# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Tatyana Roudneva' _publ_contact_author_email RUTA@ICP.AC.RU _publ_section_title ; Structure and Properties of Binuclear Nitrosyl Iron Complex with Benzimidazole-2-Thiolyl ; loop_ _publ_author_name 'Tatyana Roudneva' 'Sergey M Aldoshin' 'Evgeniya V Kurganova' 'Roman B Morgunov' ; N.Ovanesyan ; 'Nataliya Sanina' 'Gennadii V Shilov' # Attachment 'nit200.cif' data_nit200 _database_code_depnum_ccdc_archive 'CCDC 665846' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C14H10Fe2N8O4S2,2(C3H6O3) _chemical_formula_sum 'C20 H22 Fe2 N8 O6 S2' _chemical_formula_weight 646.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7370(10) _cell_length_b 9.0720(10) _cell_length_c 9.0830(10) _cell_angle_alpha 74.820(10) _cell_angle_beta 73.100(10) _cell_angle_gamma 86.620(10) _cell_volume 664.70(13) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description parallelepiped _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 330 _exptl_absorpt_coefficient_mu 1.300 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 P4 _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2572 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2080 _reflns_number_gt 1884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS v2.2, 1995' _computing_cell_refinement 'XSCANS v2.2, 1995' _computing_data_reduction 'XSCANS v2.2, 1995' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0409P)^2^+0.3425P] 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 2080 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 0.12720(4) 0.15080(3) -0.20021(4) 0.02552(13) Uani 1 1 d . . . S3 S 0.23995(7) 0.06132(6) 0.00553(7) 0.02831(17) Uani 1 1 d . . . N3 N -0.0400(2) 0.0265(2) 0.2495(2) 0.0250(4) Uani 1 1 d . . . C1 C 0.0965(3) 0.1043(2) 0.1654(3) 0.0242(5) Uani 1 1 d . . . O3 O 0.3670(2) 0.42859(19) 0.1763(2) 0.0341(4) Uani 1 1 d . . . N4 N 0.1140(2) 0.2230(2) 0.2240(2) 0.0269(4) Uani 1 1 d . . . H1 H 0.1931 0.2873 0.1865 0.032 Uiso 1 1 calc R . . C2 C -0.0156(3) 0.2240(3) 0.3533(3) 0.0259(5) Uani 1 1 d . . . N2 N 0.2747(3) 0.2340(2) -0.3634(2) 0.0333(5) Uani 1 1 d . . . O2 O 0.3559(3) 0.3269(2) -0.4678(2) 0.0570(6) Uani 1 1 d . . . C7 C -0.0564(3) 0.3197(3) 0.4546(3) 0.0343(6) Uani 1 1 d . . . H7 H 0.0091 0.4021 0.4414 0.041 Uiso 1 1 calc R . . C3 C -0.1131(3) 0.0997(2) 0.3706(3) 0.0252(5) Uani 1 1 d . . . O1 O -0.0649(3) 0.3921(2) -0.1114(3) 0.0602(6) Uani 1 1 d . . . C4 C -0.2544(3) 0.0679(3) 0.4935(3) 0.0314(6) Uani 1 1 d . . . H4 H -0.3202 -0.0145 0.5070 0.038 Uiso 1 1 calc R . . N1 N -0.0042(3) 0.2808(2) -0.1390(2) 0.0318(5) Uani 1 1 d . . . C8 C 0.5025(3) 0.3883(3) 0.1776(3) 0.0300(6) Uani 1 1 d . . . C6 C -0.1977(3) 0.2883(3) 0.5758(3) 0.0369(6) Uani 1 1 d . . . H6 H -0.2288 0.3511 0.6451 0.044 Uiso 1 1 calc R . . C5 C -0.2941(3) 0.1637(3) 0.5958(3) 0.0348(6) Uani 1 1 d . . . H5 H -0.3877 0.1440 0.6797 0.042 Uiso 1 1 calc R . . C9 C 0.6159(3) 0.4895(3) 0.2032(3) 0.0426(7) Uani 1 1 d . . . H9A H 0.7150 0.4988 0.1202 0.064 Uiso 1 1 calc R . . H9B H 0.6351 0.4460 0.3044 0.064 Uiso 1 1 calc R . . H9C H 0.5703 0.5886 0.2014 0.064 Uiso 1 1 calc R . . C10 C 0.5617(4) 0.2369(3) 0.1528(4) 0.0470(7) Uani 1 1 d . . . H10A H 0.6108 0.1867 0.2341 0.070 Uiso 1 1 calc R . . H10B H 0.6388 0.2509 0.0502 0.070 Uiso 1 1 calc R . . H10C H 0.4736 0.1754 0.1581 0.070 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 0.0282(3) 0.02501(19) 0.02547(19) -0.01051(13) -0.00638(16) -0.00420(14) S3 0.0261(4) 0.0327(3) 0.0293(3) -0.0141(2) -0.0074(3) 0.0010(2) N3 0.0255(12) 0.0262(9) 0.0265(9) -0.0114(8) -0.0078(9) -0.0015(8) C1 0.0261(15) 0.0246(10) 0.0272(11) -0.0111(9) -0.0122(11) 0.0021(10) O3 0.0293(11) 0.0348(9) 0.0397(10) -0.0125(7) -0.0089(9) -0.0033(8) N4 0.0280(12) 0.0240(9) 0.0317(10) -0.0111(8) -0.0087(9) -0.0042(8) C2 0.0281(14) 0.0268(11) 0.0268(11) -0.0095(9) -0.0117(11) 0.0019(9) N2 0.0366(14) 0.0361(11) 0.0288(11) -0.0121(9) -0.0069(10) -0.0082(10) O2 0.0657(16) 0.0609(13) 0.0338(10) -0.0073(10) 0.0030(11) -0.0264(12) C7 0.0411(17) 0.0307(12) 0.0384(13) -0.0174(10) -0.0156(13) 0.0033(11) C3 0.0299(15) 0.0258(11) 0.0244(11) -0.0100(9) -0.0115(11) 0.0026(10) O1 0.0590(15) 0.0458(12) 0.0754(15) -0.0270(11) -0.0121(12) 0.0198(11) C4 0.0306(16) 0.0350(13) 0.0301(12) -0.0106(10) -0.0084(12) -0.0014(11) N1 0.0305(13) 0.0317(11) 0.0335(11) -0.0089(9) -0.0091(10) -0.0008(9) C8 0.0330(17) 0.0340(12) 0.0220(11) -0.0062(9) -0.0057(11) -0.0075(11) C6 0.0452(18) 0.0384(13) 0.0342(13) -0.0196(11) -0.0150(13) 0.0108(12) C5 0.0330(16) 0.0435(14) 0.0290(12) -0.0142(11) -0.0070(12) 0.0056(11) C9 0.0389(18) 0.0499(16) 0.0432(15) -0.0150(12) -0.0130(14) -0.0131(13) C10 0.0400(19) 0.0407(15) 0.0672(19) -0.0204(14) -0.0210(16) 0.0070(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 Fe1 N1 1.682(2) . ? Fe1 N2 1.687(2) . ? Fe1 N3 2.0214(18) 2 ? Fe1 S3 2.3029(7) . ? S3 C1 1.736(2) . ? N3 C1 1.339(3) . ? N3 C3 1.409(3) . ? N3 Fe1 2.0215(18) 2 ? C1 N4 1.354(3) . ? O3 C8 1.221(3) . ? N4 C2 1.376(3) . ? N4 H1 0.8600 . ? C2 C7 1.385(3) . ? C2 C3 1.401(3) . ? N2 O2 1.172(3) . ? C7 C6 1.380(4) . ? C7 H7 0.9300 . ? C3 C4 1.387(4) . ? O1 N1 1.164(3) . ? C4 C5 1.393(3) . ? C4 H4 0.9300 . ? C8 C10 1.489(4) . ? C8 C9 1.493(3) . ? C6 C5 1.391(4) . ? C6 H6 0.9300 . ? C5 H5 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 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 N1 Fe1 N2 111.06(10) . . ? N1 Fe1 N3 117.33(9) . 2 ? N2 Fe1 N3 106.92(9) . 2 ? N1 Fe1 S3 103.91(7) . . ? N2 Fe1 S3 107.53(7) . . ? N3 Fe1 S3 109.73(6) 2 . ? C1 S3 Fe1 102.47(8) . . ? C1 N3 C3 105.97(17) . . ? C1 N3 Fe1 126.11(14) . 2 ? C3 N3 Fe1 127.81(16) . 2 ? N3 C1 N4 111.1(2) . . ? N3 C1 S3 126.46(16) . . ? N4 C1 S3 122.41(19) . . ? C1 N4 C2 108.7(2) . . ? C1 N4 H1 125.6 . . ? C2 N4 H1 125.6 . . ? N4 C2 C7 132.1(2) . . ? N4 C2 C3 105.84(19) . . ? C7 C2 C3 122.0(2) . . ? O2 N2 Fe1 161.6(2) . . ? C6 C7 C2 117.6(2) . . ? C6 C7 H7 121.2 . . ? C2 C7 H7 121.2 . . ? C4 C3 C2 120.1(2) . . ? C4 C3 N3 131.5(2) . . ? C2 C3 N3 108.3(2) . . ? C3 C4 C5 117.6(2) . . ? C3 C4 H4 121.2 . . ? C5 C4 H4 121.2 . . ? O1 N1 Fe1 164.6(2) . . ? O3 C8 C10 121.4(2) . . ? O3 C8 C9 121.3(2) . . ? C10 C8 C9 117.3(2) . . ? C7 C6 C5 120.8(2) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C5 C4 121.8(2) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.889 _refine_diff_density_max 0.289 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.052