Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0186 loop_ _publ_author_name 'Chris J. Pickett' 'J. Elaine Barclay' 'Sian C. Davies' 'David J. Evans' 'Shirley A. Fairhurst' ; D.L.Hughes ; 'Xiaoming. Liu' 'Mathieu. Razavet' _publ_contact_author_name 'Prof Chris J Pickett' _publ_contact_author_address ; Biological Chemistry John Innes Centre Norwich Research Park Colney Norwich Norfolk NR4 7UH UNITED KINGDOM ; _publ_contact_author_email CHRIS.PICKETT@BBSRC.AC.UK _publ_section_title ; All-iron hydrogenase: synthesis, structure and properties of {2Fe3S}- assemblies related to the di-iron sub-site of the H-cluster ; data_math2b _database_code_CSD 195090 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 4a' _chemical_melting_point ? _chemical_formula_moiety 'C11 H12 Fe2 O5 S3' _chemical_formula_structural [Fe2(CO)5{MeSCH2C(Me)(CH2S)2}] _chemical_formula_sum 'C11 H12 Fe2 O5 S3' _chemical_formula_weight 432.09 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 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 18.4670(16) _cell_length_b 10.9622(12) _cell_length_c 16.9055(18) _cell_angle_alpha 90.00 _cell_angle_beta 105.267(8) _cell_angle_gamma 90.00 _cell_volume 3301.6(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description 'diamond-shaped plates' _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 2.150 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.976 _exptl_absorpt_correction_T_max 0.997 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 5.3 _diffrn_reflns_number 3678 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 21.0 _reflns_number_total 3528 _reflns_number_gt 2614 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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=\s^-2^(Fo^2^)' _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 3528 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0614 _refine_ls_wR_factor_gt 0.0544 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Fe1A Fe 0.50533(3) 0.18425(6) 0.14432(4) 0.04434(19) Uani 1 1 d . . . Fe2A Fe 0.61164(3) 0.25895(6) 0.09049(4) 0.04429(19) Uani 1 1 d . . . S1A S 0.61434(6) 0.25722(10) 0.22440(7) 0.0457(3) Uani 1 1 d . . . C1A C 0.6081(2) 0.4136(4) 0.2596(3) 0.0478(12) Uani 1 1 d . . . H1AA H 0.5720 0.4142 0.2922 0.057 Uiso 1 1 calc R . . H1AB H 0.6565 0.4345 0.2961 0.057 Uiso 1 1 calc R . . S2A S 0.50075(6) 0.35743(10) 0.07118(7) 0.0455(3) Uani 1 1 d . . . C2A C 0.5104(2) 0.4906(4) 0.1374(3) 0.0517(13) Uani 1 1 d . . . H2AA H 0.4968 0.5619 0.1027 0.062 Uiso 1 1 calc R . . H2AB H 0.4740 0.4834 0.1693 0.062 Uiso 1 1 calc R . . S3A S 0.68206(7) 0.42744(11) 0.09397(8) 0.0564(3) Uani 1 1 d . . . C3A C 0.6461(2) 0.5435(4) 0.1503(3) 0.0566(13) Uani 1 1 d . . . H3AD H 0.6890 0.5776 0.1902 0.068 Uiso 1 1 calc R . . H3AE H 0.6257 0.6082 0.1117 0.068 Uiso 1 1 calc R . . C31A C 0.7730(2) 0.4008(5) 0.1621(4) 0.0881(19) Uani 1 1 d . . . H3AA H 0.7675 0.3671 0.2126 0.132 Uiso 1 1 calc R . . H3AB H 0.8000 0.4764 0.1729 0.132 Uiso 1 1 calc R . . H3AC H 0.8002 0.3445 0.1372 0.132 Uiso 1 1 calc R . . C4A C 0.5866(2) 0.5149(4) 0.1966(3) 0.0470(12) Uani 1 1 d . . . C41A C 0.5797(3) 0.6334(4) 0.2436(3) 0.0668(15) Uani 1 1 d . . . H4AA H 0.6273 0.6518 0.2812 0.100 Uiso 1 1 calc R . . H4AB H 0.5426 0.6226 0.2735 0.100 Uiso 1 1 calc R . . H4AC H 0.5651 0.6994 0.2054 0.100 Uiso 1 1 calc R . . C13A C 0.4399(3) 0.2137(4) 0.2039(3) 0.0526(13) Uani 1 1 d . . . O13A O 0.3993(2) 0.2343(3) 0.2425(2) 0.0853(12) Uani 1 1 d . . . C14A C 0.4445(3) 0.1203(5) 0.0543(3) 0.0624(14) Uani 1 1 d . . . O14A O 0.4062(2) 0.0812(4) -0.0043(3) 0.0991(14) Uani 1 1 d . . . C15A C 0.5374(3) 0.0363(5) 0.1839(3) 0.0618(15) Uani 1 1 d . . . O15A O 0.5589(2) -0.0555(3) 0.2095(3) 0.0998(14) Uani 1 1 d . . . C24A C 0.5883(2) 0.2250(4) -0.0152(3) 0.0545(13) Uani 1 1 d . . . O24A O 0.5740(2) 0.1993(4) -0.0839(2) 0.0854(12) Uani 1 1 d . . . C25A C 0.6787(3) 0.1417(5) 0.1126(3) 0.0558(13) Uani 1 1 d . . . O25A O 0.7222(2) 0.0642(3) 0.1282(2) 0.0825(12) Uani 1 1 d . . . Fe1B Fe 0.14217(4) 0.31461(6) 0.00262(4) 0.0578(2) Uani 1 1 d . . . Fe2B Fe 0.08842(3) 0.23087(6) 0.11361(4) 0.0483(2) Uani 1 1 d . . . S1B S 0.21187(6) 0.23413(10) 0.12092(7) 0.0539(3) Uani 1 1 d . . . C1B C 0.2442(2) 0.0805(4) 0.1081(3) 0.0571(13) Uani 1 1 d . . . H1BA H 0.2748 0.0848 0.0696 0.069 Uiso 1 1 calc R . . H1BB H 0.2769 0.0551 0.1604 0.069 Uiso 1 1 calc R . . S2B S 0.07310(6) 0.14303(10) -0.01041(7) 0.0482(3) Uani 1 1 d . . . C2B C 0.1332(3) 0.0100(4) -0.0041(3) 0.0547(13) Uani 1 1 d . . . H2BA H 0.1012 -0.0604 -0.0221 0.066 Uiso 1 1 calc R . . H2BB H 0.1631 0.0210 -0.0429 0.066 Uiso 1 1 calc R . . S3B S 0.09434(7) 0.05699(11) 0.18651(7) 0.0534(3) Uani 1 1 d . . . C3B C 0.1438(2) -0.0554(4) 0.1417(3) 0.0547(13) Uani 1 1 d . . . H3BD H 0.1796 -0.0951 0.1867 0.066 Uiso 1 1 calc R . . H3BE H 0.1074 -0.1168 0.1161 0.066 Uiso 1 1 calc R . . C31B C 0.1616(3) 0.0789(5) 0.2844(3) 0.0759(16) Uani 1 1 d . . . H3BA H 0.2071 0.1122 0.2760 0.114 Uiso 1 1 calc R . . H3BB H 0.1721 0.0020 0.3121 0.114 Uiso 1 1 calc R . . H3BC H 0.1413 0.1343 0.3170 0.114 Uiso 1 1 calc R . . C4B C 0.1862(2) -0.0200(4) 0.0790(3) 0.0470(12) Uani 1 1 d . . . C41B C 0.2299(3) -0.1368(4) 0.0673(3) 0.0736(16) Uani 1 1 d . . . H4BA H 0.2650 -0.1578 0.1183 0.110 Uiso 1 1 calc R . . H4BB H 0.2566 -0.1220 0.0266 0.110 Uiso 1 1 calc R . . H4BC H 0.1952 -0.2028 0.0498 0.110 Uiso 1 1 calc R . . C13B C 0.2068(3) 0.2845(5) -0.0578(4) 0.0740(17) Uani 1 1 d . . . O13B O 0.2503(2) 0.2577(4) -0.0917(3) 0.1017(15) Uani 1 1 d . . . C14B C 0.0647(3) 0.3813(5) -0.0711(3) 0.0768(17) Uani 1 1 d . . . O14B O 0.0144(2) 0.4226(4) -0.1172(3) 0.1126(16) Uani 1 1 d . . . C15B C 0.1723(4) 0.4603(5) 0.0434(4) 0.092(2) Uani 1 1 d . . . O15B O 0.2028(11) 0.554(2) 0.0570(12) 0.081(5) Uani 0.50 1 d P . . O19B O 0.1774(12) 0.554(2) 0.0852(12) 0.098(6) Uani 0.50 1 d P . . C24B C -0.0077(3) 0.2697(4) 0.0874(3) 0.0603(14) Uani 1 1 d . . . O24B O -0.0696(2) 0.2986(3) 0.0705(2) 0.0883(12) Uani 1 1 d . . . C25B C 0.1056(3) 0.3434(5) 0.1915(3) 0.0699(16) Uani 1 1 d . . . O25B O 0.1159(2) 0.4179(4) 0.2406(2) 0.1072(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1A 0.0462(4) 0.0364(4) 0.0486(4) -0.0045(3) 0.0092(3) -0.0019(3) Fe2A 0.0442(4) 0.0456(4) 0.0426(4) -0.0028(3) 0.0107(3) 0.0061(3) S1A 0.0513(7) 0.0401(7) 0.0418(7) -0.0001(6) 0.0053(6) -0.0028(6) C1A 0.056(3) 0.042(3) 0.046(3) -0.010(2) 0.014(2) -0.009(2) S2A 0.0468(7) 0.0434(7) 0.0443(7) -0.0011(6) 0.0085(6) 0.0050(6) C2A 0.055(3) 0.040(3) 0.061(3) 0.003(2) 0.019(3) 0.005(2) S3A 0.0537(8) 0.0576(8) 0.0630(8) 0.0031(7) 0.0243(7) -0.0013(6) C3A 0.059(3) 0.041(3) 0.072(3) 0.001(3) 0.020(3) -0.007(2) C31A 0.048(3) 0.079(4) 0.132(5) 0.000(4) 0.013(3) -0.001(3) C4A 0.053(3) 0.037(3) 0.055(3) -0.004(2) 0.021(3) -0.002(2) C41A 0.077(4) 0.046(3) 0.085(4) -0.021(3) 0.035(3) -0.007(3) C13A 0.054(3) 0.047(3) 0.053(3) -0.007(2) 0.008(3) -0.006(3) O13A 0.077(3) 0.098(3) 0.090(3) -0.022(2) 0.038(2) 0.000(2) C14A 0.055(3) 0.055(3) 0.069(4) -0.008(3) 0.003(3) 0.000(3) O14A 0.099(3) 0.087(3) 0.089(3) -0.034(3) -0.014(3) -0.008(2) C15A 0.060(3) 0.038(3) 0.078(4) -0.009(3) 0.001(3) -0.010(3) O15A 0.106(3) 0.039(2) 0.132(4) 0.010(2) -0.007(3) 0.004(2) C24A 0.048(3) 0.054(3) 0.061(4) 0.001(3) 0.015(3) 0.014(2) O24A 0.098(3) 0.104(3) 0.051(2) -0.017(2) 0.014(2) 0.023(2) C25A 0.054(3) 0.057(4) 0.054(3) -0.007(3) 0.010(3) 0.004(3) O25A 0.073(3) 0.076(3) 0.092(3) -0.003(2) 0.009(2) 0.034(2) Fe1B 0.0611(5) 0.0421(4) 0.0589(5) 0.0134(4) -0.0039(4) -0.0103(4) Fe2B 0.0461(4) 0.0411(4) 0.0512(4) -0.0016(3) 0.0011(3) 0.0029(3) S1B 0.0454(7) 0.0450(8) 0.0616(8) 0.0097(6) -0.0029(6) -0.0071(6) C1B 0.046(3) 0.054(3) 0.072(3) 0.015(3) 0.017(3) 0.005(2) S2B 0.0481(7) 0.0403(7) 0.0493(7) 0.0009(6) 0.0004(6) -0.0030(6) C2B 0.064(3) 0.043(3) 0.055(3) 0.001(2) 0.012(3) -0.003(2) S3B 0.0507(7) 0.0581(8) 0.0528(8) 0.0074(6) 0.0162(6) 0.0007(6) C3B 0.056(3) 0.042(3) 0.067(3) 0.010(3) 0.018(3) 0.003(2) C31B 0.086(4) 0.087(4) 0.046(3) 0.010(3) 0.003(3) -0.004(3) C4B 0.050(3) 0.032(3) 0.064(3) 0.010(2) 0.024(3) 0.004(2) C41B 0.074(4) 0.057(4) 0.098(4) 0.004(3) 0.037(3) 0.018(3) C13B 0.068(4) 0.073(4) 0.075(4) 0.027(3) 0.008(3) -0.019(3) O13B 0.085(3) 0.126(4) 0.098(3) 0.031(3) 0.031(3) -0.018(3) C14B 0.092(4) 0.047(3) 0.072(4) 0.012(3) -0.011(3) -0.013(3) O14B 0.123(4) 0.073(3) 0.103(3) 0.015(3) -0.040(3) 0.015(3) C15B 0.097(5) 0.056(4) 0.092(5) 0.024(4) -0.032(4) -0.012(4) O15B 0.102(12) 0.048(7) 0.078(10) 0.012(7) -0.003(6) -0.027(8) O19B 0.113(14) 0.056(8) 0.102(14) 0.009(9) -0.014(8) -0.025(9) C24B 0.059(3) 0.044(3) 0.069(4) -0.008(3) 0.003(3) 0.000(3) O24B 0.055(2) 0.077(3) 0.122(3) -0.005(2) 0.005(2) 0.016(2) C25B 0.075(4) 0.060(4) 0.064(4) -0.007(3) -0.001(3) 0.015(3) O25B 0.128(4) 0.087(3) 0.084(3) -0.041(3) -0.013(3) 0.019(3) _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 Fe1A C14A 1.779(5) . ? Fe1A C15A 1.795(6) . ? Fe1A C13A 1.795(5) . ? Fe1A S2A 2.2549(13) . ? Fe1A S1A 2.2560(12) . ? Fe1A Fe2A 2.5086(9) . ? Fe2A C25A 1.755(5) . ? Fe2A C24A 1.764(5) . ? Fe2A S3A 2.2508(14) . ? Fe2A S1A 2.2512(13) . ? Fe2A S2A 2.2614(12) . ? S1A C1A 1.828(4) . ? C1A C4A 1.517(6) . ? C1A H1AA 0.9700 . ? C1A H1AB 0.9700 . ? S2A C2A 1.820(4) . ? C2A C4A 1.519(6) . ? C2A H2AA 0.9700 . ? C2A H2AB 0.9700 . ? S3A C31A 1.792(5) . ? S3A C3A 1.817(4) . ? C3A C4A 1.539(6) . ? C3A H3AD 0.9700 . ? C3A H3AE 0.9700 . ? C31A H3AA 0.9600 . ? C31A H3AB 0.9600 . ? C31A H3AC 0.9600 . ? C4A C41A 1.546(6) . ? C41A H4AA 0.9600 . ? C41A H4AB 0.9600 . ? C41A H4AC 0.9600 . ? C13A O13A 1.138(5) . ? C14A O14A 1.139(5) . ? C15A O15A 1.125(5) . ? C24A O24A 1.155(5) . ? C25A O25A 1.152(5) . ? Fe1B C15B 1.770(6) . ? Fe1B C14B 1.787(6) . ? Fe1B C13B 1.794(7) . ? Fe1B S2B 2.2506(13) . ? Fe1B S1B 2.2537(13) . ? Fe1B Fe2B 2.5158(10) . ? Fe2B C24B 1.765(5) . ? Fe2B C25B 1.772(6) . ? Fe2B S1B 2.2505(14) . ? Fe2B S2B 2.2563(13) . ? Fe2B S3B 2.2567(14) . ? S1B C1B 1.819(4) . ? C1B C4B 1.524(6) . ? C1B H1BA 0.9700 . ? C1B H1BB 0.9700 . ? S2B C2B 1.818(4) . ? C2B C4B 1.522(6) . ? C2B H2BA 0.9700 . ? C2B H2BB 0.9700 . ? S3B C31B 1.804(4) . ? S3B C3B 1.814(4) . ? C3B C4B 1.524(6) . ? C3B H3BD 0.9700 . ? C3B H3BE 0.9700 . ? C31B H3BA 0.9600 . ? C31B H3BB 0.9600 . ? C31B H3BC 0.9600 . ? C4B C41B 1.554(6) . ? C41B H4BA 0.9600 . ? C41B H4BB 0.9600 . ? C41B H4BC 0.9600 . ? C13B O13B 1.142(6) . ? C14B O14B 1.138(5) . ? C15B O15B 1.17(2) . ? C15B O19B 1.23(2) . ? O15B O19B 0.75(2) . ? C24B O24B 1.148(5) . ? C25B O25B 1.144(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14A Fe1A C15A 92.0(2) . . ? C14A Fe1A C13A 100.6(2) . . ? C15A Fe1A C13A 99.1(2) . . ? C14A Fe1A S2A 86.49(17) . . ? C15A Fe1A S2A 157.87(18) . . ? C13A Fe1A S2A 102.88(15) . . ? C14A Fe1A S1A 156.22(17) . . ? C15A Fe1A S1A 86.65(15) . . ? C13A Fe1A S1A 103.06(14) . . ? S2A Fe1A S1A 85.94(4) . . ? C14A Fe1A Fe2A 101.33(17) . . ? C15A Fe1A Fe2A 102.53(17) . . ? C13A Fe1A Fe2A 148.43(15) . . ? S2A Fe1A Fe2A 56.38(3) . . ? S1A Fe1A Fe2A 56.09(4) . . ? C25A Fe2A C24A 91.8(2) . . ? C25A Fe2A S3A 102.98(16) . . ? C24A Fe2A S3A 100.66(16) . . ? C25A Fe2A S1A 87.28(16) . . ? C24A Fe2A S1A 162.11(16) . . ? S3A Fe2A S1A 96.95(5) . . ? C25A Fe2A S2A 160.34(16) . . ? C24A Fe2A S2A 89.09(14) . . ? S3A Fe2A S2A 96.14(5) . . ? S1A Fe2A S2A 85.91(5) . . ? C25A Fe2A Fe1A 105.06(16) . . ? C24A Fe2A Fe1A 107.03(15) . . ? S3A Fe2A Fe1A 139.49(4) . . ? S1A Fe2A Fe1A 56.27(4) . . ? S2A Fe2A Fe1A 56.13(4) . . ? C1A S1A Fe2A 109.44(14) . . ? C1A S1A Fe1A 113.91(15) . . ? Fe2A S1A Fe1A 67.64(4) . . ? C4A C1A S1A 119.0(3) . . ? C4A C1A H1AA 107.6 . . ? S1A C1A H1AA 107.6 . . ? C4A C1A H1AB 107.6 . . ? S1A C1A H1AB 107.6 . . ? H1AA C1A H1AB 107.0 . . ? C2A S2A Fe1A 110.77(15) . . ? C2A S2A Fe2A 110.83(14) . . ? Fe1A S2A Fe2A 67.49(4) . . ? C4A C2A S2A 118.0(3) . . ? C4A C2A H2AA 107.8 . . ? S2A C2A H2AA 107.8 . . ? C4A C2A H2AB 107.8 . . ? S2A C2A H2AB 107.8 . . ? H2AA C2A H2AB 107.1 . . ? C31A S3A C3A 100.8(2) . . ? C31A S3A Fe2A 108.67(18) . . ? C3A S3A Fe2A 107.45(15) . . ? C4A C3A S3A 122.1(3) . . ? C4A C3A H3AD 106.8 . . ? S3A C3A H3AD 106.8 . . ? C4A C3A H3AE 106.8 . . ? S3A C3A H3AE 106.8 . . ? H3AD C3A H3AE 106.6 . . ? S3A C31A H3AA 109.5 . . ? S3A C31A H3AB 109.5 . . ? H3AA C31A H3AB 109.5 . . ? S3A C31A H3AC 109.5 . . ? H3AA C31A H3AC 109.5 . . ? H3AB C31A H3AC 109.5 . . ? C1A C4A C2A 111.1(4) . . ? C1A C4A C3A 114.6(4) . . ? C2A C4A C3A 111.3(4) . . ? C1A C4A C41A 107.2(4) . . ? C2A C4A C41A 107.4(4) . . ? C3A C4A C41A 104.8(3) . . ? C4A C41A H4AA 109.5 . . ? C4A C41A H4AB 109.5 . . ? H4AA C41A H4AB 109.5 . . ? C4A C41A H4AC 109.5 . . ? H4AA C41A H4AC 109.5 . . ? H4AB C41A H4AC 109.5 . . ? O13A C13A Fe1A 178.6(4) . . ? O14A C14A Fe1A 178.5(5) . . ? O15A C15A Fe1A 178.7(5) . . ? O24A C24A Fe2A 177.9(4) . . ? O25A C25A Fe2A 178.7(5) . . ? C15B Fe1B C14B 90.8(2) . . ? C15B Fe1B C13B 101.5(3) . . ? C14B Fe1B C13B 102.1(3) . . ? C15B Fe1B S2B 154.7(3) . . ? C14B Fe1B S2B 86.81(17) . . ? C13B Fe1B S2B 103.60(18) . . ? C15B Fe1B S1B 87.73(18) . . ? C14B Fe1B S1B 160.7(2) . . ? C13B Fe1B S1B 97.06(17) . . ? S2B Fe1B S1B 86.34(5) . . ? C15B Fe1B Fe2B 100.6(3) . . ? C14B Fe1B Fe2B 105.58(19) . . ? C13B Fe1B Fe2B 144.06(18) . . ? S2B Fe1B Fe2B 56.18(4) . . ? S1B Fe1B Fe2B 55.99(4) . . ? C24B Fe2B C25B 89.4(2) . . ? C24B Fe2B S1B 161.31(17) . . ? C25B Fe2B S1B 88.16(17) . . ? C24B Fe2B S2B 89.87(16) . . ? C25B Fe2B S2B 160.45(18) . . ? S1B Fe2B S2B 86.28(5) . . ? C24B Fe2B S3B 103.99(16) . . ? C25B Fe2B S3B 102.05(17) . . ? S1B Fe2B S3B 94.63(5) . . ? S2B Fe2B S3B 97.08(5) . . ? C24B Fe2B Fe1B 107.03(17) . . ? C25B Fe2B Fe1B 105.78(18) . . ? S1B Fe2B Fe1B 56.10(4) . . ? S2B Fe2B Fe1B 55.96(4) . . ? S3B Fe2B Fe1B 138.04(5) . . ? C1B S1B Fe2B 109.76(14) . . ? C1B S1B Fe1B 112.68(16) . . ? Fe2B S1B Fe1B 67.91(4) . . ? C4B C1B S1B 118.9(3) . . ? C4B C1B H1BA 107.6 . . ? S1B C1B H1BA 107.6 . . ? C4B C1B H1BB 107.6 . . ? S1B C1B H1BB 107.6 . . ? H1BA C1B H1BB 107.0 . . ? C2B S2B Fe1B 110.07(15) . . ? C2B S2B Fe2B 111.26(15) . . ? Fe1B S2B Fe2B 67.86(4) . . ? C4B C2B S2B 117.5(3) . . ? C4B C2B H2BA 107.9 . . ? S2B C2B H2BA 107.9 . . ? C4B C2B H2BB 107.9 . . ? S2B C2B H2BB 107.9 . . ? H2BA C2B H2BB 107.2 . . ? C31B S3B C3B 100.0(2) . . ? C31B S3B Fe2B 108.10(18) . . ? C3B S3B Fe2B 107.61(15) . . ? C4B C3B S3B 121.7(3) . . ? C4B C3B H3BD 106.9 . . ? S3B C3B H3BD 106.9 . . ? C4B C3B H3BE 106.9 . . ? S3B C3B H3BE 106.9 . . ? H3BD C3B H3BE 106.7 . . ? S3B C31B H3BA 109.5 . . ? S3B C31B H3BB 109.5 . . ? H3BA C31B H3BB 109.5 . . ? S3B C31B H3BC 109.5 . . ? H3BA C31B H3BC 109.5 . . ? H3BB C31B H3BC 109.5 . . ? C2B C4B C3B 111.9(4) . . ? C2B C4B C1B 111.6(4) . . ? C3B C4B C1B 113.9(4) . . ? C2B C4B C41B 106.9(4) . . ? C3B C4B C41B 104.9(3) . . ? C1B C4B C41B 107.0(4) . . ? C4B C41B H4BA 109.5 . . ? C4B C41B H4BB 109.5 . . ? H4BA C41B H4BB 109.5 . . ? C4B C41B H4BC 109.5 . . ? H4BA C41B H4BC 109.5 . . ? H4BB C41B H4BC 109.5 . . ? O13B C13B Fe1B 174.3(5) . . ? O14B C14B Fe1B 178.6(6) . . ? O15B C15B O19B 36.4(10) . . ? O15B C15B Fe1B 163.5(12) . . ? O19B C15B Fe1B 160.1(11) . . ? O19B O15B C15B 76(3) . . ? O15B O19B C15B 67(3) . . ? O24B C24B Fe2B 177.9(4) . . ? O25B C25B Fe2B 178.5(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 20.98 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.240 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.057 #===END data_math5 _database_code_CSD 195091 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 4b' _chemical_melting_point ? _chemical_formula_moiety 'C17 H16 Fe2 O5 S3' _chemical_formula_structural [Fe2(CO)5{PhCH2SCH2C(Me)(CH2S)2}] _chemical_formula_sum 'C17 H16 Fe2 O5 S3' _chemical_formula_weight 508.18 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8755(11) _cell_length_b 11.3853(13) _cell_length_c 10.3912(13) _cell_angle_alpha 110.555(10) _cell_angle_beta 92.983(9) _cell_angle_gamma 104.374(9) _cell_volume 1047.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description 'elongated plates' _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 1.708 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.25 _exptl_absorpt_correction_T_max 0.30 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 0 _diffrn_reflns_number 4297 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.0 _reflns_number_total 3686 _reflns_number_gt 2715 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0579P)^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 3686 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1047 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.22416(5) 0.09208(5) 0.24546(5) 0.05051(17) Uani 1 1 d . . . Fe2 Fe 0.48554(5) 0.19468(5) 0.29537(5) 0.04454(16) Uani 1 1 d . . . S1 S 0.37303(10) 0.05117(8) 0.38571(9) 0.0482(2) Uani 1 1 d . . . C1 C 0.3646(4) 0.1343(4) 0.5688(4) 0.0539(9) Uani 1 1 d . . . H1A H 0.2664 0.1109 0.5819 0.065 Uiso 1 1 calc R . . H1B H 0.4159 0.0995 0.6218 0.065 Uiso 1 1 calc R . . S2 S 0.32786(11) 0.30558(9) 0.37748(9) 0.0519(2) Uani 1 1 d . . . C2 C 0.3345(5) 0.3442(4) 0.5646(4) 0.0624(11) Uani 1 1 d . . . H2A H 0.3715 0.4384 0.6116 0.075 Uiso 1 1 calc R . . H2B H 0.2382 0.3199 0.5826 0.075 Uiso 1 1 calc R . . S3 S 0.64995(10) 0.33229(8) 0.47697(9) 0.0480(2) Uani 1 1 d . . . C3 C 0.5790(4) 0.3316(5) 0.6352(4) 0.0697(12) Uani 1 1 d . . . H3A H 0.6238 0.2803 0.6712 0.084 Uiso 1 1 calc R . . H3B H 0.6101 0.4208 0.7028 0.084 Uiso 1 1 calc R . . C31 C 0.7950(4) 0.2647(4) 0.4911(4) 0.0612(10) Uani 1 1 d . . . H31A H 0.7573 0.1772 0.4903 0.073 Uiso 1 1 calc R . . H31B H 0.8424 0.2574 0.4104 0.073 Uiso 1 1 calc R . . C311 C 0.9014(4) 0.3455(4) 0.6204(4) 0.0537(9) Uani 1 1 d . . . C312 C 0.9597(5) 0.4791(4) 0.6583(5) 0.0740(12) Uani 1 1 d . . . H312 H 0.9324 0.5210 0.6033 0.089 Uiso 1 1 calc R . . C313 C 1.0581(5) 0.5506(5) 0.7774(5) 0.0860(15) Uani 1 1 d . . . H313 H 1.0963 0.6403 0.8024 0.103 Uiso 1 1 calc R . . C314 C 1.0994(5) 0.4899(6) 0.8582(5) 0.0812(14) Uani 1 1 d . . . H314 H 1.1679 0.5376 0.9364 0.097 Uiso 1 1 calc R . . C315 C 1.0409(5) 0.3608(6) 0.8246(5) 0.0837(14) Uani 1 1 d . . . H315 H 1.0663 0.3202 0.8818 0.100 Uiso 1 1 calc R . . C316 C 0.9425(4) 0.2881(5) 0.7046(5) 0.0683(11) Uani 1 1 d . . . H316 H 0.9041 0.1987 0.6814 0.082 Uiso 1 1 calc R . . C4 C 0.4207(4) 0.2814(4) 0.6316(3) 0.0517(9) Uani 1 1 d . . . C41 C 0.3999(5) 0.3225(5) 0.7870(4) 0.0739(13) Uani 1 1 d . . . H41A H 0.4293 0.4163 0.8309 0.111 Uiso 1 1 calc R . . H41B H 0.4555 0.2867 0.8333 0.111 Uiso 1 1 calc R . . H41C H 0.3018 0.2901 0.7927 0.111 Uiso 1 1 calc R . . C13 C 0.0604(5) 0.0553(4) 0.3073(5) 0.0707(12) Uani 1 1 d . . . O13 O -0.0452(4) 0.0306(4) 0.3465(5) 0.1119(13) Uani 1 1 d . . . C14 C 0.1721(5) 0.1447(5) 0.1128(5) 0.0766(13) Uani 1 1 d . . . O14 O 0.1400(5) 0.1770(4) 0.0275(4) 0.1212(15) Uani 1 1 d . . . C15 C 0.2186(4) -0.0629(4) 0.1179(4) 0.0645(11) Uani 1 1 d . . . O15 O 0.2186(4) -0.1609(3) 0.0380(4) 0.1012(12) Uani 1 1 d . . . C24 C 0.5185(4) 0.2744(4) 0.1774(4) 0.0622(10) Uani 1 1 d . . . O24 O 0.5368(4) 0.3234(3) 0.0979(3) 0.0931(11) Uani 1 1 d . . . C25 C 0.5690(4) 0.0777(4) 0.2013(4) 0.0586(10) Uani 1 1 d . . . O25 O 0.6193(4) -0.0011(4) 0.1396(3) 0.0918(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0472(3) 0.0474(3) 0.0524(3) 0.0149(2) 0.0010(2) 0.0127(2) Fe2 0.0489(3) 0.0426(3) 0.0392(3) 0.0143(2) 0.0049(2) 0.0100(2) S1 0.0545(5) 0.0395(5) 0.0554(5) 0.0203(4) 0.0106(4) 0.0176(4) C1 0.061(2) 0.057(2) 0.055(2) 0.0289(18) 0.0163(17) 0.0237(19) S2 0.0696(6) 0.0427(5) 0.0475(5) 0.0167(4) 0.0047(4) 0.0247(4) C2 0.091(3) 0.058(2) 0.048(2) 0.0172(18) 0.017(2) 0.041(2) S3 0.0527(5) 0.0420(5) 0.0449(5) 0.0149(4) 0.0027(4) 0.0090(4) C3 0.067(3) 0.087(3) 0.0398(19) 0.020(2) -0.0007(18) 0.004(2) C31 0.060(2) 0.046(2) 0.067(2) 0.0112(19) -0.0041(19) 0.0165(18) C311 0.047(2) 0.055(2) 0.056(2) 0.0166(18) 0.0042(16) 0.0159(17) C312 0.081(3) 0.062(3) 0.070(3) 0.021(2) -0.008(2) 0.014(2) C313 0.074(3) 0.069(3) 0.080(3) 0.007(3) -0.009(3) -0.003(2) C314 0.059(3) 0.110(4) 0.060(3) 0.021(3) 0.001(2) 0.016(3) C315 0.065(3) 0.122(5) 0.077(3) 0.053(3) 0.007(2) 0.029(3) C316 0.058(2) 0.072(3) 0.080(3) 0.036(2) 0.006(2) 0.019(2) C4 0.064(2) 0.058(2) 0.0396(18) 0.0190(16) 0.0132(16) 0.0262(19) C41 0.097(3) 0.092(3) 0.046(2) 0.027(2) 0.026(2) 0.044(3) C13 0.068(3) 0.067(3) 0.079(3) 0.024(2) 0.017(2) 0.025(2) O13 0.073(2) 0.116(3) 0.151(4) 0.047(3) 0.049(2) 0.032(2) C14 0.076(3) 0.079(3) 0.069(3) 0.023(2) -0.010(2) 0.022(2) O14 0.149(4) 0.132(4) 0.094(3) 0.059(3) -0.028(3) 0.046(3) C15 0.059(2) 0.058(3) 0.059(2) 0.009(2) 0.0085(19) 0.007(2) O15 0.117(3) 0.063(2) 0.087(2) -0.0065(19) 0.023(2) 0.011(2) C24 0.072(3) 0.058(2) 0.045(2) 0.0146(19) 0.0032(19) 0.007(2) O24 0.126(3) 0.093(2) 0.0645(18) 0.0482(19) 0.0118(19) 0.010(2) C25 0.063(2) 0.067(3) 0.047(2) 0.0209(19) 0.0133(18) 0.020(2) O25 0.114(3) 0.099(3) 0.076(2) 0.0249(19) 0.038(2) 0.060(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C13 1.779(5) . ? Fe1 C15 1.782(4) . ? Fe1 C14 1.784(5) . ? Fe1 S1 2.2574(11) . ? Fe1 S2 2.2617(11) . ? Fe1 Fe2 2.4969(8) . ? Fe2 C24 1.764(4) . ? Fe2 C25 1.767(4) . ? Fe2 S3 2.2347(10) . ? Fe2 S1 2.2516(10) . ? Fe2 S2 2.2594(11) . ? S1 C1 1.820(4) . ? C1 C4 1.507(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? S2 C2 1.830(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? S3 C31 1.808(4) . ? S3 C3 1.822(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C31 C311 1.504(5) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C311 C316 1.360(6) . ? C311 C312 1.387(6) . ? C312 C313 1.383(6) . ? C312 H312 0.9300 . ? C313 C314 1.364(7) . ? C313 H313 0.9300 . ? C314 C315 1.346(7) . ? C314 H314 0.9300 . ? C315 C316 1.391(6) . ? C315 H315 0.9300 . ? C316 H316 0.9300 . ? C4 C3 1.519(6) . ? C4 C2 1.521(5) . ? C4 C41 1.556(5) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C13 O13 1.145(5) . ? C14 O14 1.131(5) . ? C15 O15 1.133(5) . ? C24 O24 1.147(5) . ? C25 O25 1.146(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Fe1 C15 101.7(2) . . ? C13 Fe1 C14 100.1(2) . . ? C15 Fe1 C14 90.6(2) . . ? C13 Fe1 S1 102.77(15) . . ? C15 Fe1 S1 86.59(15) . . ? C14 Fe1 S1 157.09(17) . . ? C13 Fe1 S2 104.02(15) . . ? C15 Fe1 S2 154.12(14) . . ? C14 Fe1 S2 87.23(15) . . ? S1 Fe1 S2 85.49(4) . . ? C13 Fe1 Fe2 149.39(15) . . ? C15 Fe1 Fe2 99.04(13) . . ? C14 Fe1 Fe2 101.94(16) . . ? S1 Fe1 Fe2 56.27(3) . . ? S2 Fe1 Fe2 56.43(3) . . ? C24 Fe2 C25 90.24(19) . . ? C24 Fe2 S3 100.39(13) . . ? C25 Fe2 S3 103.99(13) . . ? C24 Fe2 S1 158.84(13) . . ? C25 Fe2 S1 88.69(13) . . ? S3 Fe2 S1 100.37(4) . . ? C24 Fe2 S2 90.00(15) . . ? C25 Fe2 S2 164.93(13) . . ? S3 Fe2 S2 90.78(4) . . ? S1 Fe2 S2 85.68(4) . . ? C24 Fe2 Fe1 104.23(14) . . ? C25 Fe2 Fe1 108.93(13) . . ? S3 Fe2 Fe1 138.34(3) . . ? S1 Fe2 Fe1 56.49(3) . . ? S2 Fe2 Fe1 56.52(3) . . ? C1 S1 Fe2 110.74(12) . . ? C1 S1 Fe1 112.04(13) . . ? Fe2 S1 Fe1 67.25(3) . . ? C4 C1 S1 118.3(3) . . ? C4 C1 H1A 107.7 . . ? S1 C1 H1A 107.7 . . ? C4 C1 H1B 107.7 . . ? S1 C1 H1B 107.7 . . ? H1A C1 H1B 107.1 . . ? C2 S2 Fe2 110.12(13) . . ? C2 S2 Fe1 113.84(14) . . ? Fe2 S2 Fe1 67.05(3) . . ? C4 C2 S2 118.0(2) . . ? C4 C2 H2A 107.8 . . ? S2 C2 H2A 107.8 . . ? C4 C2 H2B 107.8 . . ? S2 C2 H2B 107.8 . . ? H2A C2 H2B 107.1 . . ? C31 S3 C3 99.8(2) . . ? C31 S3 Fe2 110.66(13) . . ? C3 S3 Fe2 108.02(13) . . ? C4 C3 S3 120.3(3) . . ? C4 C3 H3A 107.2 . . ? S3 C3 H3A 107.2 . . ? C4 C3 H3B 107.2 . . ? S3 C3 H3B 107.2 . . ? H3A C3 H3B 106.9 . . ? C311 C31 S3 113.3(3) . . ? C311 C31 H31A 108.9 . . ? S3 C31 H31A 108.9 . . ? C311 C31 H31B 108.9 . . ? S3 C31 H31B 108.9 . . ? H31A C31 H31B 107.7 . . ? C316 C311 C312 118.1(4) . . ? C316 C311 C31 120.2(4) . . ? C312 C311 C31 121.7(4) . . ? C313 C312 C311 120.4(4) . . ? C313 C312 H312 119.8 . . ? C311 C312 H312 119.8 . . ? C314 C313 C312 120.2(5) . . ? C314 C313 H313 119.9 . . ? C312 C313 H313 119.9 . . ? C315 C314 C313 120.0(4) . . ? C315 C314 H314 120.0 . . ? C313 C314 H314 120.0 . . ? C314 C315 C316 120.1(5) . . ? C314 C315 H315 119.9 . . ? C316 C315 H315 119.9 . . ? C311 C316 C315 121.2(5) . . ? C311 C316 H316 119.4 . . ? C315 C316 H316 119.4 . . ? C1 C4 C3 113.5(3) . . ? C1 C4 C2 111.0(3) . . ? C3 C4 C2 113.4(3) . . ? C1 C4 C41 106.1(3) . . ? C3 C4 C41 104.9(3) . . ? C2 C4 C41 107.3(3) . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O13 C13 Fe1 179.4(5) . . ? O14 C14 Fe1 179.1(5) . . ? O15 C15 Fe1 178.2(4) . . ? O24 C24 Fe2 178.0(4) . . ? O25 C25 Fe2 177.9(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.437 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.069 #===END data_math7 _database_code_CSD 195092 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 5a' _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 N, C11 H12 Fe2 N O4 S3' _chemical_formula_structural (NEt4)[Fe2(CO)4(CN){MeCH2C(Me)(CH2S)2}] _chemical_formula_sum 'C19 H32 Fe2 N2 O4 S3' _chemical_formula_weight 560.35 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2990(14) _cell_length_b 9.357(4) _cell_length_c 16.534(3) _cell_angle_alpha 85.87(2) _cell_angle_beta 78.327(13) _cell_angle_gamma 77.90(2) _cell_volume 1228.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description rhombs _exptl_crystal_colour orange _exptl_crystal_size_max 'ca 0.5' _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 1.462 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.920 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_process_details 'EMPABS, Sheldrick et al, 1977)' _exptl_special_details ; All preparatory work on the crystals was carried out in a 'cool room' (temperature ca 5 deg.) and the crystals were coated in silicone grease due to the sensitivity of the sample to ambient temperature and air. The initial temperature of the cryostream was set to 259 K and then lowered slowly to 140 K to avoid cracking the crystal. ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 4.4 _diffrn_reflns_number 7586 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 30.0 _reflns_number_total 7138 _reflns_number_gt 5512 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+4.6394P] 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 7138 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1317 _refine_ls_goodness_of_fit_ref 1.247 _refine_ls_restrained_S_all 1.247 _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 0.38094(7) 0.70591(6) 0.28203(3) 0.01858(12) Uani 1 1 d . . . Fe2 Fe 0.43130(7) 0.76537(6) 0.12790(3) 0.01655(12) Uani 1 1 d . . . S1 S 0.17542(11) 0.78874(10) 0.21082(6) 0.01966(18) Uani 1 1 d . . . C1 C 0.0733(5) 0.6433(5) 0.1910(2) 0.0227(8) Uani 1 1 d . . . H1A H 0.0282 0.6015 0.2440 0.039(15) Uiso 1 1 calc R . . H1B H -0.0215 0.6883 0.1657 0.015(10) Uiso 1 1 calc R . . S2 S 0.48461(12) 0.53704(10) 0.18482(6) 0.01944(18) Uani 1 1 d . . . C2 C 0.3255(5) 0.4357(4) 0.1732(2) 0.0228(7) Uani 1 1 d . . . H2A H 0.3807 0.3532 0.1387 0.049(17) Uiso 1 1 calc R . . H2B H 0.2823 0.3964 0.2273 0.044(16) Uiso 1 1 calc R . . S3 S 0.34278(12) 0.71054(11) 0.01580(6) 0.02133(19) Uani 1 1 d . . . C3 C 0.2294(5) 0.5615(4) 0.0454(2) 0.0226(7) Uani 1 1 d . . . H3A H 0.1281 0.5860 0.0223 0.027(13) Uiso 1 1 calc R . . H3B H 0.2981 0.4752 0.0178 0.034(14) Uiso 1 1 calc R . . C31 C 0.1717(6) 0.8565(5) -0.0015(3) 0.0326(10) Uani 1 1 d . . . H31A H 0.2136 0.9444 -0.0179 0.07(2) Uiso 1 1 calc R . . H31B H 0.0891 0.8722 0.0485 0.030(13) Uiso 1 1 calc R . . H31C H 0.1215 0.8304 -0.0443 0.042(16) Uiso 1 1 calc R . . C4 C 0.1766(5) 0.5171(4) 0.1369(2) 0.0200(7) Uani 1 1 d . . . C41 C 0.0602(6) 0.4083(5) 0.1368(3) 0.0320(9) Uani 1 1 d . . . H41A H -0.0358 0.4563 0.1141 0.040(15) Uiso 1 1 calc R . . H41B H 0.0237 0.3745 0.1923 0.030(13) Uiso 1 1 calc R . . H41C H 0.1202 0.3266 0.1037 0.030(13) Uiso 1 1 calc R . . C13 C 0.2702(5) 0.6127(5) 0.3643(3) 0.0256(8) Uani 1 1 d . . . O13 O 0.1947(4) 0.5504(4) 0.4161(2) 0.0382(8) Uani 1 1 d . . . C14 C 0.5799(5) 0.6737(5) 0.3096(3) 0.0254(8) Uani 1 1 d . . . O14 O 0.7079(4) 0.6522(4) 0.3290(2) 0.0410(8) Uani 1 1 d . . . C15 C 0.3292(5) 0.8961(5) 0.3315(2) 0.0239(8) Uani 1 1 d . . . N15 N 0.3018(5) 1.0045(4) 0.3653(2) 0.0328(8) Uani 1 1 d . . . C24 C 0.6462(5) 0.7573(4) 0.0912(2) 0.0228(7) Uani 1 1 d . . . O24 O 0.7865(4) 0.7593(4) 0.0666(2) 0.0332(7) Uani 1 1 d . . . C25 C 0.4013(6) 0.9574(5) 0.1185(3) 0.0292(9) Uani 1 1 d . . . O25 O 0.3873(5) 1.0818(4) 0.1133(3) 0.0526(11) Uani 1 1 d . . . N5 N 0.7584(4) 0.1296(4) 0.3774(2) 0.0218(6) Uani 1 1 d . . . C51 C 0.7237(5) -0.0139(4) 0.4209(2) 0.0242(8) Uani 1 1 d . . . H51A H 0.6796 0.0038 0.4791 0.037(15) Uiso 1 1 calc R . . H51B H 0.6374 -0.0440 0.3983 0.019(11) Uiso 1 1 calc R . . C52 C 0.8749(6) -0.1385(5) 0.4134(3) 0.0312(9) Uani 1 1 d . . . H52A H 0.8425 -0.2239 0.4423 0.08(2) Uiso 1 1 calc R . . H52B H 0.9603 -0.1113 0.4371 0.041(16) Uiso 1 1 calc R . . H52C H 0.9179 -0.1592 0.3562 0.06(2) Uiso 1 1 calc R . . C53 C 0.5911(6) 0.2377(5) 0.3847(3) 0.0299(9) Uani 1 1 d . . . H53A H 0.6064 0.3207 0.3474 0.026(12) Uiso 1 1 calc R . . H53B H 0.5108 0.1909 0.3670 0.031(13) Uiso 1 1 calc R . . C54 C 0.5181(6) 0.2931(5) 0.4711(3) 0.0359(10) Uani 1 1 d . . . H54A H 0.4134 0.3603 0.4708 0.051(17) Uiso 1 1 calc R . . H54B H 0.5952 0.3421 0.4887 0.048(17) Uiso 1 1 calc R . . H54C H 0.4994 0.2122 0.5084 0.042(16) Uiso 1 1 calc R . . C55 C 0.8809(6) 0.1822(5) 0.4190(3) 0.0301(9) Uani 1 1 d . . . H55A H 0.8345 0.1888 0.4777 0.032(14) Uiso 1 1 calc R . . H55B H 0.9842 0.1093 0.4125 0.027(13) Uiso 1 1 calc R . . C56 C 0.9230(9) 0.3282(7) 0.3873(3) 0.0511(16) Uani 1 1 d . . . H56A H 1.0011 0.3523 0.4172 0.047(17) Uiso 1 1 calc R . . H56B H 0.8224 0.4023 0.3950 0.06(2) Uiso 1 1 calc R . . H56C H 0.9724 0.3226 0.3296 0.08(3) Uiso 1 1 calc R . . C57 C 0.8360(7) 0.1068(6) 0.2864(3) 0.0342(10) Uani 1 1 d . . . H57A H 0.8506 0.2007 0.2603 0.025(12) Uiso 1 1 calc R . . H57B H 0.9466 0.0447 0.2824 0.038(15) Uiso 1 1 calc R . . C58 C 0.7342(8) 0.0387(7) 0.2390(3) 0.0434(13) Uani 1 1 d . . . H58A H 0.7911 0.0281 0.1824 0.060(19) Uiso 1 1 calc R . . H58B H 0.6255 0.1006 0.2412 0.057(19) Uiso 1 1 calc R . . H58C H 0.7216 -0.0556 0.2633 0.041(16) 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 0.0183(2) 0.0202(3) 0.0182(2) -0.00384(19) -0.00414(19) -0.0043(2) Fe2 0.0166(2) 0.0142(2) 0.0191(2) -0.00242(18) -0.00301(19) -0.00347(18) S1 0.0164(4) 0.0218(4) 0.0204(4) -0.0071(3) -0.0031(3) -0.0013(3) C1 0.0179(17) 0.030(2) 0.0230(18) -0.0054(15) -0.0040(14) -0.0089(15) S2 0.0203(4) 0.0162(4) 0.0217(4) -0.0026(3) -0.0050(3) -0.0019(3) C2 0.0283(19) 0.0189(17) 0.0230(18) -0.0026(14) -0.0049(15) -0.0085(15) S3 0.0218(4) 0.0254(5) 0.0178(4) -0.0016(3) -0.0024(3) -0.0079(4) C3 0.0252(19) 0.0235(19) 0.0212(17) -0.0051(14) -0.0049(14) -0.0073(15) C31 0.035(2) 0.031(2) 0.035(2) 0.0088(18) -0.0197(19) -0.0039(18) C4 0.0230(17) 0.0203(17) 0.0197(17) -0.0019(13) -0.0025(14) -0.0123(14) C41 0.037(2) 0.036(2) 0.029(2) -0.0030(18) -0.0063(18) -0.021(2) C13 0.027(2) 0.028(2) 0.0233(19) -0.0058(16) -0.0084(16) -0.0048(16) O13 0.0370(18) 0.043(2) 0.0360(18) 0.0062(15) -0.0037(14) -0.0166(15) C14 0.0229(19) 0.0250(19) 0.030(2) -0.0088(16) -0.0058(16) -0.0044(15) O14 0.0264(16) 0.050(2) 0.049(2) -0.0109(17) -0.0150(15) -0.0036(15) C15 0.0232(18) 0.029(2) 0.0208(18) -0.0052(15) -0.0041(14) -0.0078(15) N15 0.0303(19) 0.035(2) 0.035(2) -0.0130(16) -0.0057(16) -0.0082(16) C24 0.0249(19) 0.0215(18) 0.0245(18) -0.0018(14) -0.0090(15) -0.0062(15) O24 0.0205(14) 0.0427(19) 0.0382(18) -0.0031(14) -0.0027(12) -0.0125(13) C25 0.030(2) 0.0216(19) 0.037(2) -0.0014(17) -0.0065(18) -0.0061(16) O25 0.061(3) 0.0175(16) 0.080(3) -0.0008(17) -0.014(2) -0.0091(16) N5 0.0244(16) 0.0243(16) 0.0182(15) -0.0007(12) -0.0021(12) -0.0102(13) C51 0.0256(19) 0.0234(19) 0.0230(18) 0.0001(15) -0.0027(15) -0.0059(15) C52 0.033(2) 0.028(2) 0.032(2) -0.0014(17) -0.0078(18) -0.0024(18) C53 0.034(2) 0.025(2) 0.032(2) 0.0033(17) -0.0114(18) -0.0046(17) C54 0.037(2) 0.026(2) 0.041(3) -0.0061(19) -0.008(2) 0.0044(19) C55 0.029(2) 0.037(2) 0.029(2) -0.0067(18) -0.0053(17) -0.0155(18) C56 0.072(4) 0.056(4) 0.040(3) 0.006(3) -0.015(3) -0.045(3) C57 0.045(3) 0.039(3) 0.0196(19) -0.0017(17) 0.0016(18) -0.019(2) C58 0.056(3) 0.054(3) 0.024(2) -0.007(2) -0.005(2) -0.021(3) _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 C14 1.761(4) . ? Fe1 C13 1.765(4) . ? Fe1 C15 1.941(4) . ? Fe1 S1 2.2412(12) . ? Fe1 S2 2.2486(13) . ? Fe1 Fe2 2.5378(9) . ? Fe2 C24 1.752(4) . ? Fe2 C25 1.761(4) . ? Fe2 S3 2.2547(11) . ? Fe2 S1 2.2599(11) . ? Fe2 S2 2.2646(14) . ? S1 C1 1.827(4) . ? C1 C4 1.532(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? S2 C2 1.826(4) . ? C2 C4 1.518(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? S3 C31 1.805(4) . ? S3 C3 1.826(4) . ? C3 C4 1.541(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C4 C41 1.543(5) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C13 O13 1.153(5) . ? C14 O14 1.145(5) . ? C15 N15 1.152(5) . ? C24 O24 1.156(5) . ? C25 O25 1.144(5) . ? N5 C55 1.514(5) . ? N5 C57 1.523(5) . ? N5 C53 1.525(6) . ? N5 C51 1.530(5) . ? C51 C52 1.514(6) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.517(6) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C56 1.511(7) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C58 1.517(7) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 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 C14 Fe1 C13 100.5(2) . . ? C14 Fe1 C15 89.25(18) . . ? C13 Fe1 C15 97.68(18) . . ? C14 Fe1 S1 160.04(15) . . ? C13 Fe1 S1 99.42(14) . . ? C15 Fe1 S1 87.92(13) . . ? C14 Fe1 S2 88.71(13) . . ? C13 Fe1 S2 104.12(14) . . ? C15 Fe1 S2 158.10(13) . . ? S1 Fe1 S2 86.60(4) . . ? C14 Fe1 Fe2 105.72(15) . . ? C13 Fe1 Fe2 146.04(13) . . ? C15 Fe1 Fe2 103.75(13) . . ? S1 Fe1 Fe2 56.03(3) . . ? S2 Fe1 Fe2 56.08(4) . . ? C24 Fe2 C25 88.4(2) . . ? C24 Fe2 S3 102.79(13) . . ? C25 Fe2 S3 101.90(16) . . ? C24 Fe2 S1 162.84(13) . . ? C25 Fe2 S1 88.99(15) . . ? S3 Fe2 S1 94.34(4) . . ? C24 Fe2 S2 90.75(14) . . ? C25 Fe2 S2 159.35(16) . . ? S3 Fe2 S2 98.42(5) . . ? S1 Fe2 S2 85.78(5) . . ? C24 Fe2 Fe1 109.29(13) . . ? C25 Fe2 Fe1 105.56(16) . . ? S3 Fe2 Fe1 137.85(4) . . ? S1 Fe2 Fe1 55.33(3) . . ? S2 Fe2 Fe1 55.49(4) . . ? C1 S1 Fe1 112.06(14) . . ? C1 S1 Fe2 109.62(13) . . ? Fe1 S1 Fe2 68.64(4) . . ? C4 C1 S1 118.9(3) . . ? C4 C1 H1A 107.6 . . ? S1 C1 H1A 107.6 . . ? C4 C1 H1B 107.6 . . ? S1 C1 H1B 107.6 . . ? H1A C1 H1B 107.0 . . ? C2 S2 Fe1 110.89(14) . . ? C2 S2 Fe2 110.68(14) . . ? Fe1 S2 Fe2 68.43(4) . . ? C4 C2 S2 117.9(3) . . ? C4 C2 H2A 107.8 . . ? S2 C2 H2A 107.8 . . ? C4 C2 H2B 107.8 . . ? S2 C2 H2B 107.8 . . ? H2A C2 H2B 107.2 . . ? C31 S3 C3 100.0(2) . . ? C31 S3 Fe2 107.43(16) . . ? C3 S3 Fe2 107.89(13) . . ? C4 C3 S3 120.9(3) . . ? C4 C3 H3A 107.1 . . ? S3 C3 H3A 107.1 . . ? C4 C3 H3B 107.1 . . ? S3 C3 H3B 107.1 . . ? H3A C3 H3B 106.8 . . ? S3 C31 H31A 109.5 . . ? S3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C2 C4 C1 111.7(3) . . ? C2 C4 C3 111.8(3) . . ? C1 C4 C3 114.1(3) . . ? C2 C4 C41 107.2(3) . . ? C1 C4 C41 106.5(3) . . ? C3 C4 C41 104.9(3) . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O13 C13 Fe1 177.6(4) . . ? O14 C14 Fe1 178.7(4) . . ? N15 C15 Fe1 175.6(4) . . ? O24 C24 Fe2 176.7(4) . . ? O25 C25 Fe2 177.5(5) . . ? C55 N5 C57 108.9(3) . . ? C55 N5 C53 112.2(3) . . ? C57 N5 C53 109.2(3) . . ? C55 N5 C51 107.8(3) . . ? C57 N5 C51 111.0(3) . . ? C53 N5 C51 107.7(3) . . ? C52 C51 N5 114.8(3) . . ? C52 C51 H51A 108.6 . . ? N5 C51 H51A 108.6 . . ? C52 C51 H51B 108.6 . . ? N5 C51 H51B 108.6 . . ? H51A C51 H51B 107.5 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 N5 114.3(4) . . ? C54 C53 H53A 108.7 . . ? N5 C53 H53A 108.7 . . ? C54 C53 H53B 108.7 . . ? N5 C53 H53B 108.7 . . ? H53A C53 H53B 107.6 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 N5 115.5(4) . . ? C56 C55 H55A 108.4 . . ? N5 C55 H55A 108.4 . . ? C56 C55 H55B 108.4 . . ? N5 C55 H55B 108.4 . . ? H55A C55 H55B 107.5 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 N5 114.5(4) . . ? C58 C57 H57A 108.6 . . ? N5 C57 H57A 108.6 . . ? C58 C57 H57B 108.6 . . ? N5 C57 H57B 108.6 . . ? H57A C57 H57B 107.6 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.96 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.694 _refine_diff_density_min -0.817 _refine_diff_density_rms 0.110