# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'M. Schroder' 'Alexander Blake' 'E. Stephen Davies' 'Jonathan McMaster' 'Alessandro Perra ' 'Qiang Wang.' 'Claire Wilson ' _publ_contact_author_name 'Prof M Schroder' _publ_contact_author_email M.SCHRODER@NOTTINGHAM.AC.UK _publ_section_title ; Unusual Formation of a [NiSFe2(CO)6] Cluster: A Structural Benchmark for the Inactive Form of [NiFe] Hydrogenase. ; # Attachment 'NIS5FE.CIF' data_nis5fe _database_code_depnum_ccdc_archive 'CCDC 698961' _refine_special_details ; The largest residual peak of electron density was found in the region of C8, suggesting disorder. However, disorder modelling involving split atomic sites for C8 and S3 resulted in coalescence of the disorder components, so a dynamic disorder model was adopted. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H12 Fe2 Ni O6 S4' _chemical_formula_sum 'C16 H12 Fe2 Ni O6 S4' _chemical_formula_weight 598.91 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' Ni Ni 0.3393 1.1124 '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' 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 8.1413(5) _cell_length_b 13.3463(8) _cell_length_c 18.9231(11) _cell_angle_alpha 90.00 _cell_angle_beta 92.527(1) _cell_angle_gamma 90.00 _cell_volume 2054.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7248 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.937 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 2.739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.818 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17717 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_av_sigmaI/netI 0.019 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.52 _reflns_number_total 4731 _reflns_number_gt 4251 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36A (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)' _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^)+(0.038P)^2^+2.278P] 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 4731 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 1.07 _refine_ls_restrained_S_all 1.07 _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 Ni1 Ni 0.65006(4) 0.76652(2) 0.036480(16) 0.01952(8) Uani 1 1 d . . . Fe1 Fe 0.50316(4) 0.65959(3) 0.124403(18) 0.01951(9) Uani 1 1 d . . . Fe2 Fe 0.70578(4) 0.79130(3) 0.167373(18) 0.02243(9) Uani 1 1 d . . . S1 S 0.85202(7) 0.66778(4) 0.00288(3) 0.02124(13) Uani 1 1 d . . . S2 S 0.49910(8) 0.74038(5) -0.06441(3) 0.02876(15) Uani 1 1 d . . . S3 S 0.77114(10) 0.90519(5) -0.01172(4) 0.03472(17) Uani 1 1 d . . . S4 S 0.47278(8) 0.81992(5) 0.10973(3) 0.02280(13) Uani 1 1 d . . . O1 O 0.2721(3) 0.56464(17) 0.02151(12) 0.0469(6) Uani 1 1 d . . . O2 O 0.3271(3) 0.62912(16) 0.25373(10) 0.0373(5) Uani 1 1 d . . . O3 O 0.7273(3) 0.49013(16) 0.14974(13) 0.0429(5) Uani 1 1 d . . . O4 O 0.6582(3) 0.74897(16) 0.31660(10) 0.0367(5) Uani 1 1 d . . . O5 O 1.0014(3) 0.66672(19) 0.16647(12) 0.0476(6) Uani 1 1 d . . . O6 O 0.8519(4) 0.99237(18) 0.17429(14) 0.0599(7) Uani 1 1 d . . . C1 C 0.7946(3) 0.64682(18) -0.08805(13) 0.0217(5) Uani 1 1 d . . . C2 C 0.6448(3) 0.68005(17) -0.11774(13) 0.0211(5) Uani 1 1 d . . . C3 C 0.6045(3) 0.6616(2) -0.18867(14) 0.0276(5) Uani 1 1 d . . . H3A H 0.5013 0.6829 -0.2088 0.033 Uiso 1 1 calc R . . C4 C 0.7148(4) 0.6122(2) -0.23002(14) 0.0315(6) Uani 1 1 d . . . H4A H 0.6888 0.6017 -0.2789 0.038 Uiso 1 1 calc R . . C5 C 0.8623(4) 0.5781(2) -0.20043(15) 0.0312(6) Uani 1 1 d . . . H5A H 0.9373 0.5438 -0.2290 0.037 Uiso 1 1 calc R . . C6 C 0.9012(3) 0.5935(2) -0.12954(14) 0.0277(5) Uani 1 1 d . . . H6A H 1.0011 0.5677 -0.1090 0.033 Uiso 1 1 calc R . . C7 C 1.0181(3) 0.7583(2) -0.00673(15) 0.0305(6) Uani 1 1 d . . . H7A H 1.0653 0.7756 0.0408 0.037 Uiso 1 1 calc R . . H7B H 1.1060 0.7266 -0.0335 0.037 Uiso 1 1 calc R . . C8 C 0.9640(4) 0.8530(2) -0.0439(2) 0.0489(9) Uani 1 1 d . . . H8A H 0.9490 0.8392 -0.0952 0.059 Uiso 1 1 calc R . . H8B H 1.0521 0.9038 -0.0375 0.059 Uiso 1 1 calc R . . C9 C 0.6544(5) 0.9165(2) -0.09802(16) 0.0528(10) Uani 1 1 d . . . H9A H 0.6374 0.9884 -0.1089 0.063 Uiso 1 1 calc R . . H9B H 0.7211 0.8876 -0.1355 0.063 Uiso 1 1 calc R . . C10 C 0.4917(5) 0.8655(2) -0.09969(16) 0.0464(9) Uani 1 1 d . . . H10A H 0.4474 0.8628 -0.1492 0.056 Uiso 1 1 calc R . . H10B H 0.4147 0.9058 -0.0723 0.056 Uiso 1 1 calc R . . C11 C 0.3607(3) 0.6022(2) 0.06215(14) 0.0286(5) Uani 1 1 d . . . C12 C 0.3944(3) 0.63886(19) 0.20226(13) 0.0251(5) Uani 1 1 d . . . C13 C 0.6421(3) 0.5573(2) 0.13856(14) 0.0273(5) Uani 1 1 d . . . C14 C 0.6738(3) 0.7688(2) 0.25845(14) 0.0267(5) Uani 1 1 d . . . C15 C 0.8852(3) 0.7155(2) 0.16670(14) 0.0311(6) Uani 1 1 d . . . C16 C 0.7944(4) 0.9140(2) 0.17149(16) 0.0362(6) 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 Ni1 0.02084(15) 0.02138(16) 0.01654(15) 0.00148(11) 0.00303(11) 0.00124(11) Fe1 0.01936(17) 0.02059(17) 0.01875(17) 0.00104(13) 0.00267(13) 0.00051(12) Fe2 0.02510(18) 0.02350(18) 0.01857(17) -0.00171(14) -0.00034(14) -0.00090(14) S1 0.0192(3) 0.0241(3) 0.0205(3) 0.0012(2) 0.0013(2) 0.0012(2) S2 0.0258(3) 0.0405(4) 0.0199(3) -0.0008(3) -0.0004(2) 0.0111(3) S3 0.0436(4) 0.0220(3) 0.0398(4) 0.0048(3) 0.0156(3) -0.0003(3) S4 0.0250(3) 0.0223(3) 0.0214(3) -0.0003(2) 0.0037(2) 0.0057(2) O1 0.0588(14) 0.0411(12) 0.0391(12) 0.0046(10) -0.0170(11) -0.0194(11) O2 0.0427(12) 0.0425(12) 0.0277(10) 0.0014(9) 0.0139(9) -0.0027(9) O3 0.0356(11) 0.0357(11) 0.0581(14) 0.0127(10) 0.0109(10) 0.0135(9) O4 0.0402(12) 0.0471(12) 0.0227(10) 0.0017(9) 0.0017(8) 0.0017(9) O5 0.0320(11) 0.0661(16) 0.0439(13) -0.0124(11) -0.0063(10) 0.0147(11) O6 0.0775(18) 0.0363(13) 0.0638(17) 0.0077(12) -0.0207(14) -0.0220(12) C1 0.0245(12) 0.0194(11) 0.0212(11) 0.0009(9) 0.0026(9) -0.0032(9) C2 0.0230(11) 0.0183(11) 0.0223(11) 0.0012(9) 0.0052(9) 0.0008(9) C3 0.0314(13) 0.0297(13) 0.0216(12) 0.0005(10) 0.0002(10) -0.0020(10) C4 0.0402(15) 0.0308(14) 0.0237(12) -0.0041(11) 0.0055(11) -0.0058(12) C5 0.0361(15) 0.0292(13) 0.0291(13) -0.0074(11) 0.0108(11) -0.0013(11) C6 0.0251(12) 0.0268(13) 0.0317(13) -0.0034(10) 0.0061(11) 0.0004(10) C7 0.0216(12) 0.0358(14) 0.0346(14) -0.0057(12) 0.0051(11) -0.0067(10) C8 0.0446(18) 0.0405(17) 0.064(2) 0.0017(16) 0.0252(17) -0.0081(14) C9 0.108(3) 0.0258(15) 0.0263(15) 0.0109(12) 0.0202(17) 0.0157(17) C10 0.075(2) 0.0353(16) 0.0285(15) 0.0048(13) -0.0038(15) 0.0274(16) C11 0.0324(14) 0.0266(13) 0.0268(13) 0.0064(11) 0.0019(11) -0.0032(11) C12 0.0254(12) 0.0247(12) 0.0251(12) -0.0009(10) 0.0012(10) 0.0008(10) C13 0.0250(12) 0.0309(13) 0.0268(13) 0.0030(11) 0.0078(10) 0.0002(10) C14 0.0246(13) 0.0284(13) 0.0269(13) -0.0038(10) -0.0009(10) 0.0010(10) C15 0.0283(14) 0.0405(15) 0.0241(13) -0.0052(11) -0.0029(11) -0.0014(12) C16 0.0427(16) 0.0331(15) 0.0319(14) 0.0018(12) -0.0081(13) -0.0054(13) _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 Ni1 S4 2.1654(7) . ? Ni1 S1 2.2218(7) . ? Ni1 S2 2.2517(7) . ? Ni1 S3 2.3039(7) . ? Ni1 Fe2 2.5201(5) . ? Ni1 Fe1 2.5319(5) . ? Fe1 C12 1.774(3) . ? Fe1 C13 1.786(3) . ? Fe1 C11 1.789(3) . ? Fe1 S4 2.1705(7) . ? Fe1 Fe2 2.5207(5) . ? Fe2 C15 1.778(3) . ? Fe2 C14 1.780(3) . ? Fe2 C16 1.790(3) . ? Fe2 S4 2.1799(7) . ? S1 C1 1.785(2) . ? S1 C7 1.828(3) . ? S2 C2 1.783(2) . ? S2 C10 1.798(3) . ? S3 C8 1.846(3) . ? S3 C9 1.859(4) . ? O1 C11 1.146(3) . ? O2 C12 1.146(3) . ? O3 C13 1.147(3) . ? O4 C14 1.144(3) . ? O5 C15 1.148(4) . ? O6 C16 1.147(4) . ? C1 C6 1.392(4) . ? C1 C2 1.392(3) . ? C2 C3 1.390(3) . ? C3 C4 1.384(4) . ? C4 C5 1.380(4) . ? C5 C6 1.380(4) . ? C7 C8 1.503(4) . ? C9 C10 1.489(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S4 Ni1 S1 154.28(3) . . ? S4 Ni1 S2 103.85(3) . . ? S1 Ni1 S2 92.79(3) . . ? S4 Ni1 S3 107.33(3) . . ? S1 Ni1 S3 91.62(3) . . ? S2 Ni1 S3 90.91(3) . . ? S4 Ni1 Fe2 54.82(2) . . ? S1 Ni1 Fe2 104.81(2) . . ? S2 Ni1 Fe2 157.15(2) . . ? S3 Ni1 Fe2 102.83(2) . . ? S4 Ni1 Fe1 54.367(19) . . ? S1 Ni1 Fe1 103.34(2) . . ? S2 Ni1 Fe1 102.35(2) . . ? S3 Ni1 Fe1 159.33(2) . . ? Fe2 Ni1 Fe1 59.860(13) . . ? C12 Fe1 C13 95.29(12) . . ? C12 Fe1 C11 98.47(12) . . ? C13 Fe1 C11 99.17(13) . . ? C12 Fe1 S4 101.64(8) . . ? C13 Fe1 S4 147.24(9) . . ? C11 Fe1 S4 105.72(9) . . ? C12 Fe1 Fe2 100.63(8) . . ? C13 Fe1 Fe2 94.80(9) . . ? C11 Fe1 Fe2 155.13(8) . . ? S4 Fe1 Fe2 54.76(2) . . ? C12 Fe1 Ni1 154.33(8) . . ? C13 Fe1 Ni1 102.43(8) . . ? C11 Fe1 Ni1 96.89(8) . . ? S4 Fe1 Ni1 54.177(19) . . ? Fe2 Fe1 Ni1 59.838(13) . . ? C15 Fe2 C14 93.81(12) . . ? C15 Fe2 C16 101.01(14) . . ? C14 Fe2 C16 100.82(13) . . ? C15 Fe2 S4 142.52(9) . . ? C14 Fe2 S4 110.67(9) . . ? C16 Fe2 S4 101.64(10) . . ? C15 Fe2 Ni1 91.76(9) . . ? C14 Fe2 Ni1 154.42(9) . . ? C16 Fe2 Ni1 102.57(10) . . ? S4 Fe2 Ni1 54.283(19) . . ? C15 Fe2 Fe1 97.31(9) . . ? C14 Fe2 Fe1 94.21(9) . . ? C16 Fe2 Fe1 155.36(10) . . ? S4 Fe2 Fe1 54.42(2) . . ? Ni1 Fe2 Fe1 60.302(13) . . ? C1 S1 C7 99.85(12) . . ? C1 S1 Ni1 101.71(8) . . ? C7 S1 Ni1 101.34(9) . . ? C2 S2 C10 102.80(14) . . ? C2 S2 Ni1 101.41(8) . . ? C10 S2 Ni1 100.32(12) . . ? C8 S3 C9 98.63(18) . . ? C8 S3 Ni1 102.27(11) . . ? C9 S3 Ni1 101.63(12) . . ? Ni1 S4 Fe1 71.46(2) . . ? Ni1 S4 Fe2 70.90(2) . . ? Fe1 S4 Fe2 70.82(2) . . ? C6 C1 C2 119.5(2) . . ? C6 C1 S1 118.7(2) . . ? C2 C1 S1 121.78(19) . . ? C3 C2 C1 119.9(2) . . ? C3 C2 S2 119.44(19) . . ? C1 C2 S2 120.54(19) . . ? C4 C3 C2 119.9(3) . . ? C5 C4 C3 120.2(3) . . ? C4 C5 C6 120.3(2) . . ? C5 C6 C1 120.1(3) . . ? C8 C7 S1 113.6(2) . . ? C7 C8 S3 113.5(2) . . ? C10 C9 S3 113.7(2) . . ? C9 C10 S2 113.7(2) . . ? O1 C11 Fe1 178.6(3) . . ? O2 C12 Fe1 177.1(2) . . ? O3 C13 Fe1 177.2(2) . . ? O4 C14 Fe2 175.8(2) . . ? O5 C15 Fe2 179.8(3) . . ? O6 C16 Fe2 179.7(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.20 _refine_diff_density_min -0.51 _refine_diff_density_rms 0.09 #===END of CIF