# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Changneng Chen' _publ_contact_author_address ; Chinese Academy of Sciences Fuzhou Fujian 350002 CHINA ; _publ_contact_author_email CCN@FJIRSM.AC.CN _publ_section_title ; N- CnH2n-1-1, 3-azapropanedithiolate (n = 5, 6, 7) bridged diiron complexes as mimics for the active site of [Fe]-only hydrogenases: The influence of the bridge to diiron complexes ; loop_ _publ_author_name 'Chang-Neng Chen' 'Hui Chen' 'Ming-Qiang Hu' 'Qiutian Liu' ; Chengbing Ma ; 'Youtao Si' data_1 _database_code_depnum_ccdc_archive 'CCDC 622703' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H13 Fe2 N O6 S2' _chemical_formula_weight 455.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.7471(9) _cell_length_b 11.7596(15) _cell_length_c 19.604(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.778(5) _cell_angle_gamma 90.00 _cell_volume 1785.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3301 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max .23 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 1.885 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .7295 _exptl_absorpt_correction_T_max 1.0000 _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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 13615 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4077 _reflns_number_gt 3107 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+1.1600P] 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 4077 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0707 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 -0.00647(6) 0.45820(4) 0.15836(2) 0.04382(15) Uani 1 1 d . . . Fe2 Fe 0.28461(6) 0.55033(4) 0.15636(2) 0.04381(15) Uani 1 1 d . . . S2 S 0.21740(11) 0.40471(7) 0.22564(5) 0.0456(2) Uani 1 1 d . . . S1 S 0.04917(12) 0.63366(7) 0.20033(5) 0.0472(2) Uani 1 1 d . . . O6 O 0.4841(4) 0.3873(3) 0.07593(17) 0.0878(10) Uani 1 1 d . . . O4 O 0.5666(4) 0.6589(3) 0.23355(18) 0.0855(10) Uani 1 1 d . . . O3 O -0.3097(4) 0.3761(3) 0.23053(16) 0.0771(9) Uani 1 1 d . . . C6 C 0.4074(5) 0.4509(3) 0.1068(2) 0.0569(9) Uani 1 1 d . . . C5 C 0.2605(5) 0.6442(4) 0.0848(2) 0.0606(10) Uani 1 1 d . . . O1 O -0.1876(5) 0.5682(3) 0.04467(18) 0.1033(12) Uani 1 1 d . . . O5 O 0.2418(5) 0.7036(3) 0.03938(16) 0.0909(10) Uani 1 1 d . . . O2 O 0.0673(5) 0.2540(3) 0.07944(18) 0.0979(11) Uani 1 1 d . . . C3 C -0.1911(5) 0.4084(3) 0.20402(19) 0.0515(9) Uani 1 1 d . . . C4 C 0.4579(5) 0.6176(3) 0.2034(2) 0.0563(9) Uani 1 1 d . . . C2 C 0.0354(5) 0.3335(4) 0.1095(2) 0.0626(10) Uani 1 1 d . . . C1 C -0.1168(6) 0.5260(4) 0.0890(2) 0.0649(11) Uani 1 1 d . . . N1 N 0.0338(5) 0.5198(3) 0.32313(19) 0.0814(12) Uani 1 1 d . . . C8 C 0.1853(5) 0.4507(3) 0.31393(19) 0.0593(10) Uani 1 1 d . . . H8A H 0.1767 0.3839 0.3427 0.071 Uiso 1 1 calc R . . H8B H 0.2859 0.4934 0.3290 0.071 Uiso 1 1 calc R . . C7 C 0.0578(6) 0.6312(3) 0.29423(19) 0.0676(12) Uani 1 1 d . . . H7A H 0.1688 0.6606 0.3095 0.081 Uiso 1 1 calc R . . H7B H -0.0307 0.6815 0.3114 0.081 Uiso 1 1 calc R . . C9 C -0.0599(7) 0.5091(4) 0.3803(3) 0.1008(19) Uani 1 1 d . . . H9A H 0.0245 0.5334 0.4150 0.121 Uiso 1 1 calc R . . C13 C -0.1022(7) 0.3910(4) 0.4054(3) 0.0895(16) Uani 1 1 d . . . H13A H -0.0996 0.3367 0.3682 0.107 Uiso 1 1 calc R . . H13B H -0.0201 0.3672 0.4404 0.107 Uiso 1 1 calc R . . C10 C -0.2054(7) 0.5822(4) 0.3965(3) 0.0877(15) Uani 1 1 d . . . H10A H -0.2675 0.6032 0.3551 0.105 Uiso 1 1 calc R . . H10B H -0.1650 0.6510 0.4188 0.105 Uiso 1 1 calc R . . C12 C -0.2810(9) 0.3995(5) 0.4341(4) 0.135(3) Uani 1 1 d . . . H12A H -0.3640 0.3645 0.4032 0.163 Uiso 1 1 calc R . . H12B H -0.2859 0.3605 0.4777 0.163 Uiso 1 1 calc R . . C11 C -0.3204(9) 0.5174(5) 0.4426(4) 0.131(3) Uani 1 1 d . . . H11A H -0.3003 0.5402 0.4896 0.157 Uiso 1 1 calc R . . H11B H -0.4405 0.5318 0.4309 0.157 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 0.0381(3) 0.0422(3) 0.0511(3) -0.0001(2) 0.0003(2) -0.00506(19) Fe2 0.0377(3) 0.0451(3) 0.0488(3) -0.0015(2) 0.0051(2) -0.0050(2) S2 0.0423(5) 0.0390(5) 0.0555(5) 0.0008(4) 0.0038(4) 0.0064(3) S1 0.0486(5) 0.0361(4) 0.0571(5) 0.0033(4) 0.0078(4) 0.0018(3) O6 0.075(2) 0.100(3) 0.088(2) -0.0262(19) 0.0225(18) 0.0175(19) O4 0.065(2) 0.079(2) 0.112(3) -0.0164(18) -0.0234(19) -0.0157(16) O3 0.0504(17) 0.086(2) 0.095(2) 0.0189(17) 0.0134(16) -0.0075(15) C6 0.042(2) 0.070(3) 0.060(2) -0.0036(19) 0.0085(18) -0.0046(18) C5 0.055(2) 0.066(3) 0.061(2) 0.001(2) 0.009(2) -0.0078(19) O1 0.107(3) 0.114(3) 0.087(2) 0.035(2) -0.036(2) -0.015(2) O5 0.105(3) 0.094(2) 0.073(2) 0.0318(19) 0.0054(19) -0.010(2) O2 0.110(3) 0.079(2) 0.105(3) -0.047(2) 0.019(2) -0.0115(19) C3 0.049(2) 0.048(2) 0.057(2) 0.0072(17) -0.0004(18) 0.0024(16) C4 0.049(2) 0.050(2) 0.070(3) -0.0030(18) 0.0066(19) -0.0037(17) C2 0.060(3) 0.064(3) 0.063(3) -0.009(2) 0.003(2) -0.016(2) C1 0.061(3) 0.069(3) 0.064(3) 0.012(2) -0.010(2) -0.016(2) N1 0.111(3) 0.055(2) 0.080(2) 0.0240(17) 0.053(2) 0.032(2) C8 0.066(3) 0.055(2) 0.057(2) 0.0067(18) 0.0110(19) 0.0104(19) C7 0.102(3) 0.043(2) 0.058(2) 0.0005(17) 0.027(2) 0.009(2) C9 0.092(4) 0.067(3) 0.145(5) 0.030(3) 0.064(4) 0.017(3) C13 0.112(4) 0.063(3) 0.094(4) 0.022(2) 0.036(3) 0.014(3) C10 0.105(4) 0.072(3) 0.088(3) 0.009(3) 0.045(3) 0.020(3) C12 0.129(6) 0.086(4) 0.194(7) 0.021(4) 0.097(5) -0.003(4) C11 0.110(5) 0.112(5) 0.172(6) 0.044(5) 0.069(5) 0.022(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C2 1.784(4) . ? Fe1 C1 1.785(4) . ? Fe1 C3 1.796(4) . ? Fe1 S2 2.2541(10) . ? Fe1 S1 2.2606(10) . ? Fe1 Fe2 2.5025(7) . ? Fe2 C5 1.793(4) . ? Fe2 C6 1.800(4) . ? Fe2 C4 1.801(4) . ? Fe2 S2 2.2512(10) . ? Fe2 S1 2.2523(10) . ? S2 C8 1.833(4) . ? S1 C7 1.841(4) . ? O6 C6 1.135(4) . ? O4 C4 1.132(4) . ? O3 C3 1.128(4) . ? C5 O5 1.139(5) . ? O1 C1 1.135(5) . ? O2 C2 1.134(5) . ? N1 C9 1.349(6) . ? N1 C7 1.440(5) . ? N1 C8 1.441(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C10 1.456(6) . ? C9 C13 1.511(6) . ? C9 H9A 0.9800 . ? C13 C12 1.505(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C10 C11 1.488(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C12 C11 1.430(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 C1 92.7(2) . . ? C2 Fe1 C3 98.71(18) . . ? C1 Fe1 C3 98.57(18) . . ? C2 Fe1 S2 86.62(14) . . ? C1 Fe1 S2 158.03(14) . . ? C3 Fe1 S2 103.24(12) . . ? C2 Fe1 S1 155.58(13) . . ? C1 Fe1 S1 87.50(14) . . ? C3 Fe1 S1 105.42(12) . . ? S2 Fe1 S1 84.28(4) . . ? C2 Fe1 Fe2 100.19(13) . . ? C1 Fe1 Fe2 102.53(13) . . ? C3 Fe1 Fe2 150.82(12) . . ? S2 Fe1 Fe2 56.20(3) . . ? S1 Fe1 Fe2 56.16(3) . . ? C5 Fe2 C6 91.62(19) . . ? C5 Fe2 C4 101.49(18) . . ? C6 Fe2 C4 99.55(17) . . ? C5 Fe2 S2 156.65(13) . . ? C6 Fe2 S2 87.67(13) . . ? C4 Fe2 S2 101.63(13) . . ? C5 Fe2 S1 87.44(13) . . ? C6 Fe2 S1 157.78(12) . . ? C4 Fe2 S1 102.39(13) . . ? S2 Fe2 S1 84.54(3) . . ? C5 Fe2 Fe1 101.24(13) . . ? C6 Fe2 Fe1 102.13(12) . . ? C4 Fe2 Fe1 147.92(13) . . ? S2 Fe2 Fe1 56.31(3) . . ? S1 Fe2 Fe1 56.48(3) . . ? C8 S2 Fe2 112.38(13) . . ? C8 S2 Fe1 110.91(13) . . ? Fe2 S2 Fe1 67.49(3) . . ? C7 S1 Fe2 110.92(15) . . ? C7 S1 Fe1 110.71(12) . . ? Fe2 S1 Fe1 67.36(3) . . ? O6 C6 Fe2 179.4(4) . . ? O5 C5 Fe2 178.6(4) . . ? O3 C3 Fe1 177.6(4) . . ? O4 C4 Fe2 179.2(4) . . ? O2 C2 Fe1 177.7(4) . . ? O1 C1 Fe1 179.4(4) . . ? C9 N1 C7 119.1(4) . . ? C9 N1 C8 119.9(4) . . ? C7 N1 C8 110.7(3) . . ? N1 C8 S2 113.9(3) . . ? N1 C8 H8A 108.8 . . ? S2 C8 H8A 108.8 . . ? N1 C8 H8B 108.8 . . ? S2 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? N1 C7 S1 113.9(3) . . ? N1 C7 H7A 108.8 . . ? S1 C7 H7A 108.8 . . ? N1 C7 H7B 108.8 . . ? S1 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N1 C9 C10 123.5(4) . . ? N1 C9 C13 118.6(5) . . ? C10 C9 C13 107.4(4) . . ? N1 C9 H9A 100.8 . . ? C10 C9 H9A 100.8 . . ? C13 C9 H9A 100.8 . . ? C12 C13 C9 105.4(4) . . ? C12 C13 H13A 110.7 . . ? C9 C13 H13A 110.7 . . ? C12 C13 H13B 110.7 . . ? C9 C13 H13B 110.7 . . ? H13A C13 H13B 108.8 . . ? C9 C10 C11 107.6(4) . . ? C9 C10 H10A 110.2 . . ? C11 C10 H10A 110.2 . . ? C9 C10 H10B 110.2 . . ? C11 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? C11 C12 C13 107.9(5) . . ? C11 C12 H12A 110.1 . . ? C13 C12 H12A 110.1 . . ? C11 C12 H12B 110.1 . . ? C13 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? C12 C11 C10 107.1(5) . . ? C12 C11 H11A 110.3 . . ? C10 C11 H11A 110.3 . . ? C12 C11 H11B 110.3 . . ? C10 C11 H11B 110.3 . . ? H11A C11 H11B 108.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.398 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.065 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; # Attachment '2 for B616236C.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 622704' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H15 Fe2 N O6 S2' _chemical_formula_weight 469.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6577(2) _cell_length_b 13.08730(10) _cell_length_c 14.9696(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.7930(10) _cell_angle_gamma 90.00 _cell_volume 1889.81(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 107 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 25.06 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max .56 _exptl_crystal_size_mid .50 _exptl_crystal_size_min .46 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 1.784 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .7098 _exptl_absorpt_correction_T_max 1.0000 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 9659 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.06 _reflns_number_total 3333 _reflns_number_gt 2973 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+6.2068P] _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 3333 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0625 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1328 _refine_ls_wR_factor_gt 0.1259 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.22381(7) 0.30534(5) 0.21219(5) 0.0493(2) Uani 1 1 d . . . Fe2 Fe 0.25145(7) 0.11693(5) 0.24577(5) 0.0481(2) Uani 1 1 d . . . S2 S 0.06075(14) 0.20717(9) 0.27220(9) 0.0531(3) Uani 1 1 d . . . S1 S 0.22719(14) 0.18319(11) 0.10711(9) 0.0540(3) Uani 1 1 d . . . N1 N -0.0565(5) 0.2188(4) 0.1024(4) 0.0651(12) Uani 1 1 d . . . O5 O 0.5450(5) 0.0813(4) 0.2131(4) 0.0936(15) Uani 1 1 d . . . O1 O 0.0655(5) 0.4679(4) 0.1176(4) 0.0962(15) Uani 1 1 d . . . O2 O 0.2570(6) 0.4033(4) 0.3875(3) 0.0965(16) Uani 1 1 d . . . O4 O 0.1353(6) -0.0863(4) 0.2150(4) 0.1087(19) Uani 1 1 d . . . O3 O 0.5038(5) 0.3666(4) 0.1683(4) 0.1074(18) Uani 1 1 d . . . C5 C 0.4309(6) 0.0949(4) 0.2259(4) 0.0619(14) Uani 1 1 d . . . C8 C -0.0793(5) 0.1792(4) 0.1898(4) 0.0632(15) Uani 1 1 d . . . H8A H -0.0910 0.1057 0.1857 0.076 Uiso 1 1 calc R . . H8B H -0.1648 0.2077 0.2104 0.076 Uiso 1 1 calc R . . C4 C 0.1824(6) -0.0084(4) 0.2278(4) 0.0667(15) Uani 1 1 d . . . C9 C -0.1881(7) 0.2358(5) 0.0482(5) 0.086(2) Uani 1 1 d . . . H9A H -0.2523 0.2600 0.0923 0.103 Uiso 1 1 calc R . . C3 C 0.3937(7) 0.3428(5) 0.1839(4) 0.0699(16) Uani 1 1 d . . . C7 C 0.0504(6) 0.1638(5) 0.0578(4) 0.0698(16) Uani 1 1 d . . . H7A H 0.0484 0.1850 -0.0044 0.084 Uiso 1 1 calc R . . H7B H 0.0291 0.0914 0.0590 0.084 Uiso 1 1 calc R . . C2 C 0.2449(6) 0.3655(4) 0.3189(4) 0.0649(15) Uani 1 1 d . . . C1 C 0.1249(7) 0.4040(4) 0.1534(4) 0.0672(15) Uani 1 1 d . . . O6 O 0.2974(7) 0.1015(5) 0.4407(3) 0.1133(19) Uani 1 1 d . . . C14 C -0.2566(6) 0.1390(5) 0.0118(5) 0.0763(18) Uani 1 1 d . . . H14A H -0.2745 0.0936 0.0611 0.092 Uiso 1 1 calc R . . H14B H -0.1937 0.1044 -0.0267 0.092 Uiso 1 1 calc R . . C6 C 0.2815(6) 0.1079(5) 0.3656(4) 0.0687(15) Uani 1 1 d . . . C11 C -0.3262(8) 0.3394(6) -0.0597(6) 0.105(3) Uani 1 1 d . . . H11A H -0.3876 0.3694 -0.0175 0.126 Uiso 1 1 calc R . . H11B H -0.3145 0.3882 -0.1075 0.126 Uiso 1 1 calc R . . C10 C -0.1834(9) 0.3164(6) -0.0118(7) 0.129(4) Uani 1 1 d . . . H10A H -0.1171 0.3004 -0.0564 0.155 Uiso 1 1 calc R . . H10B H -0.1509 0.3771 0.0200 0.155 Uiso 1 1 calc R . . C13 C -0.3922(9) 0.1613(7) -0.0408(7) 0.120(3) Uani 1 1 d . . . H13A H -0.4188 0.1007 -0.0748 0.144 Uiso 1 1 calc R . . H13B H -0.4634 0.1735 0.0014 0.144 Uiso 1 1 calc R . . C12 C -0.3901(11) 0.2417(7) -0.0978(8) 0.140(4) Uani 1 1 d . . . H12A H -0.4846 0.2563 -0.1189 0.168 Uiso 1 1 calc R . . H12B H -0.3393 0.2217 -0.1494 0.168 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 0.0516(4) 0.0409(4) 0.0560(4) 0.0018(3) 0.0069(3) -0.0027(3) Fe2 0.0471(4) 0.0410(4) 0.0562(4) -0.0004(3) 0.0046(3) 0.0027(3) S2 0.0508(7) 0.0449(7) 0.0646(8) 0.0017(6) 0.0147(6) 0.0020(6) S1 0.0524(7) 0.0585(8) 0.0512(7) -0.0033(6) 0.0055(6) -0.0003(6) N1 0.049(3) 0.062(3) 0.083(3) 0.003(2) -0.008(2) 0.004(2) O5 0.053(3) 0.112(4) 0.117(4) 0.001(3) 0.012(2) 0.017(3) O1 0.108(4) 0.064(3) 0.116(4) 0.029(3) -0.006(3) 0.011(3) O2 0.140(5) 0.077(3) 0.073(3) -0.019(3) 0.014(3) -0.011(3) O4 0.113(4) 0.060(3) 0.158(5) -0.025(3) 0.047(4) -0.031(3) O3 0.076(3) 0.116(4) 0.133(5) -0.031(3) 0.035(3) -0.038(3) C5 0.060(4) 0.057(3) 0.068(4) -0.002(3) -0.001(3) 0.006(3) C8 0.044(3) 0.056(3) 0.090(4) 0.003(3) 0.006(3) 0.000(2) C4 0.064(3) 0.048(3) 0.089(4) -0.002(3) 0.016(3) 0.001(3) C9 0.073(4) 0.064(4) 0.118(6) 0.017(4) -0.033(4) -0.002(3) C3 0.070(4) 0.064(4) 0.077(4) -0.009(3) 0.016(3) -0.016(3) C7 0.067(4) 0.075(4) 0.066(4) -0.002(3) -0.014(3) -0.002(3) C2 0.073(4) 0.049(3) 0.074(4) -0.003(3) 0.013(3) -0.002(3) C1 0.074(4) 0.049(3) 0.079(4) 0.008(3) 0.008(3) -0.001(3) O6 0.143(5) 0.136(5) 0.059(3) 0.009(3) -0.009(3) 0.007(4) C14 0.070(4) 0.061(4) 0.096(5) 0.005(3) -0.017(3) 0.002(3) C6 0.072(4) 0.066(4) 0.068(4) 0.004(3) 0.003(3) 0.002(3) C11 0.099(5) 0.080(5) 0.132(7) 0.028(5) -0.046(5) 0.005(4) C10 0.117(7) 0.091(6) 0.172(9) 0.047(6) -0.079(6) -0.029(5) C13 0.094(6) 0.083(5) 0.176(9) 0.014(6) -0.063(6) -0.012(4) C12 0.129(8) 0.106(7) 0.176(10) 0.016(7) -0.090(7) -0.002(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 C3 1.783(6) . ? Fe1 C2 1.784(7) . ? Fe1 C1 1.810(6) . ? Fe1 S1 2.2441(15) . ? Fe1 S2 2.2528(14) . ? Fe1 Fe2 2.5280(10) . ? Fe2 C4 1.786(6) . ? Fe2 C5 1.796(6) . ? Fe2 C6 1.806(7) . ? Fe2 S2 2.2393(14) . ? Fe2 S1 2.2511(15) . ? S2 C8 1.823(6) . ? S1 C7 1.845(6) . ? N1 C8 1.434(8) . ? N1 C7 1.448(8) . ? N1 C9 1.491(7) . ? O5 C5 1.142(7) . ? O1 C1 1.133(7) . ? O2 C2 1.141(7) . ? O4 C4 1.129(7) . ? O3 C3 1.143(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.387(10) . ? C9 C14 1.518(9) . ? C9 H9A 0.9800 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? O6 C6 1.131(7) . ? C14 C13 1.523(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C11 C12 1.519(12) . ? C11 C10 1.553(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C13 C12 1.357(12) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Fe1 C2 91.4(3) . . ? C3 Fe1 C1 99.1(3) . . ? C2 Fe1 C1 98.9(3) . . ? C3 Fe1 S1 89.1(2) . . ? C2 Fe1 S1 159.58(19) . . ? C1 Fe1 S1 101.1(2) . . ? C3 Fe1 S2 157.0(2) . . ? C2 Fe1 S2 86.91(19) . . ? C1 Fe1 S2 103.8(2) . . ? S1 Fe1 S2 84.70(5) . . ? C3 Fe1 Fe2 103.1(2) . . ? C2 Fe1 Fe2 104.23(19) . . ? C1 Fe1 Fe2 147.3(2) . . ? S1 Fe1 Fe2 55.91(4) . . ? S2 Fe1 Fe2 55.50(4) . . ? C4 Fe2 C5 100.6(3) . . ? C4 Fe2 C6 97.5(3) . . ? C5 Fe2 C6 92.5(3) . . ? C4 Fe2 S2 101.94(19) . . ? C5 Fe2 S2 157.29(19) . . ? C6 Fe2 S2 87.3(2) . . ? C4 Fe2 S1 101.2(2) . . ? C5 Fe2 S1 88.13(19) . . ? C6 Fe2 S1 160.9(2) . . ? S2 Fe2 S1 84.85(5) . . ? C4 Fe2 Fe1 146.2(2) . . ? C5 Fe2 Fe1 102.53(19) . . ? C6 Fe2 Fe1 105.8(2) . . ? S2 Fe2 Fe1 56.00(4) . . ? S1 Fe2 Fe1 55.65(4) . . ? C8 S2 Fe2 111.36(19) . . ? C8 S2 Fe1 110.8(2) . . ? Fe2 S2 Fe1 68.50(4) . . ? C7 S1 Fe1 109.5(2) . . ? C7 S1 Fe2 111.7(2) . . ? Fe1 S1 Fe2 68.44(4) . . ? C8 N1 C7 112.7(5) . . ? C8 N1 C9 112.7(5) . . ? C7 N1 C9 115.5(5) . . ? O5 C5 Fe2 179.7(6) . . ? N1 C8 S2 113.8(4) . . ? N1 C8 H8A 108.8 . . ? S2 C8 H8A 108.8 . . ? N1 C8 H8B 108.8 . . ? S2 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? O4 C4 Fe2 177.9(7) . . ? C10 C9 N1 114.3(6) . . ? C10 C9 C14 115.4(7) . . ? N1 C9 C14 114.5(5) . . ? C10 C9 H9A 103.4 . . ? N1 C9 H9A 103.4 . . ? C14 C9 H9A 103.4 . . ? O3 C3 Fe1 178.0(6) . . ? N1 C7 S1 114.5(4) . . ? N1 C7 H7A 108.6 . . ? S1 C7 H7A 108.6 . . ? N1 C7 H7B 108.6 . . ? S1 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? O2 C2 Fe1 179.2(6) . . ? O1 C1 Fe1 178.0(6) . . ? C9 C14 C13 112.0(6) . . ? C9 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? C9 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? O6 C6 Fe2 178.4(6) . . ? C12 C11 C10 110.2(7) . . ? C12 C11 H11A 109.6 . . ? C10 C11 H11A 109.6 . . ? C12 C11 H11B 109.6 . . ? C10 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? C9 C10 C11 112.9(7) . . ? C9 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? C9 C10 H10B 109.0 . . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C12 C13 C14 115.8(7) . . ? C12 C13 H13A 108.3 . . ? C14 C13 H13A 108.3 . . ? C12 C13 H13B 108.3 . . ? C14 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? C13 C12 C11 115.8(8) . . ? C13 C12 H12A 108.3 . . ? C11 C12 H12A 108.3 . . ? C13 C12 H12B 108.3 . . ? C11 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.614 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.076 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; # Attachment '3 for B616236C.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 622705' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H17 Fe2 N O6 S2' _chemical_formula_weight 483.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.604(3) _cell_length_b 12.035(4) _cell_length_c 15.428(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.439(6) _cell_angle_gamma 90.00 _cell_volume 1967.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5098 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max .62 _exptl_crystal_size_mid .60 _exptl_crystal_size_min .34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.717 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .8273 _exptl_absorpt_correction_T_max 1.0000 _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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 14835 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4478 _reflns_number_gt 3729 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+0.1022P] _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 4478 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0410 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.1074 _refine_ls_wR_factor_gt 0.0894 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 0.26685(3) 0.05147(3) 0.05797(2) 0.04105(12) Uani 1 1 d . . . Fe2 Fe 0.26935(3) 0.21088(3) 0.162959(19) 0.03606(12) Uani 1 1 d . . . S2 S 0.12952(5) 0.19390(5) 0.04954(4) 0.04050(15) Uani 1 1 d . . . S1 S 0.41595(5) 0.18540(5) 0.06309(4) 0.04104(15) Uani 1 1 d . . . C6 C 0.2752(3) 0.3591(2) 0.17808(16) 0.0515(6) Uani 1 1 d . . . N1 N 0.28144(18) 0.35605(16) -0.01521(12) 0.0411(4) Uani 1 1 d . . . C8 C 0.1681(2) 0.2940(2) -0.03548(16) 0.0473(6) Uani 1 1 d . . . H8A H 0.1778 0.2543 -0.0895 0.057 Uiso 1 1 calc R . . H8B H 0.0982 0.3454 -0.0441 0.057 Uiso 1 1 calc R . . C7 C 0.3915(2) 0.28842(19) -0.02413(16) 0.0451(6) Uani 1 1 d . . . H7A H 0.4651 0.3363 -0.0250 0.054 Uiso 1 1 calc R . . H7B H 0.3844 0.2498 -0.0793 0.054 Uiso 1 1 calc R . . C9 C 0.2920(2) 0.46897(19) -0.05478(16) 0.0437(5) Uani 1 1 d . . . H9A H 0.3742 0.4982 -0.0344 0.052 Uiso 1 1 calc R . . O5 O 0.0650(2) 0.1607(2) 0.27845(16) 0.0826(7) Uani 1 1 d . . . O6 O 0.2782(3) 0.45171(16) 0.19118(16) 0.0860(8) Uani 1 1 d . . . C10 C 0.2933(3) 0.4684(2) -0.15377(16) 0.0482(6) Uani 1 1 d . . . H10A H 0.2075 0.4600 -0.1773 0.058 Uiso 1 1 calc R . . H10B H 0.3417 0.4050 -0.1724 0.058 Uiso 1 1 calc R . . C5 C 0.1434(3) 0.1796(2) 0.23321(17) 0.0507(6) Uani 1 1 d . . . C15 C 0.1933(4) 0.5465(2) -0.0183(2) 0.0679(9) Uani 1 1 d . . . H15A H 0.1993 0.5423 0.0445 0.082 Uiso 1 1 calc R . . H15B H 0.1101 0.5201 -0.0371 0.082 Uiso 1 1 calc R . . O3 O 0.4503(3) -0.0969(2) 0.14645(17) 0.0894(8) Uani 1 1 d . . . C3 C 0.3794(3) -0.0396(2) 0.11023(18) 0.0561(7) Uani 1 1 d . . . O4 O 0.4564(2) 0.1410(2) 0.29700(15) 0.0898(8) Uani 1 1 d . . . O2 O 0.0608(2) -0.0869(2) 0.11822(16) 0.0843(7) Uani 1 1 d . . . C2 C 0.1393(3) -0.0335(2) 0.09402(18) 0.0542(7) Uani 1 1 d . . . O1 O 0.2769(3) -0.0288(2) -0.12132(15) 0.0971(9) Uani 1 1 d . . . C4 C 0.3845(3) 0.1689(2) 0.24461(17) 0.0547(6) Uani 1 1 d . . . C1 C 0.2732(3) 0.0024(2) -0.05247(19) 0.0607(7) Uani 1 1 d . . . C11 C 0.3503(3) 0.5750(3) -0.1903(2) 0.0650(8) Uani 1 1 d . . . H11A H 0.4192 0.5982 -0.1512 0.078 Uiso 1 1 calc R . . H11B H 0.3860 0.5570 -0.2454 0.078 Uiso 1 1 calc R . . C13 C 0.1670(4) 0.6921(3) -0.1386(2) 0.0781(10) Uani 1 1 d . . . H13A H 0.0938 0.6466 -0.1535 0.094 Uiso 1 1 calc R . . H13B H 0.1405 0.7691 -0.1433 0.094 Uiso 1 1 calc R . . C14 C 0.2055(4) 0.6698(3) -0.0455(2) 0.0771(10) Uani 1 1 d . . . H14A H 0.1538 0.7148 -0.0089 0.093 Uiso 1 1 calc R . . H14B H 0.2925 0.6929 -0.0354 0.093 Uiso 1 1 calc R . . C12 C 0.2623(4) 0.6722(3) -0.2043(2) 0.0831(11) Uani 1 1 d . . . H12A H 0.3133 0.7387 -0.2082 0.100 Uiso 1 1 calc R . . H12B H 0.2179 0.6624 -0.2600 0.100 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 0.0507(2) 0.0333(2) 0.0392(2) -0.00261(13) 0.00277(15) 0.00208(13) Fe2 0.0391(2) 0.03595(19) 0.03305(19) -0.00137(12) 0.00010(13) 0.00129(12) S2 0.0341(3) 0.0449(3) 0.0422(3) 0.0004(2) -0.0025(2) 0.0009(2) S1 0.0350(3) 0.0410(3) 0.0474(3) 0.0054(2) 0.0036(2) 0.0072(2) C6 0.0653(17) 0.0480(15) 0.0409(13) -0.0048(11) -0.0004(11) 0.0010(12) N1 0.0403(10) 0.0393(10) 0.0440(10) 0.0067(8) 0.0029(8) 0.0073(8) C8 0.0467(14) 0.0517(15) 0.0430(13) 0.0067(11) -0.0043(11) 0.0059(11) C7 0.0442(13) 0.0425(13) 0.0492(14) 0.0087(10) 0.0102(11) 0.0085(10) C9 0.0484(14) 0.0380(12) 0.0448(13) 0.0018(10) 0.0035(10) 0.0062(10) O5 0.0818(16) 0.0812(15) 0.0882(16) 0.0139(13) 0.0430(13) 0.0029(13) O6 0.148(3) 0.0404(12) 0.0687(15) -0.0126(10) -0.0017(14) -0.0056(12) C10 0.0530(15) 0.0480(14) 0.0439(13) 0.0038(11) 0.0073(11) 0.0074(11) C5 0.0568(16) 0.0459(14) 0.0499(14) 0.0016(11) 0.0098(12) 0.0055(12) C15 0.092(2) 0.0552(17) 0.0583(17) 0.0097(13) 0.0244(16) 0.0281(15) O3 0.0943(19) 0.0734(16) 0.1014(18) 0.0298(14) 0.0138(14) 0.0373(14) C3 0.0664(18) 0.0435(14) 0.0593(17) 0.0054(12) 0.0142(14) 0.0106(12) O4 0.0853(17) 0.113(2) 0.0676(14) 0.0133(14) -0.0336(13) 0.0075(15) O2 0.0874(18) 0.0852(16) 0.0803(16) 0.0006(12) 0.0043(13) -0.0393(14) C2 0.0653(18) 0.0467(14) 0.0502(15) -0.0045(12) -0.0047(13) -0.0078(13) O1 0.156(3) 0.0873(18) 0.0485(13) -0.0192(12) 0.0061(14) 0.0077(17) C4 0.0581(17) 0.0609(17) 0.0445(14) 0.0014(12) -0.0047(12) -0.0026(13) C1 0.087(2) 0.0453(15) 0.0500(16) -0.0048(12) 0.0051(14) 0.0035(14) C11 0.0661(19) 0.0668(18) 0.0630(18) 0.0148(15) 0.0139(15) -0.0042(15) C13 0.081(2) 0.0593(19) 0.094(3) 0.0252(17) 0.0056(19) 0.0179(17) C14 0.080(2) 0.0583(19) 0.093(2) -0.0156(17) 0.0044(19) 0.0271(17) C12 0.100(3) 0.064(2) 0.085(2) 0.0196(18) 0.003(2) 0.0094(19) _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 1.788(3) . ? Fe1 C2 1.802(3) . ? Fe1 C1 1.807(3) . ? Fe1 S2 2.2495(8) . ? Fe1 S1 2.2569(8) . ? Fe1 Fe2 2.5103(7) . ? Fe2 C4 1.789(3) . ? Fe2 C5 1.795(3) . ? Fe2 C6 1.800(3) . ? Fe2 S2 2.2542(8) . ? Fe2 S1 2.2558(8) . ? S2 C8 1.840(3) . ? S1 C7 1.840(2) . ? C6 O6 1.133(3) . ? N1 C7 1.435(3) . ? N1 C8 1.438(3) . ? N1 C9 1.496(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C15 1.528(4) . ? C9 C10 1.528(3) . ? C9 H9A 0.9800 . ? O5 C5 1.131(3) . ? C10 C11 1.535(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C15 C14 1.549(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? O3 C3 1.147(3) . ? O4 C4 1.138(3) . ? O2 C2 1.129(3) . ? O1 C1 1.129(3) . ? C11 C12 1.506(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C13 C12 1.481(5) . ? C13 C14 1.500(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Fe1 C2 90.48(14) . . ? C3 Fe1 C1 100.00(13) . . ? C2 Fe1 C1 99.43(13) . . ? C3 Fe1 S2 155.75(9) . . ? C2 Fe1 S2 87.58(10) . . ? C1 Fe1 S2 104.16(10) . . ? C3 Fe1 S1 88.21(10) . . ? C2 Fe1 S1 158.16(9) . . ? C1 Fe1 S1 102.27(10) . . ? S2 Fe1 S1 84.75(3) . . ? C3 Fe1 Fe2 100.91(9) . . ? C2 Fe1 Fe2 102.82(9) . . ? C1 Fe1 Fe2 149.14(9) . . ? S2 Fe1 Fe2 56.21(2) . . ? S1 Fe1 Fe2 56.18(2) . . ? C4 Fe2 C5 91.07(13) . . ? C4 Fe2 C6 99.79(13) . . ? C5 Fe2 C6 98.72(12) . . ? C4 Fe2 S2 158.05(10) . . ? C5 Fe2 S2 88.16(9) . . ? C6 Fe2 S2 102.02(9) . . ? C4 Fe2 S1 88.47(10) . . ? C5 Fe2 S1 159.37(9) . . ? C6 Fe2 S1 101.68(9) . . ? S2 Fe2 S1 84.67(3) . . ? C4 Fe2 Fe1 103.10(10) . . ? C5 Fe2 Fe1 103.99(9) . . ? C6 Fe2 Fe1 147.20(8) . . ? S2 Fe2 Fe1 56.04(2) . . ? S1 Fe2 Fe1 56.22(2) . . ? C8 S2 Fe1 112.17(9) . . ? C8 S2 Fe2 109.59(9) . . ? Fe1 S2 Fe2 67.75(2) . . ? C7 S1 Fe2 109.17(8) . . ? C7 S1 Fe1 112.29(9) . . ? Fe2 S1 Fe1 67.60(2) . . ? O6 C6 Fe2 177.1(2) . . ? C7 N1 C8 111.1(2) . . ? C7 N1 C9 113.63(18) . . ? C8 N1 C9 117.34(19) . . ? N1 C8 S2 113.20(16) . . ? N1 C8 H8A 108.9 . . ? S2 C8 H8A 108.9 . . ? N1 C8 H8B 108.9 . . ? S2 C8 H8B 108.9 . . ? H8A C8 H8B 107.8 . . ? N1 C7 S1 113.70(16) . . ? N1 C7 H7A 108.8 . . ? S1 C7 H7A 108.8 . . ? N1 C7 H7B 108.8 . . ? S1 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N1 C9 C15 109.9(2) . . ? N1 C9 C10 114.07(19) . . ? C15 C9 C10 114.0(2) . . ? N1 C9 H9A 106.1 . . ? C15 C9 H9A 106.1 . . ? C10 C9 H9A 106.1 . . ? C9 C10 C11 112.6(2) . . ? C9 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? C9 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? O5 C5 Fe2 179.0(3) . . ? C9 C15 C14 114.8(3) . . ? C9 C15 H15A 108.6 . . ? C14 C15 H15A 108.6 . . ? C9 C15 H15B 108.6 . . ? C14 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? O3 C3 Fe1 177.7(3) . . ? O2 C2 Fe1 178.6(3) . . ? O4 C4 Fe2 178.9(3) . . ? O1 C1 Fe1 179.7(3) . . ? C12 C11 C10 116.8(3) . . ? C12 C11 H11A 108.1 . . ? C10 C11 H11A 108.1 . . ? C12 C11 H11B 108.1 . . ? C10 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? C12 C13 C14 117.4(3) . . ? C12 C13 H13A 108.0 . . ? C14 C13 H13A 108.0 . . ? C12 C13 H13B 108.0 . . ? C14 C13 H13B 108.0 . . ? H13A C13 H13B 107.2 . . ? C13 C14 C15 114.1(3) . . ? C13 C14 H14A 108.7 . . ? C15 C14 H14A 108.7 . . ? C13 C14 H14B 108.7 . . ? C15 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C13 C12 C11 117.7(3) . . ? C13 C12 H12A 107.9 . . ? C11 C12 H12A 107.9 . . ? C13 C12 H12B 107.9 . . ? C11 C12 H12B 107.9 . . ? H12A C12 H12B 107.2 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.483 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.137 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; # Attachment '4 for B616236C.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 622706' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H31 Fe2 N O4 P2 S2' _chemical_formula_weight 551.19 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 12.4237(5) _cell_length_b 14.1988(6) _cell_length_c 14.6021(6) _cell_angle_alpha 98.3330(10) _cell_angle_beta 91.9110(10) _cell_angle_gamma 94.4710(10) _cell_volume 2538.28(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 171 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 25.68 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max .30 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 1.454 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .712 _exptl_absorpt_correction_T_max .865 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 13807 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.68 _reflns_number_total 9410 _reflns_number_gt 8377 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2318P)^2^+8.5093P] 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 SHELXL _refine_ls_extinction_coef 0.017(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9410 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0897 _refine_ls_R_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.3076 _refine_ls_wR_factor_gt 0.2815 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 0.29557(9) 0.00448(7) 0.81982(7) 0.0469(3) Uani 1 1 d . . . Fe2 Fe 0.32093(8) -0.05961(6) 0.65189(6) 0.0410(3) Uani 1 1 d . . . S2 S 0.44058(14) 0.04593(12) 0.74041(12) 0.0456(4) Uani 1 1 d . . . P2 P 0.42500(17) -0.17984(13) 0.65732(14) 0.0511(5) Uani 1 1 d . . . C6 C 0.2098(7) -0.1458(6) 0.6220(6) 0.0559(18) Uani 1 1 d . . . C1 C 0.1863(8) -0.0729(6) 0.8376(6) 0.066(2) Uani 1 1 d . . . C12 C 0.2465(7) 0.1670(5) 0.6733(6) 0.0583(19) Uani 1 1 d . . . H12A H 0.2626 0.1618 0.6083 0.070 Uiso 1 1 calc R . . H12B H 0.1876 0.2078 0.6833 0.070 Uiso 1 1 calc R . . C11 C 0.4358(6) 0.1635(5) 0.7043(6) 0.0525(17) Uani 1 1 d . . . H11A H 0.4985 0.2038 0.7321 0.063 Uiso 1 1 calc R . . H11B H 0.4417 0.1563 0.6377 0.063 Uiso 1 1 calc R . . C2 C 0.3825(9) -0.0518(7) 0.8869(6) 0.070(2) Uani 1 1 d . . . C29 C 0.9418(6) 0.2945(5) 0.7129(6) 0.0513(16) Uani 1 1 d . . . H29A H 0.9547 0.2929 0.6476 0.062 Uiso 1 1 calc R . . H29B H 1.0064 0.2758 0.7422 0.062 Uiso 1 1 calc R . . C19 C 0.8390(8) 0.4447(6) 0.5625(6) 0.063(2) Uani 1 1 d . . . O6 O 0.8628(9) 0.4241(7) 0.4881(5) 0.105(3) Uani 1 1 d . . . C28 C 0.7605(6) 0.2367(5) 0.6641(5) 0.0508(16) Uani 1 1 d . . . H28A H 0.7089 0.1815 0.6625 0.061 Uiso 1 1 calc R . . H28B H 0.7831 0.2385 0.6014 0.061 Uiso 1 1 calc R . . P4 P 0.7584(2) 0.32337(17) 0.93215(15) 0.0623(6) Uani 1 1 d . . . P3 P 0.88500(18) 0.62037(13) 0.70071(15) 0.0543(5) Uani 1 1 d . . . P1 P 0.26568(17) 0.11889(15) 0.93491(14) 0.0545(5) Uani 1 1 d . . . S1 S 0.20069(14) 0.04709(13) 0.69894(13) 0.0476(4) Uani 1 1 d . . . Fe3 Fe 0.79648(8) 0.47592(7) 0.67633(7) 0.0459(3) Uani 1 1 d . . . Fe4 Fe 0.76648(9) 0.43055(7) 0.83611(7) 0.0491(3) Uani 1 1 d . . . N1 N 0.3401(5) 0.2123(4) 0.7279(4) 0.0507(14) Uani 1 1 d . . . O3 O 0.1372(6) -0.2011(5) 0.6005(6) 0.086(2) Uani 1 1 d . . . S3 S 0.92261(14) 0.41755(13) 0.76254(14) 0.0503(4) Uani 1 1 d . . . S4 S 0.69195(14) 0.34525(12) 0.70208(12) 0.0459(4) Uani 1 1 d . . . N2 N 0.8538(5) 0.2243(4) 0.7218(4) 0.0466(13) Uani 1 1 d . . . O2 O 0.4388(8) -0.0900(7) 0.9312(6) 0.107(3) Uani 1 1 d . . . C7 C 0.3552(6) -0.0361(6) 0.5400(5) 0.0548(18) Uani 1 1 d . . . C22 C 1.0272(8) 0.6311(7) 0.7341(8) 0.079(3) Uani 1 1 d . . . H22A H 1.0542 0.6971 0.7420 0.118 Uiso 1 1 calc R . . H22B H 1.0657 0.5954 0.6868 0.118 Uiso 1 1 calc R . . H22C H 1.0373 0.6065 0.7914 0.118 Uiso 1 1 calc R . . C17 C 0.2718(10) 0.3757(7) 0.7725(8) 0.082(3) Uani 1 1 d . . . H17A H 0.2015 0.3400 0.7657 0.098 Uiso 1 1 calc R . . H17B H 0.2906 0.3946 0.8379 0.098 Uiso 1 1 calc R . . C5 C 0.1410(9) 0.1766(9) 0.9208(8) 0.087(3) Uani 1 1 d . . . H5A H 0.1345 0.2247 0.9733 0.130 Uiso 1 1 calc R . . H5B H 0.0803 0.1298 0.9165 0.130 Uiso 1 1 calc R . . H5C H 0.1427 0.2055 0.8654 0.130 Uiso 1 1 calc R . . O5 O 0.6045(7) 0.5709(7) 0.6376(8) 0.111(3) Uani 1 1 d . . . C30 C 0.8911(7) 0.1260(5) 0.7048(6) 0.0534(17) Uani 1 1 d . . . H30A H 0.9590 0.1283 0.7416 0.064 Uiso 1 1 calc R . . C33 C 0.9057(9) -0.0226(7) 0.6037(8) 0.083(3) Uani 1 1 d . . . H33A H 0.8563 -0.0532 0.5535 0.099 Uiso 1 1 calc R . . H33B H 0.9756 -0.0476 0.5948 0.099 Uiso 1 1 calc R . . C18 C 0.6807(7) 0.5323(6) 0.6538(8) 0.068(2) Uani 1 1 d . . . O1 O 0.1132(9) -0.1247(7) 0.8499(7) 0.119(3) Uani 1 1 d . . . C34 C 0.9157(8) 0.0856(6) 0.6048(7) 0.067(2) Uani 1 1 d . . . H34A H 0.8640 0.1040 0.5608 0.080 Uiso 1 1 calc R . . H34B H 0.9880 0.1079 0.5900 0.080 Uiso 1 1 calc R . . C13 C 0.3576(7) 0.3159(5) 0.7253(6) 0.0603(19) Uani 1 1 d . . . H13A H 0.4257 0.3373 0.7608 0.072 Uiso 1 1 calc R . . C27 C 0.6649(9) 0.2171(9) 0.8994(8) 0.089(3) Uani 1 1 d . . . H27A H 0.6686 0.1763 0.9462 0.133 Uiso 1 1 calc R . . H27B H 0.6843 0.1834 0.8413 0.133 Uiso 1 1 calc R . . H27C H 0.5927 0.2358 0.8936 0.133 Uiso 1 1 calc R . . C31 C 0.8149(8) 0.0490(6) 0.7371(8) 0.070(2) Uani 1 1 d . . . H31A H 0.8156 0.0555 0.8041 0.084 Uiso 1 1 calc R . . H31B H 0.7415 0.0508 0.7131 0.084 Uiso 1 1 calc R . . C21 C 0.8846(9) 0.6811(7) 0.5995(8) 0.078(3) Uani 1 1 d . . . H21A H 0.9239 0.7427 0.6144 0.117 Uiso 1 1 calc R . . H21B H 0.8114 0.6889 0.5806 0.117 Uiso 1 1 calc R . . H21C H 0.9182 0.6438 0.5499 0.117 Uiso 1 1 calc R . . O8 O 0.5610(8) 0.5105(8) 0.8726(7) 0.128(4) Uani 1 1 d . . . C26 C 0.8834(10) 0.2737(10) 0.9591(8) 0.089(3) Uani 1 1 d . . . H26A H 0.8702 0.2284 1.0011 0.133 Uiso 1 1 calc R . . H26B H 0.9353 0.3240 0.9872 0.133 Uiso 1 1 calc R . . H26C H 0.9110 0.2422 0.9031 0.133 Uiso 1 1 calc R . . C14 C 0.3707(10) 0.3485(7) 0.6305(8) 0.078(3) Uani 1 1 d . . . H14A H 0.4463 0.3536 0.6157 0.093 Uiso 1 1 calc R . . H14B H 0.3310 0.3036 0.5824 0.093 Uiso 1 1 calc R . . C24 C 0.6416(9) 0.4774(9) 0.8586(8) 0.085(3) Uani 1 1 d . . . C32 C 0.8636(11) -0.0419(7) 0.6956(10) 0.093(4) Uani 1 1 d . . . H32A H 0.9219 -0.0562 0.7359 0.112 Uiso 1 1 calc R . . H32B H 0.8091 -0.0956 0.6867 0.112 Uiso 1 1 calc R . . C23 C 0.8323(9) 0.5192(7) 0.9204(7) 0.073(2) Uani 1 1 d . . . C4 C 0.3657(9) 0.2199(7) 0.9685(7) 0.073(2) Uani 1 1 d . . . H4A H 0.3401 0.2622 1.0189 0.110 Uiso 1 1 calc R . . H4B H 0.3772 0.2536 0.9167 0.110 Uiso 1 1 calc R . . H4C H 0.4325 0.1972 0.9875 0.110 Uiso 1 1 calc R . . O4 O 0.3755(6) -0.0217(6) 0.4665(4) 0.083(2) Uani 1 1 d . . . O7 O 0.8747(9) 0.5748(6) 0.9760(7) 0.119(3) Uani 1 1 d . . . C10 C 0.3798(12) -0.2700(7) 0.7265(9) 0.098(4) Uani 1 1 d . . . H10A H 0.4305 -0.3179 0.7237 0.148 Uiso 1 1 calc R . . H10B H 0.3101 -0.2990 0.7029 0.148 Uiso 1 1 calc R . . H10C H 0.3748 -0.2409 0.7896 0.148 Uiso 1 1 calc R . . C3 C 0.2483(11) 0.0733(8) 1.0446(6) 0.085(3) Uani 1 1 d . . . H3A H 0.2357 0.1249 1.0921 0.127 Uiso 1 1 calc R . . H3B H 0.3125 0.0448 1.0610 0.127 Uiso 1 1 calc R . . H3C H 0.1877 0.0262 1.0382 0.127 Uiso 1 1 calc R . . C9 C 0.4321(13) -0.2546(9) 0.5474(7) 0.106(5) Uani 1 1 d . . . H9A H 0.4779 -0.3048 0.5543 0.159 Uiso 1 1 calc R . . H9B H 0.4614 -0.2170 0.5031 0.159 Uiso 1 1 calc R . . H9C H 0.3610 -0.2819 0.5261 0.159 Uiso 1 1 calc R . . C20 C 0.8335(12) 0.7071(7) 0.7889(9) 0.098(4) Uani 1 1 d . . . H20A H 0.8773 0.7666 0.7938 0.147 Uiso 1 1 calc R . . H20B H 0.8358 0.6839 0.8474 0.147 Uiso 1 1 calc R . . H20C H 0.7603 0.7168 0.7722 0.147 Uiso 1 1 calc R . . C8 C 0.5641(9) -0.1524(9) 0.6962(11) 0.103(4) Uani 1 1 d . . . H8A H 0.5989 -0.2106 0.6951 0.154 Uiso 1 1 calc R . . H8B H 0.5680 -0.1185 0.7583 0.154 Uiso 1 1 calc R . . H8C H 0.5999 -0.1133 0.6560 0.154 Uiso 1 1 calc R . . C15 C 0.3261(16) 0.4440(10) 0.6382(11) 0.126(6) Uani 1 1 d . . . H15A H 0.3842 0.4935 0.6371 0.151 Uiso 1 1 calc R . . H15B H 0.2758 0.4455 0.5863 0.151 Uiso 1 1 calc R . . C16 C 0.2717(18) 0.4609(10) 0.7237(12) 0.146(7) Uani 1 1 d . . . H16A H 0.1978 0.4745 0.7109 0.175 Uiso 1 1 calc R . . H16B H 0.3077 0.5160 0.7630 0.175 Uiso 1 1 calc R . . C25 C 0.7172(15) 0.3713(11) 1.0461(8) 0.120(5) Uani 1 1 d . . . H25A H 0.7151 0.3222 1.0849 0.180 Uiso 1 1 calc R . . H25B H 0.6468 0.3940 1.0410 0.180 Uiso 1 1 calc R . . H25C H 0.7680 0.4232 1.0728 0.180 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 0.0602(6) 0.0433(6) 0.0378(5) 0.0038(4) 0.0080(4) 0.0092(4) Fe2 0.0478(5) 0.0374(5) 0.0368(5) 0.0017(4) 0.0043(4) 0.0035(4) S2 0.0488(9) 0.0400(8) 0.0468(9) 0.0020(7) -0.0002(7) 0.0051(7) P2 0.0642(11) 0.0423(9) 0.0480(10) 0.0052(8) 0.0090(8) 0.0117(8) C6 0.060(4) 0.047(4) 0.061(5) 0.010(3) 0.009(4) 0.004(3) C1 0.090(6) 0.058(5) 0.050(4) 0.010(4) 0.012(4) -0.011(4) C12 0.062(4) 0.042(4) 0.073(5) 0.013(4) -0.003(4) 0.008(3) C11 0.055(4) 0.040(3) 0.063(4) 0.011(3) 0.005(3) -0.004(3) C2 0.088(6) 0.076(6) 0.055(5) 0.018(4) 0.020(4) 0.032(5) C29 0.051(4) 0.044(4) 0.061(4) 0.013(3) 0.010(3) 0.010(3) C19 0.082(6) 0.054(4) 0.053(5) 0.005(4) 0.008(4) 0.014(4) O6 0.159(8) 0.100(6) 0.058(4) -0.001(4) 0.032(5) 0.027(6) C28 0.062(4) 0.045(4) 0.045(4) 0.001(3) 0.000(3) 0.009(3) P4 0.0767(14) 0.0626(13) 0.0483(11) 0.0108(9) 0.0095(9) 0.0026(10) P3 0.0700(12) 0.0366(9) 0.0568(11) 0.0062(8) 0.0117(9) 0.0048(8) P1 0.0626(11) 0.0554(11) 0.0443(10) -0.0040(8) 0.0085(8) 0.0148(9) S1 0.0443(9) 0.0452(9) 0.0530(10) 0.0049(7) 0.0040(7) 0.0058(7) Fe3 0.0519(6) 0.0376(5) 0.0494(6) 0.0075(4) 0.0067(4) 0.0083(4) Fe4 0.0591(6) 0.0416(6) 0.0451(6) 0.0006(4) 0.0046(4) 0.0053(4) N1 0.061(4) 0.035(3) 0.055(3) -0.001(2) -0.001(3) 0.004(2) O3 0.081(4) 0.060(4) 0.108(6) -0.001(4) -0.001(4) -0.023(3) S3 0.0479(9) 0.0415(9) 0.0616(11) 0.0101(8) -0.0011(8) 0.0022(7) S4 0.0452(9) 0.0415(8) 0.0496(9) 0.0027(7) 0.0014(7) 0.0027(6) N2 0.057(3) 0.036(3) 0.048(3) 0.006(2) 0.004(3) 0.009(2) O2 0.144(8) 0.113(7) 0.077(5) 0.036(5) 0.004(5) 0.056(6) C7 0.055(4) 0.059(4) 0.046(4) -0.001(3) 0.000(3) -0.004(3) C22 0.076(6) 0.059(5) 0.102(8) 0.025(5) -0.007(5) -0.012(4) C17 0.099(7) 0.051(5) 0.094(7) -0.001(5) 0.034(6) 0.018(5) C5 0.076(6) 0.102(8) 0.079(7) -0.013(6) 0.002(5) 0.033(6) O5 0.080(5) 0.105(6) 0.160(9) 0.048(6) -0.003(5) 0.041(5) C30 0.063(4) 0.043(4) 0.055(4) 0.003(3) 0.002(3) 0.018(3) C33 0.089(7) 0.056(5) 0.095(8) -0.020(5) -0.006(6) 0.015(5) C18 0.060(5) 0.054(5) 0.093(7) 0.012(4) 0.005(4) 0.015(4) O1 0.137(8) 0.109(7) 0.107(7) 0.034(5) 0.012(6) -0.051(6) C34 0.081(6) 0.051(4) 0.070(5) 0.007(4) 0.017(4) 0.023(4) C13 0.071(5) 0.039(4) 0.070(5) 0.008(3) 0.005(4) -0.001(3) C27 0.088(7) 0.090(8) 0.091(8) 0.034(6) 0.017(6) -0.014(6) C31 0.088(6) 0.042(4) 0.084(6) 0.014(4) 0.017(5) 0.012(4) C21 0.090(7) 0.065(6) 0.085(7) 0.032(5) 0.017(5) 0.002(5) O8 0.106(7) 0.164(10) 0.112(7) -0.023(7) 0.023(5) 0.068(7) C26 0.091(7) 0.105(9) 0.074(7) 0.027(6) -0.012(6) 0.010(6) C14 0.099(7) 0.051(5) 0.087(7) 0.019(5) 0.027(6) 0.012(5) C24 0.086(7) 0.090(7) 0.075(6) -0.008(5) 0.010(5) 0.024(6) C32 0.108(9) 0.046(5) 0.131(11) 0.024(6) 0.015(8) 0.014(5) C23 0.098(7) 0.056(5) 0.058(5) -0.002(4) 0.006(5) -0.004(5) C4 0.091(7) 0.059(5) 0.066(5) -0.006(4) -0.005(5) 0.012(5) O4 0.091(5) 0.108(6) 0.051(4) 0.023(3) 0.007(3) -0.017(4) O7 0.166(9) 0.081(5) 0.092(6) -0.025(5) -0.025(6) -0.030(5) C10 0.151(11) 0.052(5) 0.107(9) 0.035(5) 0.051(8) 0.038(6) C3 0.127(9) 0.082(7) 0.046(5) 0.001(4) 0.024(5) 0.019(6) C9 0.163(12) 0.107(9) 0.048(5) -0.015(5) 0.003(6) 0.068(9) C20 0.142(11) 0.048(5) 0.105(9) 0.003(5) 0.046(8) 0.015(6) C8 0.079(7) 0.074(7) 0.157(13) 0.018(7) -0.016(8) 0.026(6) C15 0.203(17) 0.077(8) 0.113(11) 0.040(8) 0.033(11) 0.056(10) C16 0.24(2) 0.091(9) 0.131(12) 0.043(9) 0.073(13) 0.099(12) C25 0.190(16) 0.107(10) 0.062(6) -0.005(6) 0.037(8) 0.025(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 1.729(9) . ? Fe1 C2 1.747(9) . ? Fe1 P1 2.224(2) . ? Fe1 S2 2.260(2) . ? Fe1 S1 2.270(2) . ? Fe1 Fe2 2.5279(13) . ? Fe2 C6 1.770(8) . ? Fe2 C7 1.773(8) . ? Fe2 P2 2.229(2) . ? Fe2 S2 2.2560(19) . ? Fe2 S1 2.262(2) . ? S2 C11 1.826(7) . ? P2 C8 1.797(11) . ? P2 C9 1.801(9) . ? P2 C10 1.810(10) . ? C6 O3 1.153(10) . ? C1 O1 1.160(12) . ? C12 N1 1.440(10) . ? C12 S1 1.846(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C11 N1 1.449(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C2 O2 1.156(12) . ? C29 N2 1.443(9) . ? C29 S3 1.829(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C19 O6 1.138(11) . ? C19 Fe3 1.767(9) . ? C28 N2 1.448(9) . ? C28 S4 1.843(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? P4 C26 1.809(11) . ? P4 C25 1.810(12) . ? P4 C27 1.826(11) . ? P4 Fe4 2.213(2) . ? P3 C22 1.806(10) . ? P3 C21 1.816(10) . ? P3 C20 1.818(11) . ? P3 Fe3 2.226(2) . ? P1 C4 1.822(10) . ? P1 C3 1.825(10) . ? P1 C5 1.827(10) . ? Fe3 C18 1.744(9) . ? Fe3 S3 2.258(2) . ? Fe3 S4 2.265(2) . ? Fe3 Fe4 2.5403(14) . ? Fe4 C24 1.757(11) . ? Fe4 C23 1.758(9) . ? Fe4 S3 2.256(2) . ? Fe4 S4 2.274(2) . ? N1 C13 1.477(9) . ? N2 C30 1.495(9) . ? C7 O4 1.154(10) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C17 C16 1.491(16) . ? C17 C13 1.533(13) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? O5 C18 1.164(11) . ? C30 C31 1.527(12) . ? C30 C34 1.538(12) . ? C30 H30A 0.9800 . ? C33 C32 1.509(17) . ? C33 C34 1.529(13) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C13 C14 1.532(13) . ? C13 H13A 0.9800 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C31 C32 1.523(13) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? O8 C24 1.151(13) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C14 C15 1.495(15) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C23 O7 1.132(12) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C15 C16 1.44(2) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C2 92.0(5) . . ? C1 Fe1 P1 96.3(3) . . ? C2 Fe1 P1 94.4(3) . . ? C1 Fe1 S2 152.0(3) . . ? C2 Fe1 S2 87.6(3) . . ? P1 Fe1 S2 111.70(9) . . ? C1 Fe1 S1 89.0(3) . . ? C2 Fe1 S1 163.2(3) . . ? P1 Fe1 S1 102.20(8) . . ? S2 Fe1 S1 83.72(7) . . ? C1 Fe1 Fe2 97.9(3) . . ? C2 Fe1 Fe2 107.3(3) . . ? P1 Fe1 Fe2 153.52(8) . . ? S2 Fe1 Fe2 55.88(5) . . ? S1 Fe1 Fe2 55.96(5) . . ? C6 Fe2 C7 100.0(4) . . ? C6 Fe2 P2 88.0(3) . . ? C7 Fe2 P2 96.7(3) . . ? C6 Fe2 S2 159.5(3) . . ? C7 Fe2 S2 100.3(2) . . ? P2 Fe2 S2 92.78(8) . . ? C6 Fe2 S1 87.8(3) . . ? C7 Fe2 S1 104.9(3) . . ? P2 Fe2 S1 158.37(8) . . ? S2 Fe2 S1 83.99(7) . . ? C6 Fe2 Fe1 104.0(3) . . ? C7 Fe2 Fe1 148.3(3) . . ? P2 Fe2 Fe1 104.48(7) . . ? S2 Fe2 Fe1 56.04(6) . . ? S1 Fe2 Fe1 56.25(6) . . ? C11 S2 Fe2 109.5(3) . . ? C11 S2 Fe1 112.9(3) . . ? Fe2 S2 Fe1 68.08(6) . . ? C8 P2 C9 103.6(7) . . ? C8 P2 C10 102.6(7) . . ? C9 P2 C10 99.3(6) . . ? C8 P2 Fe2 118.5(4) . . ? C9 P2 Fe2 113.5(4) . . ? C10 P2 Fe2 116.7(4) . . ? O3 C6 Fe2 178.4(8) . . ? O1 C1 Fe1 179.7(10) . . ? N1 C12 S1 114.8(5) . . ? N1 C12 H12A 108.6 . . ? S1 C12 H12A 108.6 . . ? N1 C12 H12B 108.6 . . ? S1 C12 H12B 108.6 . . ? H12A C12 H12B 107.5 . . ? N1 C11 S2 115.9(5) . . ? N1 C11 H11A 108.3 . . ? S2 C11 H11A 108.3 . . ? N1 C11 H11B 108.3 . . ? S2 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? O2 C2 Fe1 179.0(11) . . ? N2 C29 S3 116.0(5) . . ? N2 C29 H29A 108.3 . . ? S3 C29 H29A 108.3 . . ? N2 C29 H29B 108.3 . . ? S3 C29 H29B 108.3 . . ? H29A C29 H29B 107.4 . . ? O6 C19 Fe3 177.7(10) . . ? N2 C28 S4 114.6(5) . . ? N2 C28 H28A 108.6 . . ? S4 C28 H28A 108.6 . . ? N2 C28 H28B 108.6 . . ? S4 C28 H28B 108.6 . . ? H28A C28 H28B 107.6 . . ? C26 P4 C25 102.0(7) . . ? C26 P4 C27 102.8(6) . . ? C25 P4 C27 103.3(7) . . ? C26 P4 Fe4 116.8(4) . . ? C25 P4 Fe4 112.8(5) . . ? C27 P4 Fe4 117.2(4) . . ? C22 P3 C21 101.6(5) . . ? C22 P3 C20 101.5(6) . . ? C21 P3 C20 102.7(5) . . ? C22 P3 Fe3 118.9(3) . . ? C21 P3 Fe3 113.5(4) . . ? C20 P3 Fe3 116.3(4) . . ? C4 P1 C3 101.7(5) . . ? C4 P1 C5 102.8(5) . . ? C3 P1 C5 102.4(6) . . ? C4 P1 Fe1 120.4(3) . . ? C3 P1 Fe1 112.3(3) . . ? C5 P1 Fe1 114.9(4) . . ? C12 S1 Fe2 110.8(3) . . ? C12 S1 Fe1 113.0(3) . . ? Fe2 S1 Fe1 67.80(6) . . ? C18 Fe3 C19 100.3(5) . . ? C18 Fe3 P3 87.2(3) . . ? C19 Fe3 P3 95.7(3) . . ? C18 Fe3 S3 157.2(4) . . ? C19 Fe3 S3 102.5(3) . . ? P3 Fe3 S3 91.18(8) . . ? C18 Fe3 S4 89.9(3) . . ? C19 Fe3 S4 103.9(3) . . ? P3 Fe3 S4 160.36(9) . . ? S3 Fe3 S4 83.98(7) . . ? C18 Fe3 Fe4 102.9(4) . . ? C19 Fe3 Fe4 148.9(3) . . ? P3 Fe3 Fe4 105.67(7) . . ? S3 Fe3 Fe4 55.70(6) . . ? S4 Fe3 Fe4 56.15(6) . . ? C24 Fe4 C23 90.8(5) . . ? C24 Fe4 P4 98.3(4) . . ? C23 Fe4 P4 92.7(3) . . ? C24 Fe4 S3 154.3(4) . . ? C23 Fe4 S3 89.5(4) . . ? P4 Fe4 S3 107.31(9) . . ? C24 Fe4 S4 89.4(4) . . ? C23 Fe4 S4 164.8(3) . . ? P4 Fe4 S4 102.35(9) . . ? S3 Fe4 S4 83.82(7) . . ? C24 Fe4 Fe3 100.2(4) . . ? C23 Fe4 Fe3 109.3(3) . . ? P4 Fe4 Fe3 150.88(8) . . ? S3 Fe4 Fe3 55.80(6) . . ? S4 Fe4 Fe3 55.79(6) . . ? C12 N1 C11 111.4(6) . . ? C12 N1 C13 113.7(6) . . ? C11 N1 C13 111.9(6) . . ? C29 S3 Fe4 112.7(2) . . ? C29 S3 Fe3 109.8(3) . . ? Fe4 S3 Fe3 68.50(6) . . ? C28 S4 Fe3 109.8(3) . . ? C28 S4 Fe4 113.0(2) . . ? Fe3 S4 Fe4 68.07(6) . . ? C29 N2 C28 111.2(6) . . ? C29 N2 C30 110.3(6) . . ? C28 N2 C30 113.6(6) . . ? O4 C7 Fe2 178.6(7) . . ? P3 C22 H22A 109.5 . . ? P3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C16 C17 C13 104.7(9) . . ? C16 C17 H17A 110.8 . . ? C13 C17 H17A 110.8 . . ? C16 C17 H17B 110.8 . . ? C13 C17 H17B 110.8 . . ? H17A C17 H17B 108.9 . . ? P1 C5 H5A 109.5 . . ? P1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C30 C31 114.5(7) . . ? N2 C30 C34 117.7(6) . . ? C31 C30 C34 105.1(7) . . ? N2 C30 H30A 106.3 . . ? C31 C30 H30A 106.3 . . ? C34 C30 H30A 106.3 . . ? C32 C33 C34 107.8(8) . . ? C32 C33 H33A 110.2 . . ? C34 C33 H33A 110.2 . . ? C32 C33 H33B 110.2 . . ? C34 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? O5 C18 Fe3 178.7(10) . . ? C33 C34 C30 103.9(8) . . ? C33 C34 H34A 111.0 . . ? C30 C34 H34A 111.0 . . ? C33 C34 H34B 111.0 . . ? C30 C34 H34B 111.0 . . ? H34A C34 H34B 109.0 . . ? N1 C13 C14 117.7(7) . . ? N1 C13 C17 114.8(7) . . ? C14 C13 C17 105.7(8) . . ? N1 C13 H13A 105.9 . . ? C14 C13 H13A 105.9 . . ? C17 C13 H13A 105.9 . . ? P4 C27 H27A 109.5 . . ? P4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? P4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C32 C31 C30 101.7(8) . . ? C32 C31 H31A 111.4 . . ? C30 C31 H31A 111.4 . . ? C32 C31 H31B 111.4 . . ? C30 C31 H31B 111.4 . . ? H31A C31 H31B 109.3 . . ? P3 C21 H21A 109.5 . . ? P3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P4 C26 H26A 109.5 . . ? P4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? P4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C15 C14 C13 105.8(9) . . ? C15 C14 H14A 110.6 . . ? C13 C14 H14A 110.6 . . ? C15 C14 H14B 110.6 . . ? C13 C14 H14B 110.6 . . ? H14A C14 H14B 108.7 . . ? O8 C24 Fe4 178.1(13) . . ? C33 C32 C31 105.8(8) . . ? C33 C32 H32A 110.6 . . ? C31 C32 H32A 110.6 . . ? C33 C32 H32B 110.6 . . ? C31 C32 H32B 110.6 . . ? H32A C32 H32B 108.7 . . ? O7 C23 Fe4 178.5(10) . . ? P1 C4 H4A 109.5 . . ? P1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P2 C10 H10A 109.5 . . ? P2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P2 C9 H9A 109.5 . . ? P2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P3 C20 H20A 109.5 . . ? P3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? P3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P2 C8 H8A 109.5 . . ? P2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C16 C15 C14 109.0(10) . . ? C16 C15 H15A 109.9 . . ? C14 C15 H15A 109.9 . . ? C16 C15 H15B 109.9 . . ? C14 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? C15 C16 C17 110.3(10) . . ? C15 C16 H16A 109.6 . . ? C17 C16 H16A 109.6 . . ? C15 C16 H16B 109.6 . . ? C17 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? P4 C25 H25A 109.5 . . ? P4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? P4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.958 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.146 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; # Attachment '5 for B616236C.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 622707' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H66 Fe4 N2 O8 P4 S4' _chemical_formula_weight 1130.43 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.819(5) _cell_length_b 10.912(2) _cell_length_c 23.588(5) _cell_angle_alpha 90.00 _cell_angle_beta 118.581(2) _cell_angle_gamma 90.00 _cell_volume 5158.0(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7091 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour gray _exptl_crystal_size_max .25 _exptl_crystal_size_mid .12 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 1.433 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .8652 _exptl_absorpt_correction_T_max 1.0000 _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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 37776 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11755 _reflns_number_gt 9040 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+5.0231P] 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 11755 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0806 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1064 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _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 0.37078(3) 1.24167(5) 0.28246(2) 0.04021(13) Uani 1 1 d . . . Fe2 Fe 0.31001(2) 1.06166(5) 0.30820(2) 0.03813(12) Uani 1 1 d . . . Fe3 Fe 0.11484(2) 0.47723(5) 0.45132(2) 0.03756(12) Uani 1 1 d . . . Fe4 Fe 0.20863(2) 0.57666(5) 0.43488(2) 0.03662(12) Uani 1 1 d . . . S1 S 0.27805(5) 1.14269(8) 0.21081(4) 0.0423(2) Uani 1 1 d . . . S2 S 0.31683(4) 1.25806(8) 0.34037(4) 0.0392(2) Uani 1 1 d . . . S3 S 0.16470(4) 0.38937(8) 0.39961(4) 0.0393(2) Uani 1 1 d . . . S4 S 0.21953(4) 0.51121(8) 0.53006(4) 0.0388(2) Uani 1 1 d . . . P2 P 0.31167(5) 0.88014(9) 0.26529(5) 0.0452(2) Uani 1 1 d . . . P4 P 0.21564(5) 0.77075(9) 0.46592(5) 0.0451(2) Uani 1 1 d . . . P3 P 0.01775(5) 0.47729(10) 0.36067(5) 0.0466(2) Uani 1 1 d . . . P1 P 0.46277(5) 1.30852(10) 0.36810(5) 0.0482(2) Uani 1 1 d . . . N1 N 0.21707(14) 1.3514(3) 0.22411(13) 0.0407(7) Uani 1 1 d . . . N2 N 0.28227(14) 0.3178(3) 0.50526(13) 0.0413(7) Uani 1 1 d . . . O1 O 0.45364(17) 1.1166(3) 0.23787(17) 0.0799(10) Uani 1 1 d . . . O2 O 0.35076(18) 1.4801(3) 0.21959(16) 0.0790(10) Uani 1 1 d . . . O3 O 0.18536(16) 1.0118(3) 0.30906(17) 0.0798(10) Uani 1 1 d . . . O4 O 0.40860(16) 0.9750(3) 0.43562(14) 0.0780(10) Uani 1 1 d . . . O5 O 0.08327(17) 0.2773(3) 0.51394(17) 0.0845(11) Uani 1 1 d . . . O6 O 0.06431(18) 0.6815(3) 0.49418(19) 0.0899(12) Uani 1 1 d . . . O7 O 0.15306(17) 0.6717(3) 0.30422(14) 0.0763(10) Uani 1 1 d . . . O8 O 0.34603(16) 0.5596(3) 0.45801(18) 0.0794(10) Uani 1 1 d . . . C1 C 0.4200(2) 1.1644(4) 0.2551(2) 0.0526(10) Uani 1 1 d . . . C2 C 0.3579(2) 1.3867(4) 0.24414(19) 0.0517(10) Uani 1 1 d . . . C3 C 0.5349(3) 1.3326(6) 0.3560(3) 0.0987(19) Uani 1 1 d . . . H3A H 0.5717 1.3611 0.3955 0.148 Uiso 1 1 calc R . . H3B H 0.5243 1.3926 0.3227 0.148 Uiso 1 1 calc R . . H3C H 0.5467 1.2568 0.3434 0.148 Uiso 1 1 calc R . . C4 C 0.4991(3) 1.2189(5) 0.4409(2) 0.0963(19) Uani 1 1 d . . . H4A H 0.5382 1.2598 0.4731 0.144 Uiso 1 1 calc R . . H4B H 0.5113 1.1397 0.4322 0.144 Uiso 1 1 calc R . . H4C H 0.4673 1.2094 0.4563 0.144 Uiso 1 1 calc R . . C5 C 0.4543(3) 1.4576(5) 0.3971(3) 0.0937(19) Uani 1 1 d . . . H5A H 0.4958 1.4801 0.4338 0.141 Uiso 1 1 calc R . . H5B H 0.4199 1.4546 0.4094 0.141 Uiso 1 1 calc R . . H5C H 0.4429 1.5173 0.3635 0.141 Uiso 1 1 calc R . . C6 C 0.2351(2) 1.0284(4) 0.30861(18) 0.0492(9) Uani 1 1 d . . . C7 C 0.3707(2) 1.0111(4) 0.38559(19) 0.0492(9) Uani 1 1 d . . . C8 C 0.3341(3) 0.7489(4) 0.3193(2) 0.0756(14) Uani 1 1 d . . . H8A H 0.3333 0.6759 0.2962 0.113 Uiso 1 1 calc R . . H8B H 0.3028 0.7410 0.3354 0.113 Uiso 1 1 calc R . . H8C H 0.3782 0.7605 0.3548 0.113 Uiso 1 1 calc R . . C9 C 0.2305(2) 0.8325(4) 0.2010(2) 0.0683(13) Uani 1 1 d . . . H9A H 0.2345 0.7541 0.1848 0.103 Uiso 1 1 calc R . . H9B H 0.2146 0.8918 0.1668 0.103 Uiso 1 1 calc R . . H9C H 0.1995 0.8267 0.2177 0.103 Uiso 1 1 calc R . . C10 C 0.3631(2) 0.8584(4) 0.2267(2) 0.0657(12) Uani 1 1 d . . . H10A H 0.3581 0.7760 0.2109 0.099 Uiso 1 1 calc R . . H10B H 0.4090 0.8731 0.2575 0.099 Uiso 1 1 calc R . . H10C H 0.3494 0.9147 0.1913 0.099 Uiso 1 1 calc R . . C11 C 0.23657(18) 1.3350(4) 0.29172(17) 0.0470(9) Uani 1 1 d . . . H11A H 0.2021 1.2881 0.2948 0.056 Uiso 1 1 calc R . . H11B H 0.2383 1.4149 0.3105 0.056 Uiso 1 1 calc R . . C12 C 0.20404(18) 1.2369(3) 0.18959(17) 0.0470(9) Uani 1 1 d . . . H12A H 0.1828 1.2543 0.1437 0.056 Uiso 1 1 calc R . . H12B H 0.1728 1.1899 0.1978 0.056 Uiso 1 1 calc R . . C13 C 0.16202(18) 1.4418(3) 0.19304(18) 0.0483(9) Uani 1 1 d . . . H13A H 0.1751 1.5139 0.2212 0.058 Uiso 1 1 calc R . . C14 C 0.09561(19) 1.3982(4) 0.1863(2) 0.0607(11) Uani 1 1 d . . . H14A H 0.1013 1.3763 0.2284 0.073 Uiso 1 1 calc R . . H14B H 0.0813 1.3255 0.1593 0.073 Uiso 1 1 calc R . . C15 C 0.0421(2) 1.4971(5) 0.1564(3) 0.0803(15) Uani 1 1 d . . . H15A H -0.0001 1.4656 0.1508 0.096 Uiso 1 1 calc R . . H15B H 0.0544 1.5671 0.1852 0.096 Uiso 1 1 calc R . . C16 C 0.0343(3) 1.5368(5) 0.0918(2) 0.0855(17) Uani 1 1 d . . . H16A H 0.0012 1.6016 0.0742 0.103 Uiso 1 1 calc R . . H16B H 0.0185 1.4682 0.0621 0.103 Uiso 1 1 calc R . . C17 C 0.0998(3) 1.5824(4) 0.0981(3) 0.0856(17) Uani 1 1 d . . . H17A H 0.1136 1.6555 0.1247 0.103 Uiso 1 1 calc R . . H17B H 0.0938 1.6038 0.0557 0.103 Uiso 1 1 calc R . . C18 C 0.1541(2) 1.4842(4) 0.1285(2) 0.0626(12) Uani 1 1 d . . . H18A H 0.1426 1.4147 0.0995 0.075 Uiso 1 1 calc R . . H18B H 0.1962 1.5172 0.1345 0.075 Uiso 1 1 calc R . . C19 C -0.0543(2) 0.4844(6) 0.3738(3) 0.0907(17) Uani 1 1 d . . . H19A H -0.0943 0.4842 0.3329 0.136 Uiso 1 1 calc R . . H19B H -0.0524 0.5582 0.3967 0.136 Uiso 1 1 calc R . . H19C H -0.0542 0.4147 0.3986 0.136 Uiso 1 1 calc R . . C20 C -0.0012(3) 0.3442(5) 0.3096(3) 0.106(2) Uani 1 1 d . . . H20A H -0.0440 0.3546 0.2722 0.160 Uiso 1 1 calc R . . H20B H -0.0020 0.2729 0.3330 0.160 Uiso 1 1 calc R . . H20C H 0.0323 0.3344 0.2964 0.160 Uiso 1 1 calc R . . C21 C 0.0002(3) 0.6007(5) 0.3034(2) 0.0941(19) Uani 1 1 d . . . H21A H -0.0432 0.5890 0.2670 0.141 Uiso 1 1 calc R . . H21B H 0.0332 0.6010 0.2892 0.141 Uiso 1 1 calc R . . H21C H 0.0014 0.6775 0.3238 0.141 Uiso 1 1 calc R . . C22 C 0.09430(19) 0.3554(4) 0.48740(19) 0.0511(10) Uani 1 1 d . . . C23 C 0.0856(2) 0.6014(4) 0.4783(2) 0.0546(10) Uani 1 1 d . . . C24 C 0.1416(2) 0.8655(4) 0.4235(3) 0.0804(15) Uani 1 1 d . . . H24A H 0.1508 0.9468 0.4412 0.121 Uiso 1 1 calc R . . H24B H 0.1056 0.8309 0.4285 0.121 Uiso 1 1 calc R . . H24C H 0.1292 0.8687 0.3785 0.121 Uiso 1 1 calc R . . C25 C 0.2403(3) 0.8045(4) 0.5496(2) 0.0724(14) Uani 1 1 d . . . H25A H 0.2411 0.8917 0.5554 0.109 Uiso 1 1 calc R . . H25B H 0.2840 0.7715 0.5768 0.109 Uiso 1 1 calc R . . H25C H 0.2089 0.7683 0.5608 0.109 Uiso 1 1 calc R . . C26 C 0.2765(2) 0.8564(4) 0.4532(2) 0.0614(11) Uani 1 1 d . . . H26A H 0.2780 0.9395 0.4672 0.092 Uiso 1 1 calc R . . H26B H 0.2640 0.8555 0.4081 0.092 Uiso 1 1 calc R . . H26C H 0.3197 0.8195 0.4775 0.092 Uiso 1 1 calc R . . C27 C 0.17399(19) 0.6315(4) 0.35556(19) 0.0495(9) Uani 1 1 d . . . C28 C 0.2920(2) 0.5633(4) 0.44962(19) 0.0497(9) Uani 1 1 d . . . C29 C 0.26636(19) 0.3673(3) 0.55314(16) 0.0439(8) Uani 1 1 d . . . H29A H 0.3076 0.3806 0.5928 0.053 Uiso 1 1 calc R . . H29B H 0.2406 0.3070 0.5620 0.053 Uiso 1 1 calc R . . C30 C 0.22387(18) 0.2718(3) 0.44994(17) 0.0432(8) Uani 1 1 d . . . H30A H 0.2010 0.2158 0.4647 0.052 Uiso 1 1 calc R . . H30B H 0.2379 0.2253 0.4235 0.052 Uiso 1 1 calc R . . C31 C 0.33912(18) 0.2311(4) 0.53181(18) 0.0470(9) Uani 1 1 d . . . H31A H 0.3391 0.1906 0.4947 0.056 Uiso 1 1 calc R . . C32 C 0.4047(2) 0.2981(4) 0.5668(3) 0.0720(14) Uani 1 1 d . . . H32A H 0.4063 0.3420 0.6033 0.086 Uiso 1 1 calc R . . H32B H 0.4081 0.3576 0.5380 0.086 Uiso 1 1 calc R . . C33 C 0.4636(2) 0.2085(5) 0.5907(3) 0.0851(16) Uani 1 1 d . . . H33A H 0.4648 0.1716 0.5538 0.102 Uiso 1 1 calc R . . H33B H 0.5050 0.2532 0.6152 0.102 Uiso 1 1 calc R . . C34 C 0.4586(2) 0.1085(4) 0.6325(2) 0.0723(14) Uani 1 1 d . . . H34A H 0.4952 0.0513 0.6448 0.087 Uiso 1 1 calc R . . H34B H 0.4619 0.1443 0.6716 0.087 Uiso 1 1 calc R . . C35 C 0.3937(2) 0.0419(4) 0.5970(2) 0.0698(13) Uani 1 1 d . . . H35A H 0.3903 -0.0193 0.6251 0.084 Uiso 1 1 calc R . . H35B H 0.3922 -0.0002 0.5601 0.084 Uiso 1 1 calc R . . C36 C 0.3346(2) 0.1299(4) 0.5739(2) 0.0537(10) Uani 1 1 d . . . H36A H 0.2934 0.0847 0.5495 0.064 Uiso 1 1 calc R . . H36B H 0.3337 0.1661 0.6110 0.064 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 0.0482(3) 0.0407(3) 0.0379(3) 0.0028(2) 0.0256(2) 0.0039(2) Fe2 0.0407(3) 0.0412(3) 0.0328(3) 0.0044(2) 0.0178(2) 0.0040(2) Fe3 0.0393(3) 0.0384(3) 0.0382(3) -0.0030(2) 0.0211(2) -0.0020(2) Fe4 0.0381(3) 0.0396(3) 0.0328(3) -0.0003(2) 0.0175(2) -0.0019(2) S1 0.0544(5) 0.0423(5) 0.0313(4) 0.0011(4) 0.0214(4) 0.0063(4) S2 0.0420(5) 0.0467(5) 0.0296(4) -0.0003(4) 0.0175(4) 0.0044(4) S3 0.0422(5) 0.0428(5) 0.0327(4) -0.0055(4) 0.0177(4) 0.0001(4) S4 0.0458(5) 0.0397(5) 0.0310(4) -0.0037(3) 0.0184(4) -0.0012(4) P2 0.0442(5) 0.0427(6) 0.0493(6) 0.0010(4) 0.0227(5) 0.0033(4) P4 0.0538(6) 0.0391(5) 0.0463(5) -0.0014(4) 0.0272(5) -0.0042(4) P3 0.0393(5) 0.0488(6) 0.0473(6) -0.0008(4) 0.0171(4) -0.0036(4) P1 0.0446(6) 0.0499(6) 0.0532(6) 0.0001(5) 0.0261(5) -0.0011(5) N1 0.0461(17) 0.0404(17) 0.0325(15) 0.0030(12) 0.0162(13) 0.0069(13) N2 0.0453(17) 0.0437(17) 0.0344(15) 0.0010(13) 0.0186(14) 0.0064(13) O1 0.096(3) 0.078(2) 0.101(3) -0.0020(19) 0.076(2) 0.0128(19) O2 0.117(3) 0.0466(18) 0.084(2) 0.0201(17) 0.056(2) 0.0076(18) O3 0.057(2) 0.106(3) 0.087(2) 0.021(2) 0.0434(19) 0.0008(18) O4 0.073(2) 0.083(2) 0.0484(18) 0.0242(16) 0.0056(16) 0.0032(17) O5 0.092(3) 0.080(2) 0.085(2) 0.0268(19) 0.044(2) -0.0162(19) O6 0.087(3) 0.077(2) 0.131(3) -0.040(2) 0.072(2) -0.0040(19) O7 0.093(2) 0.082(2) 0.0433(17) 0.0159(16) 0.0236(17) 0.0012(18) O8 0.0544(19) 0.086(2) 0.112(3) 0.015(2) 0.051(2) 0.0058(17) C1 0.066(3) 0.050(2) 0.055(2) 0.0035(18) 0.039(2) 0.002(2) C2 0.064(3) 0.053(3) 0.045(2) 0.0010(18) 0.032(2) 0.001(2) C3 0.066(3) 0.141(6) 0.105(4) -0.022(4) 0.054(3) -0.028(3) C4 0.081(4) 0.099(4) 0.069(3) 0.020(3) 0.003(3) -0.019(3) C5 0.072(3) 0.078(4) 0.114(5) -0.046(3) 0.030(3) -0.003(3) C6 0.050(2) 0.054(2) 0.043(2) 0.0083(17) 0.0221(18) 0.0033(19) C7 0.054(2) 0.047(2) 0.046(2) 0.0042(17) 0.0231(19) -0.0009(18) C8 0.098(4) 0.052(3) 0.082(3) 0.012(2) 0.047(3) 0.014(3) C9 0.056(3) 0.065(3) 0.076(3) -0.018(2) 0.025(2) -0.006(2) C10 0.064(3) 0.069(3) 0.076(3) -0.017(2) 0.043(3) -0.005(2) C11 0.045(2) 0.056(2) 0.041(2) 0.0016(17) 0.0213(17) 0.0124(18) C12 0.049(2) 0.047(2) 0.0362(19) 0.0009(16) 0.0131(17) 0.0054(17) C13 0.046(2) 0.041(2) 0.045(2) 0.0036(16) 0.0116(17) 0.0027(17) C14 0.047(2) 0.064(3) 0.066(3) 0.009(2) 0.023(2) 0.004(2) C15 0.053(3) 0.086(4) 0.081(4) -0.003(3) 0.015(3) 0.015(3) C16 0.071(3) 0.070(3) 0.072(3) 0.011(3) -0.001(3) 0.018(3) C17 0.089(4) 0.053(3) 0.075(3) 0.024(2) 0.007(3) 0.008(3) C18 0.071(3) 0.051(3) 0.055(3) 0.017(2) 0.022(2) 0.004(2) C19 0.046(3) 0.140(5) 0.084(4) 0.005(4) 0.029(3) -0.002(3) C20 0.066(3) 0.092(4) 0.112(5) -0.052(4) 0.003(3) -0.009(3) C21 0.068(3) 0.113(5) 0.074(3) 0.040(3) 0.012(3) -0.007(3) C22 0.047(2) 0.058(3) 0.048(2) -0.0002(19) 0.0224(19) -0.0052(19) C23 0.049(2) 0.059(3) 0.064(3) -0.011(2) 0.033(2) -0.0060(19) C24 0.078(3) 0.053(3) 0.114(4) 0.012(3) 0.050(3) 0.014(2) C25 0.126(4) 0.049(3) 0.064(3) -0.013(2) 0.062(3) -0.021(3) C26 0.072(3) 0.052(3) 0.066(3) -0.005(2) 0.037(2) -0.017(2) C27 0.052(2) 0.045(2) 0.048(2) -0.0034(18) 0.0206(19) -0.0050(18) C28 0.048(2) 0.053(2) 0.050(2) 0.0018(18) 0.0252(19) -0.0028(19) C29 0.051(2) 0.045(2) 0.0329(18) -0.0008(15) 0.0177(16) 0.0026(17) C30 0.048(2) 0.042(2) 0.0405(19) -0.0046(15) 0.0214(17) 0.0020(16) C31 0.042(2) 0.053(2) 0.042(2) 0.0003(17) 0.0166(17) 0.0055(17) C32 0.050(3) 0.064(3) 0.088(3) 0.016(3) 0.021(2) 0.000(2) C33 0.043(3) 0.092(4) 0.108(4) 0.019(3) 0.026(3) 0.009(3) C34 0.062(3) 0.070(3) 0.059(3) -0.001(2) 0.008(2) 0.021(2) C35 0.075(3) 0.057(3) 0.069(3) 0.011(2) 0.028(3) 0.018(2) C36 0.053(2) 0.044(2) 0.062(3) 0.0066(19) 0.026(2) 0.0073(18) _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 1.756(4) . ? Fe1 C2 1.776(4) . ? Fe1 P1 2.2276(12) . ? Fe1 S2 2.2410(11) . ? Fe1 S1 2.2536(11) . ? Fe1 Fe2 2.6374(8) . ? Fe2 C6 1.752(4) . ? Fe2 C7 1.771(4) . ? Fe2 P2 2.2329(12) . ? Fe2 S1 2.2334(11) . ? Fe2 S2 2.2540(11) . ? Fe3 C23 1.758(4) . ? Fe3 C22 1.759(4) . ? Fe3 P3 2.2244(11) . ? Fe3 S3 2.2426(10) . ? Fe3 S4 2.2468(11) . ? Fe3 Fe4 2.5887(8) . ? Fe4 C27 1.752(4) . ? Fe4 C28 1.769(4) . ? Fe4 P4 2.2216(12) . ? Fe4 S3 2.2530(11) . ? Fe4 S4 2.2535(11) . ? S1 C12 1.830(4) . ? S2 C11 1.834(4) . ? S3 C30 1.829(4) . ? S4 C29 1.829(4) . ? P2 C10 1.812(4) . ? P2 C8 1.820(4) . ? P2 C9 1.820(4) . ? P4 C25 1.812(4) . ? P4 C26 1.814(4) . ? P4 C24 1.819(5) . ? P3 C20 1.802(5) . ? P3 C21 1.811(5) . ? P3 C19 1.813(5) . ? P1 C4 1.797(5) . ? P1 C5 1.811(5) . ? P1 C3 1.819(5) . ? N1 C12 1.443(4) . ? N1 C11 1.447(4) . ? N1 C13 1.485(4) . ? N2 C30 1.438(4) . ? N2 C29 1.447(4) . ? N2 C31 1.481(4) . ? O1 C1 1.151(4) . ? O2 C2 1.144(5) . ? O3 C6 1.155(5) . ? O4 C7 1.149(4) . ? O5 C22 1.154(5) . ? O6 C23 1.147(5) . ? O7 C27 1.155(4) . ? O8 C28 1.152(4) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C18 1.518(5) . ? C13 C14 1.522(5) . ? C13 H13A 0.9800 . ? C14 C15 1.527(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.511(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.513(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.532(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.507(6) . ? C31 C36 1.520(5) . ? C31 H31A 0.9800 . ? C32 C33 1.536(6) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.512(7) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.496(6) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.527(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C2 102.72(18) . . ? C1 Fe1 P1 90.00(15) . . ? C2 Fe1 P1 91.40(14) . . ? C1 Fe1 S2 153.77(13) . . ? C2 Fe1 S2 103.51(13) . . ? P1 Fe1 S2 88.58(4) . . ? C1 Fe1 S1 91.73(14) . . ? C2 Fe1 S1 100.26(14) . . ? P1 Fe1 S1 167.53(4) . . ? S2 Fe1 S1 84.42(4) . . ? C1 Fe1 Fe2 103.07(13) . . ? C2 Fe1 Fe2 143.48(14) . . ? P1 Fe1 Fe2 113.97(4) . . ? S2 Fe1 Fe2 54.30(3) . . ? S1 Fe1 Fe2 53.64(3) . . ? C6 Fe2 C7 102.37(18) . . ? C6 Fe2 P2 92.69(14) . . ? C7 Fe2 P2 90.95(13) . . ? C6 Fe2 S1 104.37(13) . . ? C7 Fe2 S1 153.26(13) . . ? P2 Fe2 S1 87.31(4) . . ? C6 Fe2 S2 96.05(14) . . ? C7 Fe2 S2 93.15(13) . . ? P2 Fe2 S2 169.32(4) . . ? S1 Fe2 S2 84.59(4) . . ? C6 Fe2 Fe1 141.01(13) . . ? C7 Fe2 Fe1 103.35(13) . . ? P2 Fe2 Fe1 115.57(4) . . ? S1 Fe2 Fe1 54.36(3) . . ? S2 Fe2 Fe1 53.84(3) . . ? C23 Fe3 C22 99.93(19) . . ? C23 Fe3 P3 88.39(14) . . ? C22 Fe3 P3 95.27(13) . . ? C23 Fe3 S3 154.84(14) . . ? C22 Fe3 S3 105.20(14) . . ? P3 Fe3 S3 90.48(4) . . ? C23 Fe3 S4 90.63(14) . . ? C22 Fe3 S4 98.56(13) . . ? P3 Fe3 S4 166.09(4) . . ? S3 Fe3 S4 84.54(4) . . ? C23 Fe3 Fe4 102.41(13) . . ? C22 Fe3 Fe4 145.10(13) . . ? P3 Fe3 Fe4 111.74(4) . . ? S3 Fe3 Fe4 55.03(3) . . ? S4 Fe3 Fe4 55.00(3) . . ? C27 Fe4 C28 97.54(18) . . ? C27 Fe4 P4 87.18(13) . . ? C28 Fe4 P4 96.47(13) . . ? C27 Fe4 S3 91.24(13) . . ? C28 Fe4 S3 104.15(13) . . ? P4 Fe4 S3 159.34(4) . . ? C27 Fe4 S4 161.94(14) . . ? C28 Fe4 S4 100.51(13) . . ? P4 Fe4 S4 91.01(4) . . ? S3 Fe4 S4 84.14(4) . . ? C27 Fe4 Fe3 108.68(13) . . ? C28 Fe4 Fe3 145.54(13) . . ? P4 Fe4 Fe3 106.54(3) . . ? S3 Fe4 Fe3 54.65(3) . . ? S4 Fe4 Fe3 54.76(3) . . ? C12 S1 Fe2 107.96(13) . . ? C12 S1 Fe1 110.38(12) . . ? Fe2 S1 Fe1 72.00(3) . . ? C11 S2 Fe1 109.30(12) . . ? C11 S2 Fe2 109.70(13) . . ? Fe1 S2 Fe2 71.85(3) . . ? C30 S3 Fe3 110.85(12) . . ? C30 S3 Fe4 109.69(12) . . ? Fe3 S3 Fe4 70.32(3) . . ? C29 S4 Fe3 110.06(12) . . ? C29 S4 Fe4 109.81(12) . . ? Fe3 S4 Fe4 70.23(3) . . ? C10 P2 C8 102.4(2) . . ? C10 P2 C9 101.0(2) . . ? C8 P2 C9 101.1(2) . . ? C10 P2 Fe2 119.93(15) . . ? C8 P2 Fe2 116.17(17) . . ? C9 P2 Fe2 113.54(15) . . ? C25 P4 C26 102.2(2) . . ? C25 P4 C24 101.9(3) . . ? C26 P4 C24 101.5(2) . . ? C25 P4 Fe4 119.26(15) . . ? C26 P4 Fe4 112.15(15) . . ? C24 P4 Fe4 117.34(17) . . ? C20 P3 C21 101.8(3) . . ? C20 P3 C19 101.6(3) . . ? C21 P3 C19 101.5(3) . . ? C20 P3 Fe3 116.90(18) . . ? C21 P3 Fe3 118.69(17) . . ? C19 P3 Fe3 113.79(18) . . ? C4 P1 C5 102.2(3) . . ? C4 P1 C3 100.9(3) . . ? C5 P1 C3 101.4(3) . . ? C4 P1 Fe1 119.50(18) . . ? C5 P1 Fe1 114.37(17) . . ? C3 P1 Fe1 115.83(19) . . ? C12 N1 C11 112.7(3) . . ? C12 N1 C13 113.5(3) . . ? C11 N1 C13 111.6(3) . . ? C30 N2 C29 111.7(3) . . ? C30 N2 C31 113.9(3) . . ? C29 N2 C31 113.9(3) . . ? O1 C1 Fe1 177.9(4) . . ? O2 C2 Fe1 178.7(4) . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P1 C4 H4A 109.5 . . ? P1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P1 C5 H5A 109.5 . . ? P1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 Fe2 177.1(4) . . ? O4 C7 Fe2 177.6(4) . . ? P2 C8 H8A 109.5 . . ? P2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P2 C9 H9A 109.5 . . ? P2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P2 C10 H10A 109.5 . . ? P2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 S2 115.8(2) . . ? N1 C11 H11A 108.3 . . ? S2 C11 H11A 108.3 . . ? N1 C11 H11B 108.3 . . ? S2 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? N1 C12 S1 114.7(2) . . ? N1 C12 H12A 108.6 . . ? S1 C12 H12A 108.6 . . ? N1 C12 H12B 108.6 . . ? S1 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? N1 C13 C18 111.4(3) . . ? N1 C13 C14 114.1(3) . . ? C18 C13 C14 110.8(3) . . ? N1 C13 H13A 106.7 . . ? C18 C13 H13A 106.7 . . ? C14 C13 H13A 106.7 . . ? C13 C14 C15 111.4(4) . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C14 110.5(4) . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15B 109.6 . . ? C14 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C15 C16 C17 111.2(4) . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C16 C17 C18 110.8(4) . . ? C16 C17 H17A 109.5 . . ? C18 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? C13 C18 C17 111.4(4) . . ? C13 C18 H18A 109.4 . . ? C17 C18 H18A 109.4 . . ? C13 C18 H18B 109.4 . . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? P3 C19 H19A 109.5 . . ? P3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? P3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? P3 C20 H20A 109.5 . . ? P3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? P3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P3 C21 H21A 109.5 . . ? P3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O5 C22 Fe3 176.7(4) . . ? O6 C23 Fe3 177.6(4) . . ? P4 C24 H24A 109.5 . . ? P4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? P4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? P4 C25 H25A 109.5 . . ? P4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? P4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? P4 C26 H26A 109.5 . . ? P4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? P4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O7 C27 Fe4 177.1(4) . . ? O8 C28 Fe4 177.0(4) . . ? N2 C29 S4 114.7(2) . . ? N2 C29 H29A 108.6 . . ? S4 C29 H29A 108.6 . . ? N2 C29 H29B 108.6 . . ? S4 C29 H29B 108.6 . . ? H29A C29 H29B 107.6 . . ? N2 C30 S3 114.8(2) . . ? N2 C30 H30A 108.6 . . ? S3 C30 H30A 108.6 . . ? N2 C30 H30B 108.6 . . ? S3 C30 H30B 108.6 . . ? H30A C30 H30B 107.5 . . ? N2 C31 C32 111.1(3) . . ? N2 C31 C36 114.9(3) . . ? C32 C31 C36 110.7(3) . . ? N2 C31 H31A 106.5 . . ? C32 C31 H31A 106.5 . . ? C36 C31 H31A 106.5 . . ? C31 C32 C33 110.9(4) . . ? C31 C32 H32A 109.5 . . ? C33 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 111.8(4) . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33B 109.3 . . ? C32 C33 H33B 109.3 . . ? H33A C33 H33B 107.9 . . ? C35 C34 C33 110.4(4) . . ? C35 C34 H34A 109.6 . . ? C33 C34 H34A 109.6 . . ? C35 C34 H34B 109.6 . . ? C33 C34 H34B 109.6 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C36 111.2(4) . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C31 C36 C35 111.5(3) . . ? C31 C36 H36A 109.3 . . ? C35 C36 H36A 109.3 . . ? C31 C36 H36B 109.3 . . ? C35 C36 H36B 109.3 . . ? H36A C36 H36B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.452 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.077 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; # Attachment '6 for B616236C.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 622708' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H35 Fe2 N O4 P2 S2' _chemical_formula_weight 579.24 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.0584(6) _cell_length_b 22.4454(10) _cell_length_c 11.6423(6) _cell_angle_alpha 90.00 _cell_angle_beta 113.615(2) _cell_angle_gamma 90.00 _cell_volume 2647.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6000 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour gray _exptl_crystal_size_max .48 _exptl_crystal_size_mid .42 _exptl_crystal_size_min .30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 1.398 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .7822 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 20088 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6055 _reflns_number_gt 5417 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6055 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0466 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1394 _refine_ls_wR_factor_gt 0.1335 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 0.92031(3) 0.166640(14) 0.59666(3) 0.03826(12) Uani 1 1 d . . . Fe2 Fe 1.07911(3) 0.140838(15) 0.48752(3) 0.03754(12) Uani 1 1 d . . . S2 S 1.14102(6) 0.17644(2) 0.68348(5) 0.03910(15) Uani 1 1 d . . . S1 S 0.96336(6) 0.07463(2) 0.54744(5) 0.03866(15) Uani 1 1 d . . . P2 P 1.15034(8) 0.22307(3) 0.42830(7) 0.0534(2) Uani 1 1 d . . . P1 P 0.71177(7) 0.15380(4) 0.46255(7) 0.05149(19) Uani 1 1 d . . . N1 N 1.1221(2) 0.07205(8) 0.80210(17) 0.0393(4) Uani 1 1 d . . . C12 C 1.2151(2) 0.11608(11) 0.7969(2) 0.0432(5) Uani 1 1 d . . . H12A H 1.2827 0.0958 0.7752 0.052 Uiso 1 1 calc R . . H12B H 1.2605 0.1338 0.8812 0.052 Uiso 1 1 calc R . . C11 C 1.0709(3) 0.03561(10) 0.6900(2) 0.0440(5) Uani 1 1 d . . . H11A H 1.0209 0.0020 0.7049 0.053 Uiso 1 1 calc R . . H11B H 1.1463 0.0186 0.6758 0.053 Uiso 1 1 calc R . . O4 O 0.9249(2) 0.11841(11) 0.22226(18) 0.0699(6) Uani 1 1 d . . . O2 O 0.8649(3) 0.14977(12) 0.8189(2) 0.0809(8) Uani 1 1 d . . . C4 C 0.9826(3) 0.12736(12) 0.3278(2) 0.0469(6) Uani 1 1 d . . . O1 O 0.8843(3) 0.29502(10) 0.5801(3) 0.0889(8) Uani 1 1 d . . . C13 C 1.1692(3) 0.03574(11) 0.9189(2) 0.0423(5) Uani 1 1 d . . . H13A H 1.1040 0.0026 0.9029 0.051 Uiso 1 1 calc R . . C2 C 0.8874(3) 0.15484(13) 0.7325(3) 0.0523(6) Uani 1 1 d . . . O3 O 1.3063(3) 0.06867(15) 0.5114(3) 0.1002(10) Uani 1 1 d . . . C1 C 0.8998(3) 0.24424(13) 0.5850(3) 0.0549(7) Uani 1 1 d . . . C19 C 1.3030(3) 0.00575(14) 0.9474(3) 0.0578(7) Uani 1 1 d . . . H19A H 1.3043 -0.0091 0.8679 0.069 Uiso 1 1 calc R . . H19B H 1.3734 0.0361 0.9815 0.069 Uiso 1 1 calc R . . C3 C 1.2172(3) 0.09725(15) 0.5015(3) 0.0582(7) Uani 1 1 d . . . C14 C 1.1593(4) 0.07267(15) 1.0253(3) 0.0644(8) Uani 1 1 d . C . H14A H 1.2163 0.1082 1.0383 0.077 Uiso 1 1 calc R . . H14B H 1.0672 0.0869 0.9980 0.077 Uiso 1 1 calc R . . C10 C 1.1870(5) 0.21291(19) 0.2902(3) 0.0849(12) Uani 1 1 d . . . H10A H 1.2179 0.2507 0.2693 0.127 Uiso 1 1 calc R . . H10B H 1.1070 0.2001 0.2194 0.127 Uiso 1 1 calc R . . H10C H 1.2557 0.1825 0.3075 0.127 Uiso 1 1 calc R . . C7 C 0.6730(4) 0.1354(2) 0.2992(3) 0.0937(14) Uani 1 1 d . . . H7A H 0.5772 0.1316 0.2539 0.140 Uiso 1 1 calc R . . H7B H 0.7156 0.0977 0.2948 0.140 Uiso 1 1 calc R . . H7C H 0.7054 0.1671 0.2610 0.140 Uiso 1 1 calc R . . C9 C 1.3061(4) 0.2529(2) 0.5389(3) 0.0971(15) Uani 1 1 d . . . H9A H 1.3283 0.2889 0.5037 0.146 Uiso 1 1 calc R . . H9B H 1.3757 0.2231 0.5550 0.146 Uiso 1 1 calc R . . H9C H 1.2983 0.2629 0.6176 0.146 Uiso 1 1 calc R . . C6 C 0.6043(4) 0.2186(2) 0.4389(4) 0.0912(12) Uani 1 1 d . . . H6A H 0.5150 0.2086 0.3789 0.137 Uiso 1 1 calc R . . H6B H 0.6386 0.2518 0.4062 0.137 Uiso 1 1 calc R . . H6C H 0.6016 0.2302 0.5191 0.137 Uiso 1 1 calc R . . C8 C 1.0471(6) 0.28923(18) 0.3867(5) 0.1008(14) Uani 1 1 d . . . H8A H 1.0929 0.3212 0.3630 0.151 Uiso 1 1 calc R . . H8B H 1.0289 0.3020 0.4587 0.151 Uiso 1 1 calc R . . H8C H 0.9638 0.2802 0.3160 0.151 Uiso 1 1 calc R . . C5 C 0.6270(4) 0.0961(3) 0.5090(5) 0.119(2) Uani 1 1 d . . . H5A H 0.5361 0.0928 0.4463 0.179 Uiso 1 1 calc R . . H5B H 0.6261 0.1062 0.5905 0.179 Uiso 1 1 calc R . . H5C H 0.6727 0.0581 0.5153 0.179 Uiso 1 1 calc R . . C18 C 1.3343(4) -0.04573(15) 1.0395(3) 0.0674(8) Uani 1 1 d . C . H18A H 1.2531 -0.0696 1.0190 0.081 Uiso 1 1 calc R . . H18B H 1.4004 -0.0716 1.0268 0.081 Uiso 1 1 calc R . . C15 C 1.1969(6) 0.0417(3) 1.1488(4) 0.1118(18) Uani 1 1 d . . . H15A H 1.1438 0.0048 1.1351 0.134 Uiso 1 1 calc R A 1 H15B H 1.1727 0.0677 1.2050 0.134 Uiso 1 1 calc R A 1 C17 C 1.3857(5) -0.0292(2) 1.1753(4) 0.1072(17) Uani 1 1 d . . . H17A H 1.3652 -0.0627 1.2198 0.129 Uiso 1 1 calc R B 1 H17B H 1.4830 -0.0270 1.2063 0.129 Uiso 1 1 calc R B 1 C16 C 1.3416(8) 0.0253(4) 1.2150(7) 0.069(2) Uani 0.50 1 d P C 1 H16A H 1.3945 0.0588 1.2045 0.082 Uiso 0.50 1 calc PR C 1 H16B H 1.3624 0.0219 1.3058 0.082 Uiso 0.50 1 calc PR C 1 C20 C 1.2701(18) 0.0028(6) 1.2062(11) 0.135(6) Uani 0.50 1 d P C 2 H20A H 1.2122 -0.0300 1.2105 0.162 Uiso 0.50 1 calc PR C 2 H20B H 1.3146 0.0182 1.2928 0.162 Uiso 0.50 1 calc PR C 2 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 0.0404(2) 0.0349(2) 0.0383(2) 0.00027(12) 0.01446(15) 0.00412(12) Fe2 0.0402(2) 0.0384(2) 0.03243(19) -0.00087(12) 0.01286(15) -0.00073(12) S2 0.0439(3) 0.0339(3) 0.0354(3) -0.0022(2) 0.0116(2) -0.0041(2) S1 0.0436(3) 0.0332(3) 0.0344(3) -0.0033(2) 0.0106(2) -0.0033(2) P2 0.0609(5) 0.0550(4) 0.0429(4) -0.0015(3) 0.0193(3) -0.0176(3) P1 0.0387(4) 0.0642(4) 0.0487(4) 0.0070(3) 0.0145(3) 0.0036(3) N1 0.0466(11) 0.0329(9) 0.0332(9) -0.0010(7) 0.0105(8) 0.0003(8) C12 0.0460(13) 0.0406(12) 0.0351(11) 0.0004(9) 0.0079(10) -0.0023(10) C11 0.0565(15) 0.0319(11) 0.0363(11) -0.0004(9) 0.0111(10) 0.0026(10) O4 0.0840(16) 0.0749(14) 0.0381(10) -0.0059(9) 0.0110(10) -0.0116(12) O2 0.097(2) 0.0986(19) 0.0683(15) 0.0113(13) 0.0554(15) 0.0262(14) C4 0.0540(15) 0.0438(13) 0.0419(12) -0.0016(10) 0.0180(11) -0.0050(11) O1 0.105(2) 0.0415(12) 0.106(2) 0.0049(12) 0.0273(16) 0.0205(12) C13 0.0467(13) 0.0427(13) 0.0351(11) 0.0027(9) 0.0140(10) 0.0039(10) C2 0.0539(16) 0.0533(15) 0.0522(15) 0.0003(12) 0.0237(13) 0.0106(12) O3 0.0832(19) 0.120(2) 0.109(2) 0.0110(18) 0.0513(18) 0.0456(17) C1 0.0552(16) 0.0458(15) 0.0578(16) 0.0019(12) 0.0166(13) 0.0104(12) C19 0.0562(17) 0.0682(18) 0.0486(14) 0.0189(13) 0.0206(13) 0.0153(14) C3 0.0573(17) 0.0715(19) 0.0508(15) 0.0004(13) 0.0269(13) 0.0096(14) C14 0.084(2) 0.0671(19) 0.0404(14) -0.0005(12) 0.0236(15) 0.0143(16) C10 0.110(3) 0.097(3) 0.0628(19) -0.0092(18) 0.050(2) -0.039(2) C7 0.055(2) 0.156(4) 0.0565(19) -0.025(2) 0.0078(16) -0.006(2) C9 0.095(3) 0.131(4) 0.0590(19) -0.009(2) 0.0237(19) -0.067(3) C6 0.061(2) 0.109(3) 0.096(3) 0.005(2) 0.022(2) 0.031(2) C8 0.131(4) 0.059(2) 0.120(4) 0.024(2) 0.058(3) 0.000(2) C5 0.058(2) 0.153(5) 0.121(4) 0.062(3) 0.007(2) -0.031(3) C18 0.071(2) 0.0652(19) 0.0630(18) 0.0178(15) 0.0241(16) 0.0222(15) C15 0.123(4) 0.170(5) 0.0506(19) 0.013(3) 0.043(2) 0.047(4) C17 0.118(4) 0.134(4) 0.058(2) 0.034(2) 0.023(2) 0.041(3) C16 0.060(4) 0.100(6) 0.033(3) 0.007(3) 0.006(3) -0.018(4) C20 0.246(19) 0.117(10) 0.084(7) 0.057(7) 0.109(11) 0.080(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 1.755(3) . ? Fe1 C2 1.779(3) . ? Fe1 P1 2.2258(8) . ? Fe1 S1 2.2447(6) . ? Fe1 S2 2.2474(7) . ? Fe1 Fe2 2.6118(5) . ? Fe2 C4 1.760(3) . ? Fe2 C3 1.766(3) . ? Fe2 P2 2.2221(8) . ? Fe2 S1 2.2470(7) . ? Fe2 S2 2.2496(6) . ? S2 C12 1.839(2) . ? S1 C11 1.832(2) . ? P2 C8 1.817(4) . ? P2 C9 1.816(3) . ? P2 C10 1.823(3) . ? P1 C5 1.804(4) . ? P1 C7 1.821(4) . ? P1 C6 1.828(4) . ? N1 C12 1.445(3) . ? N1 C11 1.449(3) . ? N1 C13 1.489(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? O4 C4 1.153(3) . ? O2 C2 1.135(3) . ? O1 C1 1.150(4) . ? C13 C14 1.530(4) . ? C13 C19 1.535(4) . ? C13 H13A 1.0000 . ? O3 C3 1.142(4) . ? C19 C18 1.519(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C14 C15 1.498(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C18 C17 1.496(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C15 C20 1.196(11) . ? C15 C16 1.517(10) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C17 C16 1.459(11) . ? C17 C20 1.627(13) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C2 98.65(13) . . ? C1 Fe1 P1 90.49(10) . . ? C2 Fe1 P1 94.65(10) . . ? C1 Fe1 S1 158.06(10) . . ? C2 Fe1 S1 103.28(9) . . ? P1 Fe1 S1 88.16(3) . . ? C1 Fe1 S2 91.22(10) . . ? C2 Fe1 S2 100.77(10) . . ? P1 Fe1 S2 164.05(3) . . ? S1 Fe1 S2 84.36(2) . . ? C1 Fe1 Fe2 105.90(10) . . ? C2 Fe1 Fe2 144.72(9) . . ? P1 Fe1 Fe2 109.85(3) . . ? S1 Fe1 Fe2 54.485(18) . . ? S2 Fe1 Fe2 54.533(18) . . ? C4 Fe2 C3 97.97(13) . . ? C4 Fe2 P2 87.45(9) . . ? C3 Fe2 P2 95.05(11) . . ? C4 Fe2 S1 91.96(9) . . ? C3 Fe2 S1 100.61(11) . . ? P2 Fe2 S1 164.26(3) . . ? C4 Fe2 S2 160.35(10) . . ? C3 Fe2 S2 101.68(10) . . ? P2 Fe2 S2 91.02(3) . . ? S1 Fe2 S2 84.25(2) . . ? C4 Fe2 Fe1 108.09(9) . . ? C3 Fe2 Fe1 143.44(10) . . ? P2 Fe2 Fe1 110.96(3) . . ? S1 Fe2 Fe1 54.406(18) . . ? S2 Fe2 Fe1 54.455(19) . . ? C12 S2 Fe1 109.98(8) . . ? C12 S2 Fe2 109.47(8) . . ? Fe1 S2 Fe2 71.01(2) . . ? C11 S1 Fe1 109.61(8) . . ? C11 S1 Fe2 110.73(9) . . ? Fe1 S1 Fe2 71.11(2) . . ? C8 P2 C9 101.7(3) . . ? C8 P2 C10 101.8(2) . . ? C9 P2 C10 100.9(2) . . ? C8 P2 Fe2 119.92(16) . . ? C9 P2 Fe2 116.12(14) . . ? C10 P2 Fe2 113.67(13) . . ? C5 P1 C7 102.6(2) . . ? C5 P1 C6 103.4(3) . . ? C7 P1 C6 99.0(2) . . ? C5 P1 Fe1 113.56(14) . . ? C7 P1 Fe1 120.40(14) . . ? C6 P1 Fe1 115.53(16) . . ? C12 N1 C11 112.1(2) . . ? C12 N1 C13 114.74(19) . . ? C11 N1 C13 112.40(18) . . ? N1 C12 S2 114.49(17) . . ? N1 C12 H12A 108.6 . . ? S2 C12 H12A 108.6 . . ? N1 C12 H12B 108.6 . . ? S2 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? N1 C11 S1 115.08(16) . . ? N1 C11 H11A 108.5 . . ? S1 C11 H11A 108.5 . . ? N1 C11 H11B 108.5 . . ? S1 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? O4 C4 Fe2 176.7(3) . . ? N1 C13 C14 109.3(2) . . ? N1 C13 C19 113.0(2) . . ? C14 C13 C19 116.0(2) . . ? N1 C13 H13A 105.9 . . ? C14 C13 H13A 105.9 . . ? C19 C13 H13A 105.9 . . ? O2 C2 Fe1 177.1(3) . . ? O1 C1 Fe1 177.7(3) . . ? C18 C19 C13 114.4(2) . . ? C18 C19 H19A 108.7 . . ? C13 C19 H19A 108.7 . . ? C18 C19 H19B 108.7 . . ? C13 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? O3 C3 Fe2 179.3(3) . . ? C15 C14 C13 116.3(3) . . ? C15 C14 H14A 108.2 . . ? C13 C14 H14A 108.2 . . ? C15 C14 H14B 108.2 . . ? C13 C14 H14B 108.2 . . ? H14A C14 H14B 107.4 . . ? P2 C10 H10A 109.5 . . ? P2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P1 C7 H7A 109.5 . . ? P1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P2 C9 H9A 109.5 . . ? P2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P1 C6 H6A 109.5 . . ? P1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P2 C8 H8A 109.5 . . ? P2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P1 C5 H5A 109.5 . . ? P1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C17 C18 C19 116.1(3) . . ? C17 C18 H18A 108.3 . . ? C19 C18 H18A 108.3 . . ? C17 C18 H18B 108.3 . . ? C19 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? C20 C15 C14 137.8(6) . . ? C20 C15 C16 36.8(9) . . ? C14 C15 C16 115.5(5) . . ? C20 C15 H15A 72.8 . . ? C14 C15 H15A 108.4 . . ? C16 C15 H15A 108.4 . . ? C20 C15 H15B 111.2 . . ? C14 C15 H15B 108.4 . . ? C16 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? C16 C17 C18 120.7(4) . . ? C16 C17 C20 33.7(6) . . ? C18 C17 C20 110.1(6) . . ? C16 C17 H17A 107.2 . . ? C18 C17 H17A 107.2 . . ? C20 C17 H17A 81.6 . . ? C16 C17 H17B 107.2 . . ? C18 C17 H17B 107.2 . . ? C20 C17 H17B 137.1 . . ? H17A C17 H17B 106.8 . . ? C17 C16 C15 117.4(6) . . ? C17 C16 H16A 108.0 . . ? C15 C16 H16A 108.0 . . ? C17 C16 H16B 108.0 . . ? C15 C16 H16B 108.0 . . ? H16A C16 H16B 107.2 . . ? C15 C20 C17 127.9(7) . . ? C15 C20 H20A 105.3 . . ? C17 C20 H20A 105.3 . . ? C15 C20 H20B 105.3 . . ? C17 C20 H20B 105.3 . . ? H20A C20 H20B 106.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.846 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.061 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ;