Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_math5 _database_code_CSD 161064 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Davies, Sian C.' 'Hughes, David L.' 'Pickett, Christopher J.' 'Razavet, Mathieu' _publ_contact_author_name 'Prof Christopher J Pickett' _publ_contact_author_address ; Prof Christopher J Pickett Department of Biological Chemistry John Innes Centre Norwich NR4 7UH UNITED KINGDOM ; _publ_contact_author_email 'CHRIS.PICKETT@BBSRC.AC.UK' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C17 H16 Fe2 O5 S3' _chemical_formula_structural '[Fe2 (CO)5 {PhCH2SCH2C(Me)(CH2S)2}]' _chemical_formula_analytical ? _chemical_formula_sum 'C17 H16 Fe2 O5 S3' _chemical_formula_weight 508.18 _chemical_melting_point ? _chemical_compound_source ? 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' #(no. 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 ? _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_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 3686 _diffrn_reflns_av_R_equivalents 0.0000 _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_observed 2715 _reflns_observed_criterion 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-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0579P)^2^] 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 3686 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_obs 0.0373 _refine_ls_wR_factor_all 0.1047 _refine_ls_wR_factor_obs 0.0902 _refine_ls_goodness_of_fit_all 1.033 _refine_ls_goodness_of_fit_obs 1.048 _refine_ls_restrained_S_all 1.033 _refine_ls_restrained_S_obs 1.048 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.22416(5) 0.09208(5) 0.24546(5) 0.0505(2) Uani 1 d . . Fe2 Fe 0.48554(5) 0.19468(5) 0.29537(5) 0.0445(2) Uani 1 d . . S1 S 0.37303(10) 0.05117(8) 0.38571(9) 0.0482(2) Uani 1 d . . C1 C 0.3646(4) 0.1343(4) 0.5688(4) 0.0539(9) Uani 1 d . . H1A H 0.2664(4) 0.1109(4) 0.5819(4) 0.065 Uiso 1 calc R . H1B H 0.4159(4) 0.0995(4) 0.6218(4) 0.065 Uiso 1 calc R . C12 C 0.4207(4) 0.2814(4) 0.6316(3) 0.0517(9) Uani 1 d . . C121 C 0.3999(5) 0.3225(5) 0.7870(4) 0.0739(13) Uani 1 d . . H12A H 0.4293(34) 0.4163(5) 0.8309(10) 0.111 Uiso 1 calc R . H12B H 0.4555(29) 0.2867(28) 0.8333(9) 0.111 Uiso 1 calc R . H12C H 0.3018(8) 0.2901(29) 0.7927(4) 0.111 Uiso 1 calc R . S2 S 0.32786(11) 0.30558(9) 0.37748(9) 0.0519(2) Uani 1 d . . C2 C 0.3345(5) 0.3442(4) 0.5646(4) 0.0624(11) Uani 1 d . . H2A H 0.3715(5) 0.4384(4) 0.6116(4) 0.075 Uiso 1 calc R . H2B H 0.2382(5) 0.3199(4) 0.5826(4) 0.075 Uiso 1 calc R . S3 S 0.64995(10) 0.33229(8) 0.47697(9) 0.0480(2) Uani 1 d . . C3 C 0.5790(4) 0.3316(5) 0.6352(4) 0.0697(12) Uani 1 d . . H3A H 0.6238(4) 0.2803(5) 0.6712(4) 0.084 Uiso 1 calc R . H3B H 0.6101(4) 0.4208(5) 0.7028(4) 0.084 Uiso 1 calc R . C31 C 0.7950(4) 0.2647(4) 0.4911(4) 0.0612(10) Uani 1 d . . H31A H 0.7573(4) 0.1772(4) 0.4903(4) 0.073 Uiso 1 calc R . H31B H 0.8424(4) 0.2574(4) 0.4104(4) 0.073 Uiso 1 calc R . C311 C 0.9014(4) 0.3455(4) 0.6204(4) 0.0537(9) Uani 1 d . . C312 C 0.9597(5) 0.4791(4) 0.6583(5) 0.0740(12) Uani 1 d . . H312 H 0.9324(5) 0.5210(4) 0.6033(5) 0.089 Uiso 1 calc R . C313 C 1.0581(5) 0.5506(5) 0.7774(5) 0.0860(15) Uani 1 d . . H313 H 1.0963(5) 0.6403(5) 0.8024(5) 0.103 Uiso 1 calc R . C314 C 1.0994(5) 0.4899(6) 0.8582(5) 0.0812(14) Uani 1 d . . H314 H 1.1679(5) 0.5376(6) 0.9364(5) 0.097 Uiso 1 calc R . C315 C 1.0409(5) 0.3608(6) 0.8246(5) 0.0837(14) Uani 1 d . . H315 H 1.0663(5) 0.3202(6) 0.8818(5) 0.100 Uiso 1 calc R . C316 C 0.9425(4) 0.2881(5) 0.7046(5) 0.0683(11) Uani 1 d . . H316 H 0.9041(4) 0.1987(5) 0.6814(5) 0.082 Uiso 1 calc R . C13 C 0.0604(5) 0.0553(4) 0.3073(5) 0.0707(12) Uani 1 d . . O13 O -0.0452(4) 0.0306(4) 0.3465(5) 0.1119(13) Uani 1 d . . C14 C 0.1721(5) 0.1447(5) 0.1128(5) 0.0766(13) Uani 1 d . . O14 O 0.1400(5) 0.1770(4) 0.0275(4) 0.121(2) Uani 1 d . . C15 C 0.2186(4) -0.0629(4) 0.1179(4) 0.0645(11) Uani 1 d . . O15 O 0.2186(4) -0.1609(3) 0.0380(4) 0.1012(12) Uani 1 d . . C24 C 0.5185(4) 0.2744(4) 0.1774(4) 0.0622(10) Uani 1 d . . O24 O 0.5368(4) 0.3234(3) 0.0979(3) 0.0931(11) Uani 1 d . . C25 C 0.5690(4) 0.0777(4) 0.2013(4) 0.0586(10) Uani 1 d . . O25 O 0.6193(4) -0.0011(4) 0.1396(3) 0.0918(10) Uani 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) 0.029(2) 0.016(2) 0.024(2) C12 0.064(2) 0.058(2) 0.040(2) 0.019(2) 0.013(2) 0.026(2) C121 0.097(3) 0.092(3) 0.046(2) 0.027(2) 0.026(2) 0.044(3) 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) 0.017(2) 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) 0.040(2) 0.020(2) -0.001(2) 0.004(2) C31 0.060(2) 0.046(2) 0.067(2) 0.011(2) -0.004(2) 0.017(2) C311 0.047(2) 0.055(2) 0.056(2) 0.017(2) 0.004(2) 0.016(2) 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) 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) 0.008(2) 0.007(2) O15 0.117(3) 0.063(2) 0.087(2) -0.006(2) 0.023(2) 0.011(2) C24 0.072(3) 0.058(2) 0.045(2) 0.015(2) 0.003(2) 0.007(2) O24 0.126(3) 0.093(2) 0.064(2) 0.048(2) 0.012(2) 0.010(2) C25 0.063(2) 0.067(3) 0.047(2) 0.021(2) 0.013(2) 0.020(2) O25 0.114(3) 0.099(3) 0.076(2) 0.025(2) 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 C12 1.507(5) . ? C1 H1A 0.97 . ? C1 H1B 0.97 . ? C12 C3 1.519(6) . ? C12 C2 1.521(5) . ? C12 C121 1.556(5) . ? C121 H12A 0.96 . ? C121 H12B 0.96 . ? C121 H12C 0.96 . ? S2 C2 1.830(4) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? S3 C31 1.808(4) . ? S3 C3 1.822(4) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C31 C311 1.504(5) . ? C31 H31A 0.97 . ? C31 H31B 0.97 . ? C311 C316 1.360(6) . ? C311 C312 1.387(6) . ? C312 C313 1.383(6) . ? C312 H312 0.93 . ? C313 C314 1.364(7) . ? C313 H313 0.93 . ? C314 C315 1.346(7) . ? C314 H314 0.93 . ? C315 C316 1.391(6) . ? C315 H315 0.93 . ? C316 H316 0.93 . ? 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 102.8(2) . . ? C15 Fe1 S1 86.59(15) . . ? C14 Fe1 S1 157.1(2) . . ? C13 Fe1 S2 104.02(15) . . ? C15 Fe1 S2 154.12(14) . . ? C14 Fe1 S2 87.2(2) . . ? S1 Fe1 S2 85.49(4) . . ? C13 Fe1 Fe2 149.39(15) . . ? C15 Fe1 Fe2 99.04(13) . . ? C14 Fe1 Fe2 101.9(2) . . ? S1 Fe1 Fe2 56.27(3) . . ? S2 Fe1 Fe2 56.43(3) . . ? C24 Fe2 C25 90.2(2) . . ? 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) . . ? C12 C1 S1 118.3(3) . . ? C12 C1 H1A 107.7(2) . . ? S1 C1 H1A 107.75(13) . . ? C12 C1 H1B 107.7(2) . . ? S1 C1 H1B 107.75(12) . . ? H1A C1 H1B 107.1 . . ? C1 C12 C3 113.5(3) . . ? C1 C12 C2 111.0(3) . . ? C3 C12 C2 113.4(3) . . ? C1 C12 C121 106.1(3) . . ? C3 C12 C121 104.9(3) . . ? C2 C12 C121 107.3(3) . . ? C12 C121 H12A 109.5(2) . . ? C12 C121 H12B 109.5(2) . . ? H12A C121 H12B 109.5 . . ? C12 C121 H12C 109.5(2) . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C2 S2 Fe2 110.12(13) . . ? C2 S2 Fe1 113.84(15) . . ? Fe2 S2 Fe1 67.05(3) . . ? C12 C2 S2 118.0(2) . . ? C12 C2 H2A 107.8(2) . . ? S2 C2 H2A 107.81(14) . . ? C12 C2 H2B 107.8(2) . . ? S2 C2 H2B 107.81(15) . . ? H2A C2 H2B 107.1 . . ? C31 S3 C3 99.8(2) . . ? C31 S3 Fe2 110.66(13) . . ? C3 S3 Fe2 108.02(13) . . ? C12 C3 S3 120.3(3) . . ? C12 C3 H3A 107.2(2) . . ? S3 C3 H3A 107.2(2) . . ? C12 C3 H3B 107.2(2) . . ? S3 C3 H3B 107.24(15) . . ? H3A C3 H3B 106.9 . . ? C311 C31 S3 113.3(3) . . ? C311 C31 H31A 108.9(2) . . ? S3 C31 H31A 108.91(13) . . ? C311 C31 H31B 108.9(2) . . ? S3 C31 H31B 108.91(14) . . ? 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(3) . . ? C311 C312 H312 119.8(2) . . ? C314 C313 C312 120.2(5) . . ? C314 C313 H313 119.9(3) . . ? C312 C313 H313 119.9(3) . . ? C315 C314 C313 120.0(4) . . ? C315 C314 H314 120.0(3) . . ? C313 C314 H314 120.0(3) . . ? C314 C315 C316 120.1(5) . . ? C314 C315 H315 119.9(3) . . ? C316 C315 H315 119.9(3) . . ? C311 C316 C315 121.2(5) . . ? C311 C316 H316 119.4(2) . . ? C315 C316 H316 119.4(3) . . ? 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) . . ? _refine_diff_density_max 0.437 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.069