Uiso 1 1 calc R . . C21 C 0.32856(16) 0.3357(2) 0.7810(4) 0.0437(10) Uani 1 1 d . . . H21A H 0.3054 0.3772 0.7508 0.052 Uiso 1 1 calc R . . C22 C 0.35340(17) 0.3438(2) 0.8908(4) 0.0453(11) Uani 1 1 d . . . H22A H 0.3478 0.3912 0.9356 0.054 Uiso 1 1 calc R . . C23 C 0.38635(16) 0.2834(2) 0.9367(3) 0.0382(10) Uani 1 1 d . . . H23A H 0.4034 0.2889 1.0129 0.046 Uiso 1 1 calc R . . C24 C 0.39440(14) 0.2147(2) 0.8702(3) 0.0288(8) Uani 1 1 d . . . H24A H 0.4171 0.1731 0.9018 0.035 Uiso 1 1 calc R . . C25 C 0.39503(12) 0.30134(18) 0.3959(3) 0.0186(7) Uani 1 1 d . . . C26 C 0.39593(15) 0.36404(19) 0.4734(3) 0.0333(8) Uani 1 1 d . . . H26A H 0.4108 0.3565 0.5512 0.040 Uiso 1 1 calc R . . C27 C 0.37561(16) 0.4384(2) 0.4410(3) 0.0414(10) Uani 1 1 d . . . H27A H 0.3769 0.4813 0.4963 0.050 Uiso 1 1 calc R . . C28 C 0.35366(14) 0.4503(2) 0.3294(3) 0.0358(9) Uani 1 1 d . . . H28A H 0.3397 0.5014 0.3075 0.043 Uiso 1 1 calc R . . C29 C 0.35192(15) 0.3889(2) 0.2499(3) 0.0339(9) Uani 1 1 d . . . H29A H 0.3365 0.3968 0.1726 0.041 Uiso 1 1 calc R . . C30 C 0.37266(14) 0.3149(2) 0.2823(3) 0.0275(8) Uani 1 1 d . . . H30A H 0.3717 0.2725 0.2263 0.033 Uiso 1 1 calc R . . C31 C 0.46376(12) 0.18479(18) 0.2978(3) 0.0207(7) Uani 1 1 d . . . C32 C 0.45241(14) 0.12577(19) 0.2148(3) 0.0241(8) Uani 1 1 d . . . H32A H 0.4226 0.0892 0.2297 0.029 Uiso 1 1 calc R . . C33 C 0.48332(15) 0.1186(2) 0.1106(3) 0.0311(9) Uani 1 1 d . . . H33A H 0.4747 0.0778 0.0548 0.037 Uiso 1 1 calc R . . C34 C 0.52696(16) 0.1715(2) 0.0884(3) 0.0377(10) Uani 1 1 d . . . H34A H 0.5489 0.1667 0.0179 0.045 Uiso 1 1 calc R . . C35 C 0.53830(15) 0.2316(2) 0.1703(4) 0.0408(10) Uani 1 1 d . . . H35A H 0.5677 0.2687 0.1550 0.049 Uiso 1 1 calc R . . C36 C 0.50743(14) 0.2375(2) 0.2726(3) 0.0341(9) Uani 1 1 d . . . H36A H 0.5160 0.2786 0.3280 0.041 Uiso 1 1 calc R . . C37 C 0.54349(14) 0.3677(2) 0.6787(3) 0.0296(8) Uani 1 1 d . . . C38 C 0.49870(15) 0.3876(2) 0.7502(3) 0.0386(9) Uani 1 1 d . . . H38A H 0.4860 0.3504 0.8082 0.046 Uiso 1 1 calc R . . C39 C 0.47152(18) 0.4601(3) 0.7404(4) 0.0490(11) Uani 1 1 d . . . H39A H 0.4404 0.4723 0.7907 0.059 Uiso 1 1 calc R . . C40 C 0.48966(19) 0.5141(2) 0.6580(4) 0.0510(12) Uani 1 1 d . . . H40A H 0.4714 0.5643 0.6519 0.061 Uiso 1 1 calc R . . C41 C 0.53362(18) 0.4969(3) 0.5844(4) 0.0518(12) Uani 1 1 d . . . H41A H 0.5460 0.5350 0.5274 0.062 Uiso 1 1 calc R . . C42 C 0.56048(15) 0.4232(2) 0.5931(4) 0.0410(10) Uani 1 1 d . . . H42A H 0.5906 0.4107 0.5404 0.049 Uiso 1 1 calc R . . C43 C 0.61931(13) 0.2815(2) 0.8293(3) 0.0275(8) Uani 1 1 d . . . C44 C 0.65482(16) 0.2191(3) 0.8606(4) 0.0558(13) Uani 1 1 d . . . H44A H 0.6591 0.1752 0.8079 0.067 Uiso 1 1 calc R . . C45 C 0.68422(16) 0.2198(3) 0.9675(4) 0.0595(13) Uani 1 1 d . . . H45A H 0.7076 0.1759 0.9880 0.071 Uiso 1 1 calc R . . C46 C 0.67984(15) 0.2830(2) 1.0435(4) 0.0419(10) Uani 1 1 d . . . H46A H 0.6999 0.2834 1.1168 0.050 Uiso 1 1 calc R . . C47 C 0.64580(16) 0.3464(2) 1.0122(3) 0.0382(10) Uani 1 1 d . . . H47A H 0.6430 0.3913 1.0634 0.046 Uiso 1 1 calc R . . C48 C 0.61582(15) 0.3448(2) 0.9071(3) 0.0319(9) Uani 1 1 d . . . H48A H 0.5921 0.3885 0.8878 0.038 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 0.0196(2) 0.0276(3) 0.0219(2) 0.0036(2) -0.0030(2) -0.0013(2) Fe2 0.0132(2) 0.0158(2) 0.0189(2) 0.0019(2) 0.00032(19) 0.00087(18) P1 0.0171(4) 0.0175(5) 0.0189(4) 0.0011(4) 0.0005(3) -0.0014(3) P2 0.0143(4) 0.0174(4) 0.0202(4) 0.0018(4) 0.0006(3) 0.0002(3) P3 0.0225(5) 0.0314(6) 0.0333(5) -0.0035(4) 0.0021(4) -0.0052(4) S1 0.0186(4) 0.0212(4) 0.0221(4) 0.0037(4) -0.0005(4) -0.0032(3) S2 0.0154(4) 0.0217(5) 0.0273(4) 0.0054(4) 0.0025(4) 0.0025(3) O1 0.0278(15) 0.080(2) 0.059(2) 0.0191(17) -0.0141(14) -0.0172(15) O2 0.107(3) 0.048(2) 0.0337(16) 0.0003(15) 0.0035(17) 0.0308(19) O3 0.0443(16) 0.0575(18) 0.0284(15) 0.0140(13) 0.0026(12) -0.0112(14) O4 0.0300(13) 0.0233(13) 0.0327(13) -0.0018(11) 0.0033(11) 0.0113(11) C1 0.036(2) 0.039(2) 0.0249(19) 0.0097(17) -0.0049(16) -0.0072(18) C2 0.052(3) 0.040(3) 0.0217(19) 0.0044(18) -0.0064(18) 0.006(2) C3 0.0228(18) 0.035(2) 0.0280(19) -0.0019(17) -0.0075(15) 0.0033(16) C4 0.0216(16) 0.0212(19) 0.0170(15) 0.0069(14) -0.0023(13) -0.0055(14) C5 0.0132(17) 0.031(2) 0.0318(19) 0.0088(16) 0.0018(14) -0.0080(15) C6 0.0159(17) 0.031(2) 0.0308(19) 0.0054(16) 0.0079(14) 0.0040(15) C7 0.0155(17) 0.032(2) 0.039(2) 0.0046(16) 0.0077(15) 0.0028(15) C8 0.0198(16) 0.0189(18) 0.0243(17) 0.0034(14) -0.0027(14) 0.0031(13) C9 0.0124(16) 0.0172(17) 0.0288(17) 0.0000(15) -0.0008(14) 0.0002(14) C10 0.0165(17) 0.0165(18) 0.0257(17) 0.0035(14) 0.0029(14) -0.0017(14) C11 0.0211(18) 0.027(2) 0.0287(19) 0.0012(15) -0.0048(14) 0.0016(15) C12 0.0242(18) 0.026(2) 0.036(2) 0.0053(16) 0.0001(16) 0.0018(16) C13 0.0217(17) 0.026(2) 0.0203(16) 0.0035(14) -0.0043(14) -0.0036(15) C14 0.030(2) 0.028(2) 0.0291(19) 0.0037(16) 0.0003(15) 0.0010(16) C15 0.048(2) 0.022(2) 0.047(2) 0.0119(19) -0.006(2) -0.0047(17) C16 0.047(2) 0.043(3) 0.037(2) 0.019(2) -0.003(2) -0.018(2) C17 0.035(2) 0.043(2) 0.0232(18) 0.0043(17) 0.0032(16) -0.0108(18) C18 0.034(2) 0.030(2) 0.0202(16) 0.0021(15) -0.0018(15) -0.0060(17) C19 0.0171(16) 0.024(2) 0.0303(18) -0.0001(15) 0.0056(14) -0.0057(15) C20 0.0274(19) 0.028(2) 0.034(2) -0.0102(17) 0.0059(16) -0.0001(16) C21 0.042(2) 0.030(2) 0.059(3) -0.011(2) 0.009(2) 0.0038(19) C22 0.055(3) 0.030(2) 0.052(3) -0.019(2) 0.021(2) -0.012(2) C23 0.049(2) 0.037(2) 0.0287(19) -0.0125(18) 0.0159(18) -0.0180(19) C24 0.031(2) 0.032(2) 0.0228(17) 0.0002(16) 0.0059(15) -0.0089(16) C25 0.0145(15) 0.0161(17) 0.0252(17) 0.0016(14) 0.0035(13) -0.0015(13) C26 0.044(2) 0.0229(19) 0.033(2) 0.0006(18) -0.0143(19) 0.0039(16) C27 0.059(3) 0.017(2) 0.048(2) -0.0067(18) -0.022(2) 0.0043(18) C28 0.038(2) 0.025(2) 0.044(2) 0.0042(18) -0.013(2) 0.0080(16) C29 0.043(2) 0.030(2) 0.0285(19) 0.0079(16) -0.0077(17) 0.0081(18) C30 0.037(2) 0.023(2) 0.0223(17) 0.0017(15) -0.0008(15) 0.0051(16) C31 0.0166(16) 0.0217(18) 0.0238(17) 0.0056(15) 0.0035(13) 0.0030(13) C32 0.0253(18) 0.023(2) 0.0242(18) 0.0047(15) 0.0026(15) 0.0077(15) C33 0.042(2) 0.030(2) 0.0211(18) 0.0002(16) 0.0066(17) 0.0117(18) C34 0.036(2) 0.047(3) 0.030(2) 0.0066(19) 0.0160(17) 0.017(2) C35 0.032(2) 0.043(2) 0.047(2) 0.011(2) 0.0168(19) -0.0049(19) C36 0.030(2) 0.034(2) 0.039(2) -0.0046(17) 0.0122(17) -0.0039(17) C37 0.0293(19) 0.026(2) 0.033(2) -0.0048(16) -0.0062(17) -0.0096(16) C38 0.039(2) 0.034(2) 0.043(2) 0.0017(18) 0.0038(19) -0.0063(19) C39 0.047(3) 0.043(3) 0.057(3) -0.009(2) -0.006(2) 0.009(2) C40 0.062(3) 0.028(2) 0.063(3) -0.004(2) -0.025(3) 0.007(2) C41 0.058(3) 0.043(3) 0.054(3) 0.022(2) -0.013(2) -0.012(2) C42 0.028(2) 0.050(3) 0.044(2) 0.001(2) -0.0061(18) -0.008(2) C43 0.0171(17) 0.029(2) 0.036(2) -0.0023(17) -0.0003(15) -0.0052(15) C44 0.039(2) 0.052(3) 0.077(3) -0.030(2) -0.026(2) 0.018(2) C45 0.036(2) 0.057(3) 0.086(4) -0.006(3) -0.029(2) 0.021(2) C46 0.032(2) 0.045(3) 0.048(2) -0.004(2) -0.0136(19) -0.010(2) C47 0.053(2) 0.029(2) 0.032(2) 0.0004(17) -0.0087(19) -0.0064(19) C48 0.038(2) 0.025(2) 0.033(2) 0.0076(17) -0.0032(17) -0.0034(17) _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 C3 1.779(4) . ? Fe1 C2 1.782(4) . ? Fe1 C1 1.790(4) . ? Fe1 S1 2.2578(9) . ? Fe1 S2 2.2679(9) . ? Fe1 Fe2 2.5778(6) . ? Fe2 C4 1.736(3) . ? Fe2 P1 2.2152(9) . ? Fe2 P2 2.2241(9) . ? Fe2 S1 2.2483(8) . ? Fe2 S2 2.2665(9) . ? P1 C13 1.828(3) . ? P1 C8 1.841(3) . ? P1 C19 1.845(3) . ? P2 C25 1.837(3) . ? P2 C31 1.839(3) . ? P2 C10 1.846(3) . ? P3 C43 1.840(4) . ? P3 C11 1.842(3) . ? P3 C37 1.842(4) . ? S1 C5 1.826(3) . ? S2 C7 1.827(3) . ? O1 C1 1.141(4) . ? O2 C2 1.143(4) . ? O3 C3 1.145(4) . ? O4 C4 1.168(3) . ? C5 C6 1.509(4) . ? C6 C7 1.515(4) . ? C8 C9 1.564(4) . ? C9 C12 1.528(4) . ? C9 C10 1.547(4) . ? C9 C11 1.559(4) . ? C13 C18 1.382(4) . ? C13 C14 1.415(5) . ? C14 C15 1.380(5) . ? C15 C16 1.370(5) . ? C16 C17 1.380(5) . ? C17 C18 1.382(4) . ? C19 C24 1.389(4) . ? C19 C20 1.395(5) . ? C20 C21 1.383(5) . ? C21 C22 1.372(5) . ? C22 C23 1.378(5) . ? C23 C24 1.385(5) . ? C25 C26 1.364(4) . ? C25 C30 1.399(4) . ? C26 C27 1.386(4) . ? C27 C28 1.370(5) . ? C28 C29 1.364(5) . ? C29 C30 1.383(4) . ? C31 C32 1.385(4) . ? C31 C36 1.390(4) . ? C32 C33 1.384(4) . ? C33 C34 1.385(5) . ? C34 C35 1.389(5) . ? C35 C36 1.365(5) . ? C37 C38 1.372(5) . ? C37 C42 1.397(5) . ? C38 C39 1.380(5) . ? C39 C40 1.363(6) . ? C40 C41 1.360(6) . ? C41 C42 1.393(5) . ? C43 C48 1.376(5) . ? C43 C44 1.388(5) . ? C44 C45 1.386(6) . ? C45 C46 1.364(5) . ? C46 C47 1.379(5) . ? C47 C48 1.376(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Fe1 C2 88.93(16) . . ? C3 Fe1 C1 101.71(15) . . ? C2 Fe1 C1 103.43(17) . . ? C3 Fe1 S1 160.39(11) . . ? C2 Fe1 S1 87.92(11) . . ? C1 Fe1 S1 97.85(11) . . ? C3 Fe1 S2 90.18(11) . . ? C2 Fe1 S2 154.85(13) . . ? C1 Fe1 S2 101.37(12) . . ? S1 Fe1 S2 84.56(3) . . ? C3 Fe1 Fe2 106.90(10) . . ? C2 Fe1 Fe2 101.10(12) . . ? C1 Fe1 Fe2 142.35(11) . . ? S1 Fe1 Fe2 54.93(2) . . ? S2 Fe1 Fe2 55.33(2) . . ? C4 Fe2 P1 94.51(10) . . ? C4 Fe2 P2 90.51(10) . . ? P1 Fe2 P2 90.62(3) . . ? C4 Fe2 S1 86.88(10) . . ? P1 Fe2 S1 100.52(3) . . ? P2 Fe2 S1 168.72(4) . . ? C4 Fe2 S2 151.51(10) . . ? P1 Fe2 S2 113.78(3) . . ? P2 Fe2 S2 92.37(3) . . ? S1 Fe2 S2 84.81(3) . . ? C4 Fe2 Fe1 97.91(10) . . ? P1 Fe2 Fe1 151.80(3) . . ? P2 Fe2 Fe1 114.39(3) . . ? S1 Fe2 Fe1 55.28(3) . . ? S2 Fe2 Fe1 55.38(3) . . ? C13 P1 C8 101.32(14) . . ? C13 P1 C19 102.19(15) . . ? C8 P1 C19 103.58(14) . . ? C13 P1 Fe2 115.08(10) . . ? C8 P1 Fe2 110.71(11) . . ? C19 P1 Fe2 121.54(11) . . ? C25 P2 C31 97.90(13) . . ? C25 P2 C10 99.56(14) . . ? C31 P2 C10 104.22(13) . . ? C25 P2 Fe2 118.33(10) . . ? C31 P2 Fe2 119.70(10) . . ? C10 P2 Fe2 114.01(10) . . ? C43 P3 C11 97.13(15) . . ? C43 P3 C37 101.82(15) . . ? C11 P3 C37 104.49(15) . . ? C5 S1 Fe2 113.91(11) . . ? C5 S1 Fe1 110.97(11) . . ? Fe2 S1 Fe1 69.79(3) . . ? C7 S2 Fe2 115.07(11) . . ? C7 S2 Fe1 107.64(12) . . ? Fe2 S2 Fe1 69.29(3) . . ? O1 C1 Fe1 176.9(3) . . ? O2 C2 Fe1 178.6(3) . . ? O3 C3 Fe1 177.1(3) . . ? O4 C4 Fe2 177.3(3) . . ? C6 C5 S1 116.7(2) . . ? C5 C6 C7 115.0(3) . . ? C6 C7 S2 115.5(2) . . ? C9 C8 P1 118.3(2) . . ? C12 C9 C10 110.7(3) . . ? C12 C9 C11 110.3(3) . . ? C10 C9 C11 106.3(2) . . ? C12 C9 C8 109.4(3) . . ? C10 C9 C8 113.7(2) . . ? C11 C9 C8 106.3(2) . . ? C9 C10 P2 121.5(2) . . ? C9 C11 P3 117.6(2) . . ? C18 C13 C14 117.7(3) . . ? C18 C13 P1 123.4(3) . . ? C14 C13 P1 118.6(2) . . ? C15 C14 C13 120.1(3) . . ? C16 C15 C14 121.2(3) . . ? C15 C16 C17 119.2(3) . . ? C16 C17 C18 120.5(3) . . ? C17 C18 C13 121.2(3) . . ? C24 C19 C20 118.2(3) . . ? C24 C19 P1 121.8(3) . . ? C20 C19 P1 120.0(3) . . ? C21 C20 C19 120.2(3) . . ? C22 C21 C20 120.5(4) . . ? C21 C22 C23 120.4(4) . . ? C22 C23 C24 119.2(4) . . ? C23 C24 C19 121.4(4) . . ? C26 C25 C30 117.4(3) . . ? C26 C25 P2 125.1(2) . . ? C30 C25 P2 117.4(2) . . ? C25 C26 C27 121.5(3) . . ? C28 C27 C26 120.2(3) . . ? C29 C28 C27 119.9(3) . . ? C28 C29 C30 119.7(3) . . ? C29 C30 C25 121.3(3) . . ? C32 C31 C36 117.5(3) . . ? C32 C31 P2 122.0(2) . . ? C36 C31 P2 120.2(2) . . ? C33 C32 C31 121.7(3) . . ? C32 C33 C34 119.5(3) . . ? C33 C34 C35 119.3(3) . . ? C36 C35 C34 120.3(3) . . ? C35 C36 C31 121.6(3) . . ? C38 C37 C42 117.5(3) . . ? C38 C37 P3 126.7(3) . . ? C42 C37 P3 115.8(3) . . ? C37 C38 C39 122.0(4) . . ? C40 C39 C38 119.4(4) . . ? C41 C40 C39 120.8(4) . . ? C40 C41 C42 119.7(4) . . ? C41 C42 C37 120.5(4) . . ? C48 C43 C44 117.2(3) . . ? C48 C43 P3 126.1(3) . . ? C44 C43 P3 116.7(3) . . ? C45 C44 C43 121.2(4) . . ? C46 C45 C44 120.5(4) . . ? C45 C46 C47 119.0(4) . . ? C48 C47 C46 120.3(4) . . ? C47 C48 C43 121.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Fe1 Fe2 C4 -91.13(15) . . . . ? C2 Fe1 Fe2 C4 1.15(16) . . . . ? C1 Fe1 Fe2 C4 131.1(2) . . . . ? S1 Fe1 Fe2 C4 80.61(10) . . . . ? S2 Fe1 Fe2 C4 -169.23(10) . . . . ? C3 Fe1 Fe2 P1 153.59(13) . . . . ? C2 Fe1 Fe2 P1 -114.13(14) . . . . ? C1 Fe1 Fe2 P1 15.8(2) . . . . ? S1 Fe1 Fe2 P1 -34.67(7) . . . . ? S2 Fe1 Fe2 P1 75.49(7) . . . . ? C3 Fe1 Fe2 P2 3.05(12) . . . . ? C2 Fe1 Fe2 P2 95.32(13) . . . . ? C1 Fe1 Fe2 P2 -134.77(19) . . . . ? S1 Fe1 Fe2 P2 174.79(4) . . . . ? S2 Fe1 Fe2 P2 -75.05(4) . . . . ? C3 Fe1 Fe2 S1 -171.74(12) . . . . ? C2 Fe1 Fe2 S1 -79.46(13) . . . . ? C1 Fe1 Fe2 S1 50.44(19) . . . . ? S2 Fe1 Fe2 S1 110.16(4) . . . . ? C3 Fe1 Fe2 S2 78.10(12) . . . . ? C2 Fe1 Fe2 S2 170.38(13) . . . . ? C1 Fe1 Fe2 S2 -59.72(19) . . . . ? S1 Fe1 Fe2 S2 -110.16(4) . . . . ? C4 Fe2 P1 C13 -78.65(15) . . . . ? P2 Fe2 P1 C13 -169.21(12) . . . . ? S1 Fe2 P1 C13 9.01(12) . . . . ? S2 Fe2 P1 C13 97.93(12) . . . . ? Fe1 Fe2 P1 C13 37.40(14) . . . . ? C4 Fe2 P1 C8 35.47(14) . . . . ? P2 Fe2 P1 C8 -55.09(11) . . . . ? S1 Fe2 P1 C8 123.12(11) . . . . ? S2 Fe2 P1 C8 -147.95(11) . . . . ? Fe1 Fe2 P1 C8 151.52(11) . . . . ? C4 Fe2 P1 C19 157.24(15) . . . . ? P2 Fe2 P1 C19 66.68(12) . . . . ? S1 Fe2 P1 C19 -115.10(12) . . . . ? S2 Fe2 P1 C19 -26.18(12) . . . . ? Fe1 Fe2 P1 C19 -86.71(13) . . . . ? C4 Fe2 P2 C25 159.61(15) . . . . ? P1 Fe2 P2 C25 -105.88(11) . . . . ? S1 Fe2 P2 C25 83.1(2) . . . . ? S2 Fe2 P2 C25 7.96(12) . . . . ? Fe1 Fe2 P2 C25 60.69(12) . . . . ? C4 Fe2 P2 C31 40.45(15) . . . . ? P1 Fe2 P2 C31 134.97(11) . . . . ? S1 Fe2 P2 C31 -36.0(2) . . . . ? S2 Fe2 P2 C31 -111.20(11) . . . . ? Fe1 Fe2 P2 C31 -58.47(11) . . . . ? C4 Fe2 P2 C10 -83.86(14) . . . . ? P1 Fe2 P2 C10 10.66(11) . . . . ? S1 Fe2 P2 C10 -160.33(19) . . . . ? S2 Fe2 P2 C10 124.49(11) . . . . ? Fe1 Fe2 P2 C10 177.22(11) . . . . ? C4 Fe2 S1 C5 153.43(15) . . . . ? P1 Fe2 S1 C5 59.42(12) . . . . ? P2 Fe2 S1 C5 -129.7(2) . . . . ? S2 Fe2 S1 C5 -53.85(12) . . . . ? Fe1 Fe2 S1 C5 -104.71(12) . . . . ? C4 Fe2 S1 Fe1 -101.86(10) . . . . ? P1 Fe2 S1 Fe1 164.13(3) . . . . ? P2 Fe2 S1 Fe1 -25.03(18) . . . . ? S2 Fe2 S1 Fe1 50.87(3) . . . . ? C3 Fe1 S1 C5 132.9(4) . . . . ? C2 Fe1 S1 C5 -146.14(17) . . . . ? C1 Fe1 S1 C5 -42.87(17) . . . . ? S2 Fe1 S1 C5 57.89(12) . . . . ? Fe2 Fe1 S1 C5 108.75(12) . . . . ? C3 Fe1 S1 Fe2 24.2(3) . . . . ? C2 Fe1 S1 Fe2 105.12(13) . . . . ? C1 Fe1 S1 Fe2 -151.61(12) . . . . ? S2 Fe1 S1 Fe2 -50.85(3) . . . . ? C4 Fe2 S2 C7 123.2(2) . . . . ? P1 Fe2 S2 C7 -49.59(14) . . . . ? P2 Fe2 S2 C7 -141.31(13) . . . . ? S1 Fe2 S2 C7 49.63(13) . . . . ? Fe1 Fe2 S2 C7 100.42(13) . . . . ? C4 Fe2 S2 Fe1 22.8(2) . . . . ? P1 Fe2 S2 Fe1 -150.00(3) . . . . ? P2 Fe2 S2 Fe1 118.27(3) . . . . ? S1 Fe2 S2 Fe1 -50.78(3) . . . . ? C3 Fe1 S2 C7 138.64(15) . . . . ? C2 Fe1 S2 C7 -133.5(3) . . . . ? C1 Fe1 S2 C7 36.65(16) . . . . ? S1 Fe1 S2 C7 -60.28(11) . . . . ? Fe2 Fe1 S2 C7 -110.80(11) . . . . ? C3 Fe1 S2 Fe2 -110.56(11) . . . . ? C2 Fe1 S2 Fe2 -22.7(3) . . . . ? C1 Fe1 S2 Fe2 147.45(11) . . . . ? S1 Fe1 S2 Fe2 50.52(3) . . . . ? C3 Fe1 C1 O1 -160(6) . . . . ? C2 Fe1 C1 O1 108(6) . . . . ? S1 Fe1 C1 O1 19(6) . . . . ? S2 Fe1 C1 O1 -67(6) . . . . ? Fe2 Fe1 C1 O1 -21(7) . . . . ? C3 Fe1 C2 O2 -13(16) . . . . ? C1 Fe1 C2 O2 89(16) . . . . ? S1 Fe1 C2 O2 -173(100) . . . . ? S2 Fe1 C2 O2 -101(16) . . . . ? Fe2 Fe1 C2 O2 -120(16) . . . . ? C2 Fe1 C3 O3 32(6) . . . . ? C1 Fe1 C3 O3 -71(6) . . . . ? S1 Fe1 C3 O3 113(6) . . . . ? S2 Fe1 C3 O3 -173(100) . . . . ? Fe2 Fe1 C3 O3 133(6) . . . . ? P1 Fe2 C4 O4 130(6) . . . . ? P2 Fe2 C4 O4 -139(6) . . . . ? S1 Fe2 C4 O4 30(6) . . . . ? S2 Fe2 C4 O4 -43(6) . . . . ? Fe1 Fe2 C4 O4 -24(6) . . . . ? Fe2 S1 C5 C6 12.5(3) . . . . ? Fe1 S1 C5 C6 -64.0(3) . . . . ? S1 C5 C6 C7 58.1(4) . . . . ? C5 C6 C7 S2 -63.1(4) . . . . ? Fe2 S2 C7 C6 -2.8(3) . . . . ? Fe1 S2 C7 C6 72.1(3) . . . . ? C13 P1 C8 C9 -174.9(2) . . . . ? C19 P1 C8 C9 -69.3(3) . . . . ? Fe2 P1 C8 C9 62.6(2) . . . . ? P1 C8 C9 C12 -126.7(2) . . . . ? P1 C8 C9 C10 -2.4(4) . . . . ? P1 C8 C9 C11 114.2(3) . . . . ? C12 C9 C10 P2 67.4(3) . . . . ? C11 C9 C10 P2 -172.8(2) . . . . ? C8 C9 C10 P2 -56.2(3) . . . . ? C25 P2 C10 C9 174.2(2) . . . . ? C31 P2 C10 C9 -85.1(3) . . . . ? Fe2 P2 C10 C9 47.2(3) . . . . ? C12 C9 C11 P3 63.2(3) . . . . ? C10 C9 C11 P3 -56.9(3) . . . . ? C8 C9 C11 P3 -178.3(2) . . . . ? C43 P3 C11 C9 -166.8(2) . . . . ? C37 P3 C11 C9 89.0(3) . . . . ? C8 P1 C13 C18 125.5(3) . . . . ? C19 P1 C13 C18 18.8(3) . . . . ? Fe2 P1 C13 C18 -115.0(3) . . . . ? C8 P1 C13 C14 -60.4(3) . . . . ? C19 P1 C13 C14 -167.1(3) . . . . ? Fe2 P1 C13 C14 59.1(3) . . . . ? C18 C13 C14 C15 1.0(5) . . . . ? P1 C13 C14 C15 -173.4(3) . . . . ? C13 C14 C15 C16 0.2(5) . . . . ? C14 C15 C16 C17 -1.1(6) . . . . ? C15 C16 C17 C18 0.7(5) . . . . ? C16 C17 C18 C13 0.6(5) . . . . ? C14 C13 C18 C17 -1.4(5) . . . . ? P1 C13 C18 C17 172.8(3) . . . . ? C13 P1 C19 C24 60.9(3) . . . . ? C8 P1 C19 C24 -44.1(3) . . . . ? Fe2 P1 C19 C24 -169.2(2) . . . . ? C13 P1 C19 C20 -120.3(3) . . . . ? C8 P1 C19 C20 134.7(3) . . . . ? Fe2 P1 C19 C20 9.6(3) . . . . ? C24 C19 C20 C21 -0.9(5) . . . . ? P1 C19 C20 C21 -179.7(3) . . . . ? C19 C20 C21 C22 1.4(5) . . . . ? C20 C21 C22 C23 -1.1(6) . . . . ? C21 C22 C23 C24 0.4(5) . . . . ? C22 C23 C24 C19 0.1(5) . . . . ? C20 C19 C24 C23 0.2(5) . . . . ? P1 C19 C24 C23 179.0(2) . . . . ? C31 P2 C25 C26 -131.1(3) . . . . ? C10 P2 C25 C26 -25.1(3) . . . . ? Fe2 P2 C25 C26 98.9(3) . . . . ? C31 P2 C25 C30 50.5(3) . . . . ? C10 P2 C25 C30 156.5(2) . . . . ? Fe2 P2 C25 C30 -79.5(3) . . . . ? C30 C25 C26 C27 -0.1(5) . . . . ? P2 C25 C26 C27 -178.5(3) . . . . ? C25 C26 C27 C28 0.4(6) . . . . ? C26 C27 C28 C29 -0.1(6) . . . . ? C27 C28 C29 C30 -0.4(6) . . . . ? C28 C29 C30 C25 0.7(5) . . . . ? C26 C25 C30 C29 -0.4(5) . . . . ? P2 C25 C30 C29 178.1(3) . . . . ? C25 P2 C31 C32 -117.5(3) . . . . ? C10 P2 C31 C32 140.5(3) . . . . ? Fe2 P2 C31 C32 11.6(3) . . . . ? C25 P2 C31 C36 56.9(3) . . . . ? C10 P2 C31 C36 -45.1(3) . . . . ? Fe2 P2 C31 C36 -174.0(2) . . . . ? C36 C31 C32 C33 0.4(5) . . . . ? P2 C31 C32 C33 174.8(2) . . . . ? C31 C32 C33 C34 0.2(5) . . . . ? C32 C33 C34 C35 -1.0(5) . . . . ? C33 C34 C35 C36 1.2(6) . . . . ? C34 C35 C36 C31 -0.6(6) . . . . ? C32 C31 C36 C35 -0.2(5) . . . . ? P2 C31 C36 C35 -174.8(3) . . . . ? C43 P3 C37 C38 -66.8(3) . . . . ? C11 P3 C37 C38 33.9(3) . . . . ? C43 P3 C37 C42 113.2(3) . . . . ? C11 P3 C37 C42 -146.1(3) . . . . ? C42 C37 C38 C39 -1.0(5) . . . . ? P3 C37 C38 C39 179.0(3) . . . . ? C37 C38 C39 C40 -0.4(6) . . . . ? C38 C39 C40 C41 0.9(6) . . . . ? C39 C40 C41 C42 0.1(6) . . . . ? C40 C41 C42 C37 -1.6(6) . . . . ? C38 C37 C42 C41 2.0(5) . . . . ? P3 C37 C42 C41 -178.0(3) . . . . ? C11 P3 C43 C48 -109.3(3) . . . . ? C37 P3 C43 C48 -2.8(3) . . . . ? C11 P3 C43 C44 74.3(3) . . . . ? C37 P3 C43 C44 -179.3(3) . . . . ? C48 C43 C44 C45 1.7(6) . . . . ? P3 C43 C44 C45 178.5(3) . . . . ? C43 C44 C45 C46 -1.5(7) . . . . ? C44 C45 C46 C47 -0.2(7) . . . . ? C45 C46 C47 C48 1.4(6) . . . . ? C46 C47 C48 C43 -1.1(5) . . . . ? C44 C43 C48 C47 -0.4(5) . . . . ? P3 C43 C48 C47 -176.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.681 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.077 #===END data_str0459 _database_code_depnum_ccdc_archive 'CCDC 639870' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H31 Fe2 N O4 P2 S2' _chemical_formula_weight 755.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.8036(6) _cell_length_b 17.9672(12) _cell_length_c 18.4965(12) _cell_angle_alpha 90.00 _cell_angle_beta 100.9190(10) _cell_angle_gamma 90.00 _cell_volume 3199.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 423(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 1.178 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8159 _exptl_absorpt_correction_T_max 0.9544 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 423(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27778 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7641 _reflns_number_gt 6556 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+1.2266P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7641 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.65872(3) 0.678835(14) 0.215303(14) 0.01544(7) Uani 1 1 d . . . Fe2 Fe 0.54249(3) 0.614895(15) 0.092700(14) 0.01765(7) Uani 1 1 d . . . P1 P 0.87033(5) 0.63464(3) 0.25595(2) 0.01520(10) Uani 1 1 d . . . P2 P 0.65150(5) 0.60552(3) 0.31093(2) 0.01530(10) Uani 1 1 d . . . S1 S 0.43198(5) 0.67838(3) 0.17030(3) 0.02083(11) Uani 1 1 d . . . S2 S 0.68892(5) 0.71357(3) 0.10416(3) 0.02077(10) Uani 1 1 d . . . N1 N 0.82373(15) 0.58311(8) 0.32540(8) 0.0167(3) Uani 1 1 d . . . O1 O 0.67460(19) 0.83051(8) 0.26881(9) 0.0364(4) Uani 1 1 d . . . O2 O 0.32712(17) 0.62616(9) -0.04110(8) 0.0354(4) Uani 1 1 d . . . O3 O 0.74895(16) 0.53793(10) 0.02516(9) 0.0374(4) Uani 1 1 d . . . O4 O 0.4524(2) 0.46845(9) 0.13421(9) 0.0448(5) Uani 1 1 d . . . C1 C 0.6728(2) 0.76839(11) 0.25248(10) 0.0234(4) Uani 1 1 d . . . C2 C 0.4128(2) 0.62311(11) 0.01039(11) 0.0238(4) Uani 1 1 d . . . C3 C 0.6710(2) 0.56772(11) 0.05337(11) 0.0243(4) Uani 1 1 d . . . C4 C 0.4871(2) 0.52699(12) 0.12230(11) 0.0269(4) Uani 1 1 d . . . C5 C 0.3799(2) 0.77099(12) 0.13309(12) 0.0309(5) Uani 1 1 d . . . H5A H 0.2793 0.7723 0.1203 0.037 Uiso 1 1 calc R . . H5B H 0.4080 0.8072 0.1719 0.037 Uiso 1 1 calc R . . C6 C 0.4371(2) 0.79567(12) 0.06620(12) 0.0312(5) Uani 1 1 d . . . H6A H 0.4041 0.7615 0.0261 0.037 Uiso 1 1 calc R . . H6B H 0.3994 0.8444 0.0513 0.037 Uiso 1 1 calc R . . C7 C 0.5940(2) 0.79988(11) 0.07695(12) 0.0297(5) Uani 1 1 d . . . H7A H 0.6260 0.8373 0.1141 0.036 Uiso 1 1 calc R . . H7B H 0.6182 0.8170 0.0313 0.036 Uiso 1 1 calc R . . C8 C 0.9092(2) 0.56109(11) 0.39669(10) 0.0225(4) Uani 1 1 d . . . H8A H 0.8498 0.5369 0.4260 0.027 Uiso 1 1 calc R . . H8B H 0.9464 0.6057 0.4228 0.027 Uiso 1 1 calc R . . C9 C 1.0264(2) 0.51031(13) 0.39082(11) 0.0301(5) Uani 1 1 d . . . H9A H 1.0067 0.4664 0.3642 0.036 Uiso 1 1 calc R . . C10 C 1.1563(3) 0.52407(17) 0.42118(13) 0.0465(7) Uani 1 1 d . . . H10A H 1.1790 0.5675 0.4481 0.056 Uiso 1 1 calc R . . H10B H 1.2257 0.4903 0.4158 0.056 Uiso 1 1 calc R . . C11 C 0.95009(18) 0.57279(10) 0.19785(10) 0.0175(4) Uani 1 1 d . . . C12 C 1.0222(2) 0.60296(11) 0.14641(11) 0.0256(4) Uani 1 1 d . . . H12A H 1.0319 0.6543 0.1433 0.031 Uiso 1 1 calc R . . C13 C 1.0793(2) 0.55693(13) 0.10000(12) 0.0304(5) Uani 1 1 d . . . H13A H 1.1287 0.5775 0.0666 0.036 Uiso 1 1 calc R . . C14 C 1.0635(2) 0.48107(13) 0.10306(12) 0.0302(5) Uani 1 1 d . . . H14A H 1.1037 0.4503 0.0725 0.036 Uiso 1 1 calc R . . C15 C 0.9880(2) 0.45061(12) 0.15150(12) 0.0288(4) Uani 1 1 d . . . H15A H 0.9753 0.3994 0.1527 0.035 Uiso 1 1 calc R . . C16 C 0.9308(2) 0.49641(11) 0.19860(11) 0.0229(4) Uani 1 1 d . . . H16A H 0.8793 0.4756 0.2308 0.028 Uiso 1 1 calc R . . C17 C 1.01622(19) 0.69144(10) 0.30270(10) 0.0183(4) Uani 1 1 d . . . C18 C 1.1532(2) 0.68114(12) 0.29400(14) 0.0336(5) Uani 1 1 d . . . H18A H 1.1734 0.6451 0.2615 0.040 Uiso 1 1 calc R . . C19 C 1.2597(2) 0.72415(14) 0.33339(15) 0.0404(6) Uani 1 1 d . . . H19A H 1.3504 0.7176 0.3263 0.048 Uiso 1 1 calc R . . C20 C 1.2313(2) 0.77651(12) 0.38289(12) 0.0318(5) Uani 1 1 d . . . H20A H 1.3031 0.8039 0.4107 0.038 Uiso 1 1 calc R . . C21 C 1.0963(2) 0.78825(12) 0.39107(12) 0.0291(5) Uani 1 1 d . . . H21A H 1.0767 0.8244 0.4236 0.035 Uiso 1 1 calc R . . C22 C 0.9895(2) 0.74636(12) 0.35085(11) 0.0271(4) Uani 1 1 d . . . H22A H 0.8984 0.7552 0.3562 0.032 Uiso 1 1 calc R . . C23 C 0.61247(19) 0.64100(10) 0.39814(10) 0.0183(4) Uani 1 1 d . . . C24 C 0.6223(2) 0.71694(11) 0.41415(11) 0.0229(4) Uani 1 1 d . . . H24A H 0.6570 0.7490 0.3825 0.028 Uiso 1 1 calc R . . C25 C 0.5815(2) 0.74529(12) 0.47611(11) 0.0255(4) Uani 1 1 d . . . H25A H 0.5887 0.7961 0.4856 0.031 Uiso 1 1 calc R . . C26 C 0.5302(2) 0.69884(12) 0.52399(11) 0.0276(4) Uani 1 1 d . . . H26A H 0.4995 0.7183 0.5647 0.033 Uiso 1 1 calc R . . C27 C 0.5249(3) 0.62334(13) 0.51090(12) 0.0352(5) Uani 1 1 d . . . H27A H 0.4946 0.5914 0.5442 0.042 Uiso 1 1 calc R . . C28 C 0.5646(3) 0.59464(12) 0.44808(11) 0.0308(5) Uani 1 1 d . . . H28A H 0.5590 0.5436 0.4394 0.037 Uiso 1 1 calc R . . C29 C 0.55785(19) 0.51755(10) 0.30414(10) 0.0182(4) Uani 1 1 d . . . C30 C 0.6243(2) 0.44875(11) 0.30741(10) 0.0219(4) Uani 1 1 d . . . H30A H 0.7207 0.4467 0.3150 0.026 Uiso 1 1 calc R . . C31 C 0.5479(2) 0.38329(11) 0.29942(11) 0.0276(4) Uani 1 1 d . . . H31A H 0.5933 0.3376 0.3023 0.033 Uiso 1 1 calc R . . C32 C 0.4042(2) 0.38577(12) 0.28721(11) 0.0300(5) Uani 1 1 d . . . H32A H 0.3530 0.3419 0.2814 0.036 Uiso 1 1 calc R . . C33 C 0.3368(2) 0.45377(13) 0.28369(12) 0.0309(5) Uani 1 1 d . . . H33A H 0.2403 0.4555 0.2754 0.037 Uiso 1 1 calc R . . C34 C 0.4132(2) 0.51938(12) 0.29250(11) 0.0255(4) Uani 1 1 d . . . H34A H 0.3674 0.5649 0.2906 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01582(14) 0.01547(13) 0.01419(13) -0.00013(9) 0.00073(10) 0.00192(9) Fe2 0.01809(14) 0.01946(14) 0.01535(13) -0.00074(10) 0.00300(10) 0.00024(10) P1 0.0145(2) 0.0157(2) 0.0149(2) -0.00003(17) 0.00173(16) 0.00069(17) P2 0.0153(2) 0.0168(2) 0.0138(2) -0.00076(17) 0.00263(17) 0.00238(17) S1 0.0160(2) 0.0269(2) 0.0192(2) -0.00088(18) 0.00228(17) 0.00450(18) S2 0.0235(2) 0.0204(2) 0.0178(2) 0.00299(18) 0.00219(17) -0.00137(18) N1 0.0151(7) 0.0196(7) 0.0151(7) 0.0026(6) 0.0021(6) 0.0028(6) O1 0.0563(11) 0.0196(7) 0.0333(9) -0.0031(6) 0.0088(8) 0.0025(7) O2 0.0342(9) 0.0388(9) 0.0282(8) -0.0022(7) -0.0069(7) 0.0012(7) O3 0.0292(8) 0.0494(10) 0.0351(9) -0.0131(8) 0.0100(7) 0.0063(7) O4 0.0799(14) 0.0290(9) 0.0281(9) -0.0025(7) 0.0165(9) -0.0158(9) C1 0.0277(10) 0.0229(10) 0.0187(9) 0.0019(7) 0.0023(8) 0.0036(8) C2 0.0253(10) 0.0234(10) 0.0229(10) -0.0017(8) 0.0050(8) -0.0002(8) C3 0.0249(10) 0.0268(10) 0.0201(9) -0.0031(8) 0.0016(8) -0.0015(8) C4 0.0367(12) 0.0278(11) 0.0173(9) -0.0033(8) 0.0077(8) -0.0010(9) C5 0.0282(11) 0.0316(11) 0.0292(11) -0.0022(9) -0.0035(9) 0.0157(9) C6 0.0382(12) 0.0223(10) 0.0279(11) 0.0027(8) -0.0069(9) 0.0080(9) C7 0.0385(12) 0.0198(9) 0.0273(11) 0.0071(8) -0.0023(9) 0.0002(9) C8 0.0209(9) 0.0306(10) 0.0153(9) 0.0041(8) 0.0017(7) 0.0040(8) C9 0.0346(12) 0.0325(11) 0.0219(10) 0.0055(9) 0.0023(9) 0.0144(9) C10 0.0280(12) 0.077(2) 0.0336(13) 0.0062(13) 0.0043(10) 0.0212(13) C11 0.0141(8) 0.0213(9) 0.0167(8) -0.0009(7) 0.0020(7) 0.0017(7) C12 0.0253(10) 0.0246(10) 0.0291(10) 0.0031(8) 0.0104(8) -0.0013(8) C13 0.0289(11) 0.0369(12) 0.0297(11) 0.0036(9) 0.0166(9) 0.0006(9) C14 0.0297(11) 0.0362(12) 0.0274(11) -0.0068(9) 0.0121(9) 0.0044(9) C15 0.0375(12) 0.0227(10) 0.0287(11) -0.0044(8) 0.0124(9) -0.0007(9) C16 0.0268(10) 0.0229(9) 0.0211(9) -0.0013(8) 0.0097(8) -0.0026(8) C17 0.0169(9) 0.0174(8) 0.0187(9) 0.0015(7) -0.0012(7) 0.0001(7) C18 0.0203(10) 0.0307(11) 0.0467(14) -0.0151(10) -0.0018(9) 0.0052(8) C19 0.0160(10) 0.0438(14) 0.0578(16) -0.0159(12) -0.0020(10) 0.0028(9) C20 0.0258(11) 0.0292(11) 0.0355(12) -0.0062(9) -0.0066(9) -0.0031(9) C21 0.0301(11) 0.0297(11) 0.0269(11) -0.0105(9) 0.0034(9) -0.0015(9) C22 0.0198(10) 0.0348(11) 0.0275(10) -0.0079(9) 0.0067(8) -0.0007(8) C23 0.0171(9) 0.0224(9) 0.0152(8) -0.0028(7) 0.0026(7) 0.0018(7) C24 0.0236(10) 0.0241(10) 0.0213(9) -0.0027(8) 0.0049(8) -0.0028(8) C25 0.0257(10) 0.0264(10) 0.0241(10) -0.0078(8) 0.0044(8) -0.0011(8) C26 0.0289(11) 0.0359(11) 0.0190(9) -0.0087(8) 0.0067(8) -0.0020(9) C27 0.0538(15) 0.0347(12) 0.0215(11) -0.0024(9) 0.0184(10) -0.0083(11) C28 0.0505(14) 0.0220(10) 0.0220(10) -0.0018(8) 0.0122(9) -0.0013(9) C29 0.0208(9) 0.0214(9) 0.0130(8) -0.0005(7) 0.0051(7) -0.0008(7) C30 0.0221(10) 0.0225(9) 0.0227(10) -0.0001(8) 0.0085(8) 0.0010(8) C31 0.0383(12) 0.0214(10) 0.0259(10) -0.0017(8) 0.0131(9) -0.0030(9) C32 0.0380(13) 0.0327(11) 0.0213(10) -0.0045(8) 0.0105(9) -0.0158(9) C33 0.0219(10) 0.0436(13) 0.0272(11) -0.0021(9) 0.0047(8) -0.0088(9) C34 0.0211(10) 0.0298(11) 0.0255(10) -0.0008(8) 0.0039(8) 0.0000(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 1.745(2) . ? Fe1 P1 2.2156(5) . ? Fe1 P2 2.2172(5) . ? Fe1 S1 2.2211(5) . ? Fe1 S2 2.2212(5) . ? Fe1 Fe2 2.6042(4) . ? Fe2 C3 1.784(2) . ? Fe2 C4 1.789(2) . ? Fe2 C2 1.795(2) . ? Fe2 S1 2.2637(5) . ? Fe2 S2 2.2657(5) . ? P1 N1 1.7143(15) . ? P1 C11 1.8218(18) . ? P1 C17 1.8348(19) . ? P1 P2 2.5956(7) . ? P2 N1 1.7069(15) . ? P2 C29 1.8202(19) . ? P2 C23 1.8408(18) . ? S1 C5 1.836(2) . ? S2 C7 1.830(2) . ? N1 C8 1.476(2) . ? O1 C1 1.156(2) . ? O2 C2 1.146(2) . ? O3 C3 1.137(2) . ? O4 C4 1.140(3) . ? C5 C6 1.518(3) . ? C6 C7 1.514(3) . ? C8 C9 1.487(3) . ? C9 C10 1.315(3) . ? C11 C16 1.386(3) . ? C11 C12 1.398(3) . ? C12 C13 1.384(3) . ? C13 C14 1.374(3) . ? C14 C15 1.379(3) . ? C15 C16 1.391(3) . ? C17 C22 1.387(3) . ? C17 C18 1.394(3) . ? C18 C19 1.390(3) . ? C19 C20 1.378(3) . ? C20 C21 1.376(3) . ? C21 C22 1.386(3) . ? C23 C28 1.390(3) . ? C23 C24 1.396(3) . ? C24 C25 1.381(3) . ? C25 C26 1.379(3) . ? C26 C27 1.377(3) . ? C27 C28 1.392(3) . ? C29 C30 1.393(3) . ? C29 C34 1.394(3) . ? C30 C31 1.387(3) . ? C31 C32 1.385(3) . ? C32 C33 1.384(3) . ? C33 C34 1.389(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 P1 101.41(7) . . ? C1 Fe1 P2 104.21(6) . . ? P1 Fe1 P2 71.683(18) . . ? C1 Fe1 S1 98.62(7) . . ? P1 Fe1 S1 158.77(2) . . ? P2 Fe1 S1 96.65(2) . . ? C1 Fe1 S2 95.24(7) . . ? P1 Fe1 S2 97.72(2) . . ? P2 Fe1 S2 159.26(2) . . ? S1 Fe1 S2 87.34(2) . . ? C1 Fe1 Fe2 137.63(6) . . ? P1 Fe1 Fe2 111.375(16) . . ? P2 Fe1 Fe2 110.960(17) . . ? S1 Fe1 Fe2 55.269(14) . . ? S2 Fe1 Fe2 55.323(15) . . ? C3 Fe2 C4 89.09(9) . . ? C3 Fe2 C2 97.74(9) . . ? C4 Fe2 C2 97.17(9) . . ? C3 Fe2 S1 163.30(6) . . ? C4 Fe2 S1 92.37(7) . . ? C2 Fe2 S1 98.58(7) . . ? C3 Fe2 S2 85.75(7) . . ? C4 Fe2 S2 152.33(7) . . ? C2 Fe2 S2 110.45(7) . . ? S1 Fe2 S2 85.25(2) . . ? C3 Fe2 Fe1 109.78(6) . . ? C4 Fe2 Fe1 103.36(6) . . ? C2 Fe2 Fe1 145.59(6) . . ? S1 Fe2 Fe1 53.742(15) . . ? S2 Fe2 Fe1 53.728(14) . . ? N1 P1 C11 108.52(8) . . ? N1 P1 C17 103.99(8) . . ? C11 P1 C17 103.53(9) . . ? N1 P1 Fe1 94.73(5) . . ? C11 P1 Fe1 119.83(6) . . ? C17 P1 Fe1 123.83(6) . . ? N1 P1 P2 40.55(5) . . ? C11 P1 P2 125.95(6) . . ? C17 P1 P2 123.77(6) . . ? Fe1 P1 P2 54.188(16) . . ? N1 P2 C29 106.08(8) . . ? N1 P2 C23 107.93(8) . . ? C29 P2 C23 100.10(8) . . ? N1 P2 Fe1 94.89(5) . . ? C29 P2 Fe1 123.56(6) . . ? C23 P2 Fe1 122.45(6) . . ? N1 P2 P1 40.76(5) . . ? C29 P2 P1 126.26(6) . . ? C23 P2 P1 126.72(6) . . ? Fe1 P2 P1 54.129(16) . . ? C5 S1 Fe1 108.95(8) . . ? C5 S1 Fe2 110.58(7) . . ? Fe1 S1 Fe2 70.989(17) . . ? C7 S2 Fe1 110.04(8) . . ? C7 S2 Fe2 110.92(7) . . ? Fe1 S2 Fe2 70.949(17) . . ? C8 N1 P2 125.49(12) . . ? C8 N1 P1 128.87(13) . . ? P2 N1 P1 98.70(8) . . ? O1 C1 Fe1 171.82(18) . . ? O2 C2 Fe2 177.29(19) . . ? O3 C3 Fe2 176.78(18) . . ? O4 C4 Fe2 173.09(18) . . ? C6 C5 S1 116.78(15) . . ? C7 C6 C5 115.50(17) . . ? C6 C7 S2 116.42(15) . . ? N1 C8 C9 114.51(16) . . ? C10 C9 C8 123.6(2) . . ? C16 C11 C12 118.57(17) . . ? C16 C11 P1 121.58(14) . . ? C12 C11 P1 119.60(15) . . ? C13 C12 C11 120.44(19) . . ? C14 C13 C12 120.33(19) . . ? C13 C14 C15 119.93(19) . . ? C14 C15 C16 120.1(2) . . ? C11 C16 C15 120.51(18) . . ? C22 C17 C18 118.15(18) . . ? C22 C17 P1 118.22(15) . . ? C18 C17 P1 123.60(15) . . ? C19 C18 C17 120.7(2) . . ? C20 C19 C18 120.1(2) . . ? C21 C20 C19 119.8(2) . . ? C20 C21 C22 120.15(19) . . ? C21 C22 C17 121.01(19) . . ? C28 C23 C24 117.60(17) . . ? C28 C23 P2 121.83(15) . . ? C24 C23 P2 120.46(14) . . ? C25 C24 C23 121.15(18) . . ? C26 C25 C24 120.53(19) . . ? C27 C26 C25 119.30(19) . . ? C26 C27 C28 120.3(2) . . ? C23 C28 C27 121.05(19) . . ? C30 C29 C34 118.76(18) . . ? C30 C29 P2 122.82(14) . . ? C34 C29 P2 118.38(15) . . ? C31 C30 C29 120.63(19) . . ? C32 C31 C30 120.1(2) . . ? C33 C32 C31 119.82(19) . . ? C32 C33 C34 120.1(2) . . ? C33 C34 C29 120.53(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Fe1 Fe2 C3 122.38(12) . . . . ? P1 Fe1 Fe2 C3 -15.72(7) . . . . ? P2 Fe1 Fe2 C3 -93.51(7) . . . . ? S1 Fe1 Fe2 C3 -176.92(7) . . . . ? S2 Fe1 Fe2 C3 68.81(7) . . . . ? C1 Fe1 Fe2 C4 -143.71(12) . . . . ? P1 Fe1 Fe2 C4 78.19(7) . . . . ? P2 Fe1 Fe2 C4 0.40(7) . . . . ? S1 Fe1 Fe2 C4 -83.02(7) . . . . ? S2 Fe1 Fe2 C4 162.71(8) . . . . ? C1 Fe1 Fe2 C2 -18.71(16) . . . . ? P1 Fe1 Fe2 C2 -156.81(12) . . . . ? P2 Fe1 Fe2 C2 125.40(12) . . . . ? S1 Fe1 Fe2 C2 41.98(12) . . . . ? S2 Fe1 Fe2 C2 -72.28(12) . . . . ? C1 Fe1 Fe2 S1 -60.69(10) . . . . ? P1 Fe1 Fe2 S1 161.21(2) . . . . ? P2 Fe1 Fe2 S1 83.42(2) . . . . ? S2 Fe1 Fe2 S1 -114.26(2) . . . . ? C1 Fe1 Fe2 S2 53.57(10) . . . . ? P1 Fe1 Fe2 S2 -84.53(2) . . . . ? P2 Fe1 Fe2 S2 -162.32(2) . . . . ? S1 Fe1 Fe2 S2 114.26(2) . . . . ? C1 Fe1 P1 N1 101.73(8) . . . . ? P2 Fe1 P1 N1 0.37(5) . . . . ? S1 Fe1 P1 N1 -58.61(8) . . . . ? S2 Fe1 P1 N1 -161.30(5) . . . . ? Fe2 Fe1 P1 N1 -105.60(5) . . . . ? C1 Fe1 P1 C11 -143.75(10) . . . . ? P2 Fe1 P1 C11 114.88(7) . . . . ? S1 Fe1 P1 C11 55.91(10) . . . . ? S2 Fe1 P1 C11 -46.78(7) . . . . ? Fe2 Fe1 P1 C11 8.92(7) . . . . ? C1 Fe1 P1 C17 -8.60(10) . . . . ? P2 Fe1 P1 C17 -109.97(8) . . . . ? S1 Fe1 P1 C17 -168.95(8) . . . . ? S2 Fe1 P1 C17 88.36(8) . . . . ? Fe2 Fe1 P1 C17 144.07(7) . . . . ? C1 Fe1 P1 P2 101.37(7) . . . . ? S1 Fe1 P1 P2 -58.98(6) . . . . ? S2 Fe1 P1 P2 -161.67(2) . . . . ? Fe2 Fe1 P1 P2 -105.966(19) . . . . ? C1 Fe1 P2 N1 -97.90(9) . . . . ? P1 Fe1 P2 N1 -0.37(5) . . . . ? S1 Fe1 P2 N1 161.43(5) . . . . ? S2 Fe1 P2 N1 61.29(8) . . . . ? Fe2 Fe1 P2 N1 106.15(5) . . . . ? C1 Fe1 P2 C29 149.12(10) . . . . ? P1 Fe1 P2 C29 -113.35(8) . . . . ? S1 Fe1 P2 C29 48.45(8) . . . . ? S2 Fe1 P2 C29 -51.69(10) . . . . ? Fe2 Fe1 P2 C29 -6.83(8) . . . . ? C1 Fe1 P2 C23 16.96(10) . . . . ? P1 Fe1 P2 C23 114.49(7) . . . . ? S1 Fe1 P2 C23 -83.71(7) . . . . ? S2 Fe1 P2 C23 176.15(8) . . . . ? Fe2 Fe1 P2 C23 -138.99(7) . . . . ? C1 Fe1 P2 P1 -97.53(7) . . . . ? S1 Fe1 P2 P1 161.80(2) . . . . ? S2 Fe1 P2 P1 61.66(6) . . . . ? Fe2 Fe1 P2 P1 106.518(18) . . . . ? C11 P1 P2 N1 75.88(11) . . . . ? C17 P1 P2 N1 -70.48(11) . . . . ? Fe1 P1 P2 N1 179.43(8) . . . . ? N1 P1 P2 C29 -71.04(11) . . . . ? C11 P1 P2 C29 4.84(11) . . . . ? C17 P1 P2 C29 -141.52(10) . . . . ? Fe1 P1 P2 C29 108.39(8) . . . . ? N1 P1 P2 C23 73.90(11) . . . . ? C11 P1 P2 C23 149.78(10) . . . . ? C17 P1 P2 C23 3.42(11) . . . . ? Fe1 P1 P2 C23 -106.66(8) . . . . ? N1 P1 P2 Fe1 -179.43(8) . . . . ? C11 P1 P2 Fe1 -103.56(7) . . . . ? C17 P1 P2 Fe1 110.09(7) . . . . ? C1 Fe1 S1 C5 37.58(10) . . . . ? P1 Fe1 S1 C5 -161.90(9) . . . . ? P2 Fe1 S1 C5 143.11(7) . . . . ? S2 Fe1 S1 C5 -57.32(8) . . . . ? Fe2 Fe1 S1 C5 -105.95(8) . . . . ? C1 Fe1 S1 Fe2 143.53(7) . . . . ? P1 Fe1 S1 Fe2 -55.95(6) . . . . ? P2 Fe1 S1 Fe2 -110.939(19) . . . . ? S2 Fe1 S1 Fe2 48.637(17) . . . . ? C3 Fe2 S1 C5 113.9(2) . . . . ? C4 Fe2 S1 C5 -151.40(10) . . . . ? C2 Fe2 S1 C5 -53.78(10) . . . . ? S2 Fe2 S1 C5 56.22(8) . . . . ? Fe1 Fe2 S1 C5 103.74(8) . . . . ? C3 Fe2 S1 Fe1 10.1(2) . . . . ? C4 Fe2 S1 Fe1 104.86(7) . . . . ? C2 Fe2 S1 Fe1 -157.52(7) . . . . ? S2 Fe2 S1 Fe1 -47.521(17) . . . . ? C1 Fe1 S2 C7 -40.98(10) . . . . ? P1 Fe1 S2 C7 -143.27(8) . . . . ? P2 Fe1 S2 C7 159.25(9) . . . . ? S1 Fe1 S2 C7 57.44(8) . . . . ? Fe2 Fe1 S2 C7 106.03(8) . . . . ? C1 Fe1 S2 Fe2 -147.01(7) . . . . ? P1 Fe1 S2 Fe2 110.700(18) . . . . ? P2 Fe1 S2 Fe2 53.22(6) . . . . ? S1 Fe1 S2 Fe2 -48.594(17) . . . . ? C3 Fe2 S2 C7 136.78(10) . . . . ? C4 Fe2 S2 C7 -143.34(17) . . . . ? C2 Fe2 S2 C7 40.09(11) . . . . ? S1 Fe2 S2 C7 -57.30(8) . . . . ? Fe1 Fe2 S2 C7 -104.84(8) . . . . ? C3 Fe2 S2 Fe1 -118.38(6) . . . . ? C4 Fe2 S2 Fe1 -38.51(15) . . . . ? C2 Fe2 S2 Fe1 144.93(7) . . . . ? S1 Fe2 S2 Fe1 47.532(17) . . . . ? C29 P2 N1 C8 -79.81(16) . . . . ? C23 P2 N1 C8 26.76(17) . . . . ? Fe1 P2 N1 C8 153.18(15) . . . . ? P1 P2 N1 C8 152.72(19) . . . . ? C29 P2 N1 P1 127.48(8) . . . . ? C23 P2 N1 P1 -125.96(8) . . . . ? Fe1 P2 N1 P1 0.46(7) . . . . ? C11 P1 N1 C8 84.54(17) . . . . ? C17 P1 N1 C8 -25.20(17) . . . . ? Fe1 P1 N1 C8 -151.82(15) . . . . ? P2 P1 N1 C8 -151.4(2) . . . . ? C11 P1 N1 P2 -124.11(8) . . . . ? C17 P1 N1 P2 126.15(8) . . . . ? Fe1 P1 N1 P2 -0.46(7) . . . . ? P1 Fe1 C1 O1 132.7(14) . . . . ? P2 Fe1 C1 O1 -153.6(14) . . . . ? S1 Fe1 C1 O1 -54.4(14) . . . . ? S2 Fe1 C1 O1 33.7(14) . . . . ? Fe2 Fe1 C1 O1 -7.9(14) . . . . ? C3 Fe2 C2 O2 105(4) . . . . ? C4 Fe2 C2 O2 15(4) . . . . ? S1 Fe2 C2 O2 -78(4) . . . . ? S2 Fe2 C2 O2 -166(4) . . . . ? Fe1 Fe2 C2 O2 -111(4) . . . . ? C4 Fe2 C3 O3 100(3) . . . . ? C2 Fe2 C3 O3 3(3) . . . . ? S1 Fe2 C3 O3 -164(3) . . . . ? S2 Fe2 C3 O3 -107(3) . . . . ? Fe1 Fe2 C3 O3 -156(3) . . . . ? C3 Fe2 C4 O4 -45.8(18) . . . . ? C2 Fe2 C4 O4 51.9(18) . . . . ? S1 Fe2 C4 O4 150.8(18) . . . . ? S2 Fe2 C4 O4 -124.9(17) . . . . ? Fe1 Fe2 C4 O4 -155.9(18) . . . . ? Fe1 S1 C5 C6 66.23(17) . . . . ? Fe2 S1 C5 C6 -9.95(19) . . . . ? S1 C5 C6 C7 -60.1(2) . . . . ? C5 C6 C7 S2 59.0(2) . . . . ? Fe1 S2 C7 C6 -65.04(17) . . . . ? Fe2 S2 C7 C6 11.51(19) . . . . ? P2 N1 C8 C9 150.91(15) . . . . ? P1 N1 C8 C9 -64.7(2) . . . . ? N1 C8 C9 C10 125.6(2) . . . . ? N1 P1 C11 C16 18.77(18) . . . . ? C17 P1 C11 C16 128.82(16) . . . . ? Fe1 P1 C11 C16 -88.23(16) . . . . ? P2 P1 C11 C16 -22.90(19) . . . . ? N1 P1 C11 C12 -167.09(15) . . . . ? C17 P1 C11 C12 -57.03(17) . . . . ? Fe1 P1 C11 C12 85.91(16) . . . . ? P2 P1 C11 C12 151.24(13) . . . . ? C16 C11 C12 C13 -3.4(3) . . . . ? P1 C11 C12 C13 -177.73(16) . . . . ? C11 C12 C13 C14 1.2(3) . . . . ? C12 C13 C14 C15 1.3(3) . . . . ? C13 C14 C15 C16 -1.7(3) . . . . ? C12 C11 C16 C15 3.1(3) . . . . ? P1 C11 C16 C15 177.29(16) . . . . ? C14 C15 C16 C11 -0.6(3) . . . . ? N1 P1 C17 C22 -67.94(17) . . . . ? C11 P1 C17 C22 178.68(16) . . . . ? Fe1 P1 C17 C22 37.68(18) . . . . ? P2 P1 C17 C22 -28.79(18) . . . . ? N1 P1 C17 C18 110.28(18) . . . . ? C11 P1 C17 C18 -3.1(2) . . . . ? Fe1 P1 C17 C18 -144.09(16) . . . . ? P2 P1 C17 C18 149.44(16) . . . . ? C22 C17 C18 C19 0.9(3) . . . . ? P1 C17 C18 C19 -177.34(19) . . . . ? C17 C18 C19 C20 1.5(4) . . . . ? C18 C19 C20 C21 -2.6(4) . . . . ? C19 C20 C21 C22 1.5(4) . . . . ? C20 C21 C22 C17 0.9(3) . . . . ? C18 C17 C22 C21 -2.1(3) . . . . ? P1 C17 C22 C21 176.25(17) . . . . ? N1 P2 C23 C28 -92.89(18) . . . . ? C29 P2 C23 C28 17.81(19) . . . . ? Fe1 P2 C23 C28 158.94(15) . . . . ? P1 P2 C23 C28 -134.13(16) . . . . ? N1 P2 C23 C24 91.02(16) . . . . ? C29 P2 C23 C24 -158.29(16) . . . . ? Fe1 P2 C23 C24 -17.15(18) . . . . ? P1 P2 C23 C24 49.77(18) . . . . ? C28 C23 C24 C25 -2.1(3) . . . . ? P2 C23 C24 C25 174.11(16) . . . . ? C23 C24 C25 C26 0.2(3) . . . . ? C24 C25 C26 C27 2.4(3) . . . . ? C25 C26 C27 C28 -3.1(4) . . . . ? C24 C23 C28 C27 1.5(3) . . . . ? P2 C23 C28 C27 -174.72(19) . . . . ? C26 C27 C28 C23 1.1(4) . . . . ? N1 P2 C29 C30 -2.68(17) . . . . ? C23 P2 C29 C30 -114.81(16) . . . . ? Fe1 P2 C29 C30 104.64(15) . . . . ? P1 P2 C29 C30 37.31(18) . . . . ? N1 P2 C29 C34 179.71(14) . . . . ? C23 P2 C29 C34 67.58(16) . . . . ? Fe1 P2 C29 C34 -72.98(16) . . . . ? P1 P2 C29 C34 -140.31(13) . . . . ? C34 C29 C30 C31 -0.2(3) . . . . ? P2 C29 C30 C31 -177.76(15) . . . . ? C29 C30 C31 C32 0.7(3) . . . . ? C30 C31 C32 C33 -0.6(3) . . . . ? C31 C32 C33 C34 -0.1(3) . . . . ? C32 C33 C34 C29 0.7(3) . . . . ? C30 C29 C34 C33 -0.6(3) . . . . ? P2 C29 C34 C33 177.14(15) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.746 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.078