#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2014623.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2014623 loop_ _publ_author_name 'Dale, Sophie H.' 'Elsegood, Mark R. J.' 'Holmes, Kathryn E.' 'Kelly, Paul F.' _publ_section_title ; The effect of hydrogen-bonding anions on the structure of metal--sulfimide complexes ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m34 _journal_page_last m39 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Fe (C12 H11 N S)6] Cl3' _chemical_formula_moiety 'C72 H66 Fe N6 S6 3+, 3Cl -' _chemical_formula_sum 'C72 H66 Cl3 Fe N6 S6' _chemical_formula_weight 1369.93 _chemical_name_systematic ; hexakis(S,S-diphenylsulfimide)iron(III) trichloride ; _space_group_IT_number 205 _symmetry_cell_setting cubic _symmetry_space_group_name_Hall '-P 2ac 2ab 3' _symmetry_space_group_name_H-M 'P a -3' _atom_sites_solution_hydrogens 'placed geometrically except NH which were refined with restraints' _atom_sites_solution_primary direct _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 18.8566(4) _cell_length_b 18.8566(4) _cell_length_c 18.8566(4) _cell_measurement_reflns_used 28769 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 2.91 _cell_volume 6704.9(2) _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)' _computing_data_collection 'COLLECT, (Hooft, 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)' _computing_molecular_graphics SHELXTL _computing_publication_material 'SHELXTL and local programs' _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 2000)' _diffrn_ambient_temperature 120(2) _diffrn_detector_area_resol_mean 9.091 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Nonius KappaCCD area-detector' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enraf Nonius FR591 rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.133 _diffrn_reflns_av_sigmaI/netI 0.048 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 64482 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_min 3.06 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.579 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_correction_T_min 0.942 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SORTAV; Blessing, 1995)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'prism ## AUTHOR: what shape of prism?' _exptl_crystal_F_000 2852 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.66 _refine_diff_density_min -0.89 _refine_ls_extinction_coef 0.0011(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 138 _refine_ls_number_reflns 2572 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0462 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.052P)^2^+4.568P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1010 _refine_ls_wR_factor_ref 0.1131 _reflns_number_gt 1840 _reflns_number_total 2572 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bm1594.cif _[local]_cod_data_source_block II _cod_depositor_comments ; The following automatic conversions were performed: '_geom_bond_publ_flag' value 'Y' changed to 'y' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_angle_publ_flag' value 'Y' changed to 'y' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2014623 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Fe1 0.0000 0.5000 0.5000 0.0180(2) Uani d S 1 Fe N1 0.03185(11) 0.57209(11) 0.42297(11) 0.0220(5) Uani d . 1 N H1A -0.0004(17) 0.5942(16) 0.4034(16) 0.033 Uiso d . 1 H S1 0.10695(3) 0.60826(3) 0.41344(3) 0.02230(18) Uani d . 1 S C1 0.12315(14) 0.61979(13) 0.32077(13) 0.0256(5) Uani d . 1 C C2 0.06855(15) 0.63534(14) 0.27394(14) 0.0313(6) Uani d . 1 C H2 0.0215 0.6423 0.2906 0.038 Uiso calc R 1 H C3 0.08410(18) 0.64050(16) 0.20221(15) 0.0412(7) Uani d . 1 C H3 0.0475 0.6508 0.1692 0.049 Uiso calc R 1 H C4 0.15299(19) 0.63060(16) 0.17889(16) 0.0445(8) Uani d . 1 C H4 0.1631 0.6340 0.1296 0.053 Uiso calc R 1 H C5 0.20720(18) 0.61597(16) 0.22546(17) 0.0433(8) Uani d . 1 C H5 0.2544 0.6103 0.2087 0.052 Uiso calc R 1 H C6 0.19204(15) 0.60964(15) 0.29753(15) 0.0341(6) Uani d . 1 C H6 0.2286 0.5985 0.3303 0.041 Uiso calc R 1 H C7 0.10215(13) 0.69942(13) 0.44071(13) 0.0237(5) Uani d . 1 C C8 0.16229(14) 0.74159(14) 0.43413(14) 0.0315(6) Uani d . 1 C H8 0.2041 0.7232 0.4129 0.038 Uiso calc R 1 H C9 0.16052(15) 0.81049(15) 0.45880(15) 0.0346(6) Uani d . 1 C H9 0.2014 0.8396 0.4547 0.042 Uiso calc R 1 H C10 0.09977(16) 0.83715(14) 0.48932(14) 0.0338(6) Uani d . 1 C H10 0.0987 0.8847 0.5058 0.041 Uiso calc R 1 H C11 0.04041(15) 0.79486(14) 0.49594(14) 0.0310(6) Uani d . 1 C H11 -0.0013 0.8135 0.5173 0.037 Uiso calc R 1 H C12 0.04108(13) 0.72533(13) 0.47173(13) 0.0264(6) Uani d . 1 C H12 0.0003 0.6961 0.4764 0.032 Uiso calc R 1 H Cl1 -0.12579(3) 0.62579(3) 0.37421(3) 0.0303(3) Uani d S 1 Cl Cl2 0.0000 0.5000 0.0000 0.0911(10) Uani d S 1 Cl loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.0180(2) 0.0180(2) 0.0180(2) -0.00028(18) 0.00028(18) -0.00028(18) N1 0.0199(10) 0.0208(11) 0.0252(11) 0.0008(8) 0.0010(9) 0.0026(9) S1 0.0206(3) 0.0216(3) 0.0246(3) -0.0003(2) 0.0014(2) 0.0042(2) C1 0.0313(14) 0.0198(12) 0.0257(13) -0.0024(10) 0.0065(11) 0.0023(10) C2 0.0354(15) 0.0303(14) 0.0282(14) -0.0007(12) 0.0017(11) 0.0048(11) C3 0.0576(19) 0.0379(17) 0.0280(15) -0.0058(15) -0.0020(14) 0.0042(12) C4 0.068(2) 0.0356(16) 0.0296(15) -0.0093(15) 0.0160(15) 0.0006(13) C5 0.0473(18) 0.0380(16) 0.0446(18) -0.0018(14) 0.0229(15) 0.0012(14) C6 0.0317(14) 0.0318(14) 0.0390(16) -0.0018(12) 0.0077(12) 0.0025(12) C7 0.0265(13) 0.0221(12) 0.0224(12) -0.0033(10) -0.0038(10) 0.0035(10) C8 0.0274(13) 0.0325(15) 0.0345(15) -0.0034(11) -0.0004(11) 0.0039(12) C9 0.0349(15) 0.0299(14) 0.0391(16) -0.0107(12) -0.0046(13) 0.0045(12) C10 0.0478(17) 0.0244(13) 0.0291(14) -0.0051(12) -0.0049(13) 0.0010(11) C11 0.0390(16) 0.0269(14) 0.0271(14) 0.0002(11) 0.0037(12) -0.0010(11) C12 0.0283(14) 0.0253(13) 0.0255(13) -0.0026(10) 0.0009(11) 0.0030(10) Cl1 0.0303(3) 0.0303(3) 0.0303(3) 0.0054(2) -0.0054(2) 0.0054(2) Cl2 0.0911(10) 0.0911(10) 0.0911(10) -0.0293(8) 0.0293(8) 0.0293(8) 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Fe1 N1 6_456 86.21(9) y S1 N1 Fe1 . 128.32(13) ? S1 N1 H1A . 113(2) ? Fe1 N1 H1A . 115(2) ? N1 S1 C1 . 108.45(12) ? N1 S1 C7 . 109.57(11) ? C1 S1 C7 . 99.90(11) ? C6 C1 C2 . 121.6(2) ? C6 C1 S1 . 116.9(2) ? C2 C1 S1 . 121.4(2) ? C3 C2 C1 . 118.6(3) ? C3 C2 H2 . 120.7 ? C1 C2 H2 . 120.7 ? C4 C3 C2 . 119.9(3) ? C4 C3 H3 . 120.0 ? C2 C3 H3 . 120.0 ? C5 C4 C3 . 121.4(3) ? C5 C4 H4 . 119.3 ? C3 C4 H4 . 119.3 ? C4 C5 C6 . 119.2(3) ? C4 C5 H5 . 120.4 ? C6 C5 H5 . 120.4 ? C1 C6 C5 . 119.3(3) ? C1 C6 H6 . 120.4 ? C5 C6 H6 . 120.4 ? C12 C7 C8 . 121.0(2) ? C12 C7 S1 . 120.12(19) ? C8 C7 S1 . 118.7(2) ? C9 C8 C7 . 119.2(3) ? C9 C8 H8 . 120.4 ? C7 C8 H8 . 120.4 ? C10 C9 C8 . 120.3(3) ? C10 C9 H9 . 119.8 ? C8 C9 H9 . 119.8 ? C9 C10 C11 . 120.1(3) ? C9 C10 H10 . 119.9 ? C11 C10 H10 . 119.9 ? C10 C11 C12 . 120.6(3) ? C10 C11 H11 . 119.7 ? C12 C11 H11 . 119.7 ? C7 C12 C11 . 118.7(2) ? C7 C12 H12 . 120.6 ? C11 C12 H12 . 120.6 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Fe1 N1 2.078(2) y N1 S1 1.582(2) ? N1 H1A 0.82(3) ? S1 C1 1.787(3) ? S1 C7 1.797(2) ? C1 C6 1.384(4) ? C1 C2 1.388(4) ? C2 C3 1.387(4) ? C2 H2 0.9500 ? C3 C4 1.384(5) ? C3 H3 0.9500 ? C4 C5 1.376(5) ? C4 H4 0.9500 ? C5 C6 1.394(4) ? C5 H5 0.9500 ? C6 H6 0.9500 ? C7 C12 1.381(4) ? C7 C8 1.391(4) ? C8 C9 1.380(4) ? C8 H8 0.9500 ? C9 C10 1.377(4) ? C9 H9 0.9500 ? C10 C11 1.380(4) ? C10 H10 0.9500 ? C11 C12 1.388(4) ? C11 H11 0.9500 ? C12 H12 0.9500 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N1 H1A Cl1 0.82(3) 2.50(3) 3.272(2) 157(3)