Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_cd24296 _database_code_depnum_ccdc_archive 'CCDC 267652' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H12 Fe2 O6 S' _chemical_formula_weight 492.06 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.900(3) _cell_length_b 8.359(3) _cell_length_c 15.538(6) _cell_angle_alpha 86.338(7) _cell_angle_beta 83.797(8) _cell_angle_gamma 89.919(7) _cell_volume 1017.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 508 _cell_measurement_theta_min 5.285 _cell_measurement_theta_max 35.814 _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.172 _exptl_crystal_size_mid 0.079 _exptl_crystal_size_min 0.038 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 1.561 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.85524 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5841 _diffrn_reflns_av_R_equivalents 0.0996 _diffrn_reflns_av_sigmaI/netI 0.2876 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 26.99 _reflns_number_total 4263 _reflns_number_gt 1354 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4263 _refine_ls_number_parameters 248 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.2118 _refine_ls_R_factor_gt 0.0780 _refine_ls_wR_factor_ref 0.2070 _refine_ls_wR_factor_gt 0.1713 _refine_ls_goodness_of_fit_ref 0.833 _refine_ls_restrained_S_all 0.837 _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 0.98820(19) 0.63237(17) 0.83800(10) 0.0479(5) Uani 1 1 d . . . Fe2 Fe 1.03066(19) 0.83829(17) 0.70798(10) 0.0464(5) Uani 1 1 d . . . S S 1.0368(4) 0.5690(3) 0.69770(18) 0.0535(8) Uani 1 1 d . . . O2 O 0.9693(11) 0.8108(10) 0.9955(5) 0.081(3) Uani 1 1 d . . . O3 O 1.3061(13) 0.4733(12) 0.8793(7) 0.118(4) Uani 1 1 d . . . O4 O 0.7408(11) 0.3767(10) 0.8985(6) 0.089(3) Uani 1 1 d . . . O5 O 1.0429(10) 1.1596(9) 0.7719(6) 0.081(3) Uani 1 1 d . . . O6 O 0.8495(12) 0.9053(11) 0.5539(6) 0.092(3) Uani 1 1 d . . . O7 O 1.3995(13) 0.8666(14) 0.6376(8) 0.131(4) Uani 1 1 d . . . C1 C 0.8507(13) 0.7924(11) 0.7947(6) 0.044(3) Uani 1 1 d . . . C2 C 0.9802(13) 0.7413(14) 0.9328(8) 0.058(3) Uani 1 1 d . . . C3 C 1.1851(17) 0.5325(14) 0.8618(8) 0.068(4) Uani 1 1 d . . . C4 C 0.8412(15) 0.4746(13) 0.8762(8) 0.059(3) Uani 1 1 d . . . C5 C 1.0397(13) 1.0331(13) 0.7461(7) 0.052(3) Uani 1 1 d . . . C6 C 0.9168(14) 0.8851(13) 0.6112(8) 0.058(3) Uani 1 1 d . . . C7 C 1.2612(19) 0.8503(17) 0.6659(10) 0.091(5) Uani 1 1 d . . . C8 C 0.6879(14) 0.8693(12) 0.8252(7) 0.051(3) Uani 1 1 d . . . C9 C 0.6325(15) 1.0088(12) 0.7790(7) 0.062(3) Uani 1 1 d . . . H9 H 0.6942 1.0500 0.7281 0.074 Uiso 1 1 calc R . . C10 C 0.4839(16) 1.0813(15) 0.8122(8) 0.068(4) Uani 1 1 d . . . H10 H 0.4530 1.1786 0.7860 0.082 Uiso 1 1 calc R . . C11 C 0.3822(15) 1.0168(14) 0.8808(7) 0.060(3) Uani 1 1 d . . . H11 H 0.2777 1.0619 0.8988 0.072 Uiso 1 1 calc R . . C12 C 0.4397(15) 0.8819(14) 0.9227(8) 0.063(3) Uani 1 1 d . . . H12 H 0.3741 0.8413 0.9726 0.076 Uiso 1 1 calc R . . C13 C 0.5855(13) 0.8023(13) 0.8972(7) 0.055(3) Uani 1 1 d . . . H13 H 0.6152 0.7076 0.9264 0.066 Uiso 1 1 calc R . . C14 C 0.8388(18) 0.4906(18) 0.6564(10) 0.109(5) Uani 1 1 d D . . C15 C 0.871(2) 0.3752(19) 0.5929(10) 0.132(6) Uiso 1 1 d D . . H15 H 0.9815 0.3464 0.5725 0.158 Uiso 1 1 calc R . . C16 C 0.7366(15) 0.3119(14) 0.5649(8) 0.070(4) Uani 1 1 d D . . H16 H 0.7488 0.2365 0.5232 0.084 Uiso 1 1 calc R . . C17 C 0.5745(15) 0.3602(15) 0.5992(7) 0.066(3) Uani 1 1 d D . . C18 C 0.5389(17) 0.4721(15) 0.6604(8) 0.074(4) Uani 1 1 d D . . H18 H 0.4287 0.5015 0.6804 0.089 Uiso 1 1 calc R . . C19 C 0.6728(19) 0.5321(19) 0.6873(10) 0.115(5) Uiso 1 1 d D . . H19 H 0.6581 0.6067 0.7294 0.138 Uiso 1 1 calc R . . C20 C 0.4147(18) 0.2893(16) 0.5637(9) 0.112(5) Uiso 1 1 d . . . H20A H 0.3148 0.3457 0.5856 0.168 Uiso 1 1 calc R . . H20B H 0.4030 0.1777 0.5823 0.168 Uiso 1 1 calc R . . H20C H 0.4280 0.3009 0.5015 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 0.0485(11) 0.0430(10) 0.0506(11) -0.0009(8) 0.0007(8) -0.0006(8) Fe2 0.0483(11) 0.0412(9) 0.0478(10) -0.0008(8) 0.0018(8) -0.0016(8) S 0.056(2) 0.0468(17) 0.0583(19) -0.0104(15) -0.0036(15) 0.0029(15) O2 0.086(7) 0.092(7) 0.068(6) -0.029(5) -0.002(5) 0.004(5) O3 0.088(8) 0.117(8) 0.158(10) -0.035(7) -0.034(7) 0.039(7) O4 0.085(7) 0.071(6) 0.109(8) 0.023(6) -0.014(6) -0.023(5) O5 0.082(7) 0.052(5) 0.114(8) -0.016(5) -0.023(5) -0.004(5) O6 0.081(7) 0.121(8) 0.077(7) 0.000(6) -0.028(6) 0.002(6) O7 0.060(7) 0.164(11) 0.174(11) -0.082(9) 0.010(7) -0.013(8) C1 0.063(8) 0.037(6) 0.033(6) -0.006(5) -0.006(5) 0.012(5) C2 0.041(7) 0.070(8) 0.063(8) 0.001(7) -0.012(6) 0.005(6) C3 0.066(10) 0.059(8) 0.082(9) -0.011(7) -0.014(8) 0.016(7) C4 0.063(9) 0.047(7) 0.066(8) 0.004(7) -0.008(7) 0.012(6) C5 0.047(7) 0.040(6) 0.066(8) 0.011(6) -0.002(6) -0.015(6) C6 0.041(8) 0.050(7) 0.078(10) 0.000(7) 0.010(7) 0.004(6) C7 0.070(10) 0.095(11) 0.110(12) -0.040(9) -0.006(9) -0.006(10) C8 0.059(8) 0.045(7) 0.053(7) -0.002(6) -0.021(6) -0.006(6) C9 0.065(9) 0.056(7) 0.061(8) 0.009(7) 0.001(7) 0.018(7) C10 0.075(10) 0.067(8) 0.062(8) -0.008(7) -0.002(7) 0.034(7) C11 0.048(8) 0.078(9) 0.050(8) 0.002(7) 0.009(6) 0.010(7) C12 0.056(9) 0.072(9) 0.058(8) -0.001(7) 0.009(6) -0.025(7) C13 0.043(8) 0.051(7) 0.064(8) 0.008(6) 0.017(6) 0.001(6) C14 0.077(11) 0.110(12) 0.143(15) -0.038(11) -0.005(10) 0.006(9) C16 0.067(9) 0.074(8) 0.071(9) -0.023(7) -0.014(7) 0.005(7) C17 0.056(9) 0.082(9) 0.052(8) 0.024(7) 0.006(6) 0.004(7) C18 0.084(10) 0.086(10) 0.055(8) 0.004(8) -0.018(7) -0.027(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C2 1.776(13) . ? Fe1 C4 1.787(13) . ? Fe1 C3 1.826(13) . ? Fe1 C1 1.860(9) . ? Fe1 S 2.268(3) . ? Fe1 Fe2 2.563(2) . ? Fe2 C5 1.772(12) . ? Fe2 C6 1.855(13) . ? Fe2 C7 1.868(15) . ? Fe2 C1 1.872(10) . ? Fe2 S 2.267(3) . ? S C14 1.887(14) . ? O2 C2 1.161(12) . ? O3 C3 1.127(12) . ? O4 C4 1.151(12) . ? O5 C5 1.155(11) . ? O6 C6 1.089(12) . ? O7 C7 1.138(14) . ? C1 C8 1.482(14) . ? C8 C13 1.395(13) . ? C8 C9 1.423(13) . ? C9 C10 1.385(14) . ? C9 H9 0.9300 . ? C10 C11 1.347(14) . ? C10 H10 0.9300 . ? C11 C12 1.368(14) . ? C11 H11 0.9300 . ? C12 C13 1.364(14) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C19 1.398(14) . ? C14 C15 1.426(14) . ? C15 C16 1.317(13) . ? C15 H15 0.9300 . ? C16 C17 1.402(12) . ? C16 H16 0.9300 . ? C17 C18 1.384(12) . ? C17 C20 1.564(17) . ? C18 C19 1.292(13) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 C4 99.6(5) . . ? C2 Fe1 C3 92.2(5) . . ? C4 Fe1 C3 98.8(5) . . ? C2 Fe1 C1 86.3(4) . . ? C4 Fe1 C1 103.6(5) . . ? C3 Fe1 C1 157.6(5) . . ? C2 Fe1 S 161.4(4) . . ? C4 Fe1 S 98.2(4) . . ? C3 Fe1 S 90.2(4) . . ? C1 Fe1 S 84.4(3) . . ? C2 Fe1 Fe2 106.8(4) . . ? C4 Fe1 Fe2 137.0(4) . . ? C3 Fe1 Fe2 113.1(4) . . ? C1 Fe1 Fe2 46.8(3) . . ? S Fe1 Fe2 55.56(9) . . ? C5 Fe2 C6 99.3(5) . . ? C5 Fe2 C7 90.7(5) . . ? C6 Fe2 C7 104.6(6) . . ? C5 Fe2 C1 88.0(4) . . ? C6 Fe2 C1 102.1(5) . . ? C7 Fe2 C1 153.1(6) . . ? C5 Fe2 S 163.7(4) . . ? C6 Fe2 S 96.3(4) . . ? C7 Fe2 S 89.7(4) . . ? C1 Fe2 S 84.2(3) . . ? C5 Fe2 Fe1 109.2(3) . . ? C6 Fe2 Fe1 134.5(3) . . ? C7 Fe2 Fe1 109.6(5) . . ? C1 Fe2 Fe1 46.5(3) . . ? S Fe2 Fe1 55.62(9) . . ? C14 S Fe2 112.4(5) . . ? C14 S Fe1 112.0(5) . . ? Fe2 S Fe1 68.82(9) . . ? C8 C1 Fe1 136.0(7) . . ? C8 C1 Fe2 136.2(7) . . ? Fe1 C1 Fe2 86.7(4) . . ? O2 C2 Fe1 177.7(10) . . ? O3 C3 Fe1 177.5(13) . . ? O4 C4 Fe1 176.6(10) . . ? O5 C5 Fe2 178.8(11) . . ? O6 C6 Fe2 176.7(12) . . ? O7 C7 Fe2 175.7(16) . . ? C13 C8 C9 119.7(11) . . ? C13 C8 C1 120.3(9) . . ? C9 C8 C1 120.0(10) . . ? C10 C9 C8 118.1(11) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? C11 C10 C9 122.7(11) . . ? C11 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? C10 C11 C12 117.0(12) . . ? C10 C11 H11 121.5 . . ? C12 C11 H11 121.5 . . ? C13 C12 C11 125.2(11) . . ? C13 C12 H12 117.4 . . ? C11 C12 H12 117.4 . . ? C12 C13 C8 117.0(10) . . ? C12 C13 H13 121.5 . . ? C8 C13 H13 121.5 . . ? C19 C14 C15 121.5(15) . . ? C19 C14 S 124.4(12) . . ? C15 C14 S 114.0(11) . . ? C16 C15 C14 116.2(16) . . ? C16 C15 H15 121.9 . . ? C14 C15 H15 121.9 . . ? C15 C16 C17 118.7(13) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C18 C17 C16 126.4(12) . . ? C18 C17 C20 114.8(11) . . ? C16 C17 C20 118.7(12) . . ? C19 C18 C17 113.8(15) . . ? C19 C18 H18 123.1 . . ? C17 C18 H18 123.1 . . ? C18 C19 C14 123.3(16) . . ? C18 C19 H19 118.3 . . ? C14 C19 H19 118.3 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Fe1 Fe2 C5 -0.3(5) . . . . ? C4 Fe1 Fe2 C5 125.3(6) . . . . ? C3 Fe1 Fe2 C5 -100.2(5) . . . . ? C1 Fe1 Fe2 C5 67.6(5) . . . . ? S Fe1 Fe2 C5 -173.5(4) . . . . ? C2 Fe1 Fe2 C6 -125.9(6) . . . . ? C4 Fe1 Fe2 C6 -0.3(7) . . . . ? C3 Fe1 Fe2 C6 134.2(6) . . . . ? C1 Fe1 Fe2 C6 -58.0(6) . . . . ? S Fe1 Fe2 C6 60.9(5) . . . . ? C2 Fe1 Fe2 C7 97.6(5) . . . . ? C4 Fe1 Fe2 C7 -136.8(7) . . . . ? C3 Fe1 Fe2 C7 -2.3(6) . . . . ? C1 Fe1 Fe2 C7 165.6(6) . . . . ? S Fe1 Fe2 C7 -75.6(4) . . . . ? C2 Fe1 Fe2 C1 -67.9(5) . . . . ? C4 Fe1 Fe2 C1 57.6(7) . . . . ? C3 Fe1 Fe2 C1 -167.9(6) . . . . ? S Fe1 Fe2 C1 118.8(4) . . . . ? C2 Fe1 Fe2 S 173.2(4) . . . . ? C4 Fe1 Fe2 S -61.2(5) . . . . ? C3 Fe1 Fe2 S 73.3(4) . . . . ? C1 Fe1 Fe2 S -118.8(4) . . . . ? C5 Fe2 S C14 128.3(14) . . . . ? C6 Fe2 S C14 -35.3(6) . . . . ? C7 Fe2 S C14 -140.0(7) . . . . ? C1 Fe2 S C14 66.3(6) . . . . ? Fe1 Fe2 S C14 105.9(5) . . . . ? C5 Fe2 S Fe1 22.3(13) . . . . ? C6 Fe2 S Fe1 -141.2(4) . . . . ? C7 Fe2 S Fe1 114.1(5) . . . . ? C1 Fe2 S Fe1 -39.7(3) . . . . ? C2 Fe1 S C14 -127.2(12) . . . . ? C4 Fe1 S C14 36.4(6) . . . . ? C3 Fe1 S C14 135.2(6) . . . . ? C1 Fe1 S C14 -66.6(6) . . . . ? Fe2 Fe1 S C14 -106.5(5) . . . . ? C2 Fe1 S Fe2 -20.7(11) . . . . ? C4 Fe1 S Fe2 142.9(3) . . . . ? C3 Fe1 S Fe2 -118.2(4) . . . . ? C1 Fe1 S Fe2 39.9(3) . . . . ? C2 Fe1 C1 C8 -52.0(11) . . . . ? C4 Fe1 C1 C8 47.0(11) . . . . ? C3 Fe1 C1 C8 -138.9(13) . . . . ? S Fe1 C1 C8 144.2(10) . . . . ? Fe2 Fe1 C1 C8 -169.3(12) . . . . ? C2 Fe1 C1 Fe2 117.3(4) . . . . ? C4 Fe1 C1 Fe2 -143.7(4) . . . . ? C3 Fe1 C1 Fe2 30.4(14) . . . . ? S Fe1 C1 Fe2 -46.5(3) . . . . ? C5 Fe2 C1 C8 50.2(10) . . . . ? C6 Fe2 C1 C8 -48.9(11) . . . . ? C7 Fe2 C1 C8 137.9(12) . . . . ? S Fe2 C1 C8 -144.1(10) . . . . ? Fe1 Fe2 C1 C8 169.3(12) . . . . ? C5 Fe2 C1 Fe1 -119.1(5) . . . . ? C6 Fe2 C1 Fe1 141.8(4) . . . . ? C7 Fe2 C1 Fe1 -31.3(12) . . . . ? S Fe2 C1 Fe1 46.6(3) . . . . ? C4 Fe1 C2 O2 -30(27) . . . . ? C3 Fe1 C2 O2 -129(27) . . . . ? C1 Fe1 C2 O2 73(27) . . . . ? S Fe1 C2 O2 133(26) . . . . ? Fe2 Fe1 C2 O2 116(27) . . . . ? C2 Fe1 C3 O3 7(29) . . . . ? C4 Fe1 C3 O3 -94(29) . . . . ? C1 Fe1 C3 O3 92(29) . . . . ? S Fe1 C3 O3 168(29) . . . . ? Fe2 Fe1 C3 O3 116(29) . . . . ? C2 Fe1 C4 O4 105(19) . . . . ? C3 Fe1 C4 O4 -161(19) . . . . ? C1 Fe1 C4 O4 17(20) . . . . ? S Fe1 C4 O4 -70(19) . . . . ? Fe2 Fe1 C4 O4 -23(20) . . . . ? C6 Fe2 C5 O5 92(53) . . . . ? C7 Fe2 C5 O5 -163(53) . . . . ? C1 Fe2 C5 O5 -10(53) . . . . ? S Fe2 C5 O5 -71(53) . . . . ? Fe1 Fe2 C5 O5 -52(53) . . . . ? C5 Fe2 C6 O6 -173(21) . . . . ? C7 Fe2 C6 O6 94(21) . . . . ? C1 Fe2 C6 O6 -83(21) . . . . ? S Fe2 C6 O6 2(21) . . . . ? Fe1 Fe2 C6 O6 -44(21) . . . . ? C5 Fe2 C7 O7 -52(17) . . . . ? C6 Fe2 C7 O7 48(17) . . . . ? C1 Fe2 C7 O7 -139(16) . . . . ? S Fe2 C7 O7 144(17) . . . . ? Fe1 Fe2 C7 O7 -163(17) . . . . ? Fe1 C1 C8 C13 -12.2(16) . . . . ? Fe2 C1 C8 C13 -176.7(8) . . . . ? Fe1 C1 C8 C9 170.1(8) . . . . ? Fe2 C1 C8 C9 5.6(16) . . . . ? C13 C8 C9 C10 5.4(16) . . . . ? C1 C8 C9 C10 -176.9(10) . . . . ? C8 C9 C10 C11 -6.7(18) . . . . ? C9 C10 C11 C12 6.1(18) . . . . ? C10 C11 C12 C13 -4.6(18) . . . . ? C11 C12 C13 C8 3.6(18) . . . . ? C9 C8 C13 C12 -3.9(15) . . . . ? C1 C8 C13 C12 178.4(9) . . . . ? Fe2 S C14 C19 -47.1(16) . . . . ? Fe1 S C14 C19 28.1(16) . . . . ? Fe2 S C14 C15 136.5(11) . . . . ? Fe1 S C14 C15 -148.3(11) . . . . ? C19 C14 C15 C16 1(2) . . . . ? S C14 C15 C16 177.2(11) . . . . ? C14 C15 C16 C17 -1(2) . . . . ? C15 C16 C17 C18 1(2) . . . . ? C15 C16 C17 C20 178.0(13) . . . . ? C16 C17 C18 C19 -1.1(18) . . . . ? C20 C17 C18 C19 -178.4(12) . . . . ? C17 C18 C19 C14 1(2) . . . . ? C15 C14 C19 C18 -1(3) . . . . ? S C14 C19 C18 -177.2(11) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.142 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.116