#------------------------------------------------------------------------------ #$Date: 2011-09-28 17:24:46 +0300 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/52/2015267.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_2015267 loop_ _publ_author_name 'Li, Wen-Ge' 'Zhang, You-Cai' 'Wang, Zuo-Wei' 'Li, Yi-Zhi' 'Zheng, He-Gen' _publ_section_title ; Bis(2,2'-bipyridine)iodo(oxo)tri-\m~3~-sulfido-tricopper(I)tungsten(VI) ; _journal_coeditor_code OB1248 _journal_issue 4 _journal_name_full 'Acta Crystallographica, Section C' _journal_page_first m159 _journal_page_last m160 _journal_volume 62 _journal_year 2006 _chemical_formula_iupac '[Cu3 W I O S3 (C10 H8 N2)2]' _chemical_formula_moiety 'C20 H16 Cu3 I N4 O S3 W' _chemical_formula_sum 'C20 H16 Cu3 I N4 O S3 W' _chemical_formula_weight 925.97 _chemical_name_systematic ; Bis(2,2'-bipyridine)iodo(oxo)tri-\m~3~-sulfido-tricopper(I)tungsten(VI) ; _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1 ' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 79.660(10) _cell_angle_beta 85.900(10) _cell_angle_gamma 67.380(10) _cell_formula_units_Z 2 _cell_length_a 8.8950(10) _cell_length_b 9.8280(10) _cell_length_c 16.331(2) _cell_measurement_reflns_used 3064 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.82 _cell_measurement_theta_min 2.42 _cell_volume 1296.4(3) _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction SAINT _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Bruker, 2000)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_device_type 'Bruker SMART APEX CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 6494 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.28 _exptl_absorpt_coefficient_mu 8.302 _exptl_absorpt_correction_T_max 0.191 _exptl_absorpt_correction_T_min 0.148 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_crystal_colour brown _exptl_crystal_density_diffrn 2.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 868 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 1.326 _refine_diff_density_min -1.351 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 298 _refine_ls_number_reflns 4503 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.051 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0332 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.03P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.0789 _reflns_number_gt 3824 _reflns_number_total 4503 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ob1248.cif _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 2015267 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _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 W W1 0.47708(3) 0.61446(3) 0.221255(14) 0.03868(10) Uani d . 1 Cu Cu1 0.24673(10) 0.70810(9) 0.33506(5) 0.0487(2) Uani d . 1 Cu Cu2 0.24730(10) 0.70558(9) 0.10520(5) 0.0480(2) Uani d . 1 Cu Cu3 0.41980(10) 0.36417(9) 0.25406(5) 0.0492(2) Uani d . 1 S S1 0.2598(2) 0.83236(18) 0.20645(10) 0.0487(4) Uani d . 1 S S2 0.4595(2) 0.47961(19) 0.12609(10) 0.0488(4) Uani d . 1 S S3 0.4649(2) 0.48618(18) 0.34909(9) 0.0443(4) Uani d . 1 I I1 0.34111(7) 0.14822(6) 0.28889(3) 0.06171(15) Uani d . 1 O O1 0.6552(6) 0.6454(6) 0.2085(3) 0.0643(14) Uani d . 1 C C1 -0.0540(9) 0.6287(9) 0.3468(4) 0.067(2) Uani d . 1 H H1 -0.0258 0.6054 0.2937 0.081 Uiso calc R 1 C C2 -0.1858(9) 0.6023(9) 0.3858(5) 0.070(2) Uani d . 1 H H2 -0.2446 0.5615 0.3601 0.084 Uiso calc R 1 C C3 -0.2264(9) 0.6385(9) 0.4633(5) 0.069(2) Uani d . 1 H H3 -0.3134 0.6211 0.4916 0.083 Uiso calc R 1 C C4 -0.1396(8) 0.7005(8) 0.5000(5) 0.0594(19) Uani d . 1 H H4 -0.1688 0.7282 0.5522 0.071 Uiso calc R 1 C C5 -0.0068(7) 0.7210(7) 0.4573(4) 0.0450(15) Uani d . 1 C C6 0.0983(8) 0.7820(7) 0.4931(4) 0.0439(15) Uani d . 1 C C7 0.0741(10) 0.8223(8) 0.5722(4) 0.063(2) Uani d . 1 H H7 -0.0113 0.8121 0.6056 0.076 Uiso calc R 1 C C8 0.1781(12) 0.8769(9) 0.5998(5) 0.079(3) Uani d . 1 H H8 0.1641 0.9043 0.6523 0.095 Uiso calc R 1 C C9 0.3031(10) 0.8908(8) 0.5493(5) 0.068(2) Uani d . 1 H H9 0.3754 0.9268 0.5673 0.082 Uiso calc R 1 C C10 0.3201(9) 0.8507(7) 0.4714(4) 0.0555(18) Uani d . 1 H H10 0.4040 0.8618 0.4370 0.067 Uiso calc R 1 N N1 0.0348(6) 0.6858(6) 0.3817(3) 0.0490(14) Uani d . 1 N N2 0.2209(6) 0.7969(5) 0.4438(3) 0.0428(12) Uani d . 1 C C11 0.3648(9) 0.9037(8) -0.0339(4) 0.0567(18) Uani d . 1 H H11 0.4431 0.8934 0.0040 0.068 Uiso calc R 1 C C12 0.3647(9) 0.9844(8) -0.1091(5) 0.063(2) Uani d . 1 H H12 0.4400 1.0296 -0.1222 0.075 Uiso calc R 1 C C13 0.2522(10) 0.9995(9) -0.1666(5) 0.070(2) Uani d . 1 H H13 0.2502 1.0540 -0.2196 0.085 Uiso calc R 1 C C14 0.1421(8) 0.9320(8) -0.1439(4) 0.0559(18) Uani d . 1 H H14 0.0648 0.9404 -0.1820 0.067 Uiso calc R 1 C C15 0.1460(7) 0.8514(7) -0.0645(3) 0.0407(14) Uani d . 1 C C16 0.0321(7) 0.7779(7) -0.0329(4) 0.0426(15) Uani d . 1 C C17 -0.0862(8) 0.7766(8) -0.0836(4) 0.0543(17) Uani d . 1 H H17 -0.0949 0.8209 -0.1393 0.065 Uiso calc R 1 C C18 -0.1903(9) 0.7080(8) -0.0493(5) 0.061(2) Uani d . 1 H H18 -0.2712 0.7065 -0.0818 0.074 Uiso calc R 1 C C19 -0.1752(8) 0.6428(8) 0.0315(5) 0.0573(18) Uani d . 1 H H19 -0.2446 0.5959 0.0552 0.069 Uiso calc R 1 C C20 -0.0537(8) 0.6474(8) 0.0783(4) 0.0527(17) Uani d . 1 H H20 -0.0432 0.6024 0.1339 0.063 Uiso calc R 1 N N3 0.2600(6) 0.8367(6) -0.0097(3) 0.0439(12) Uani d . 1 N N4 0.0481(6) 0.7130(6) 0.0475(3) 0.0427(12) Uani d . 1 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 W1 0.04201(16) 0.05145(18) 0.03022(14) -0.02765(13) -0.00218(10) -0.00227(11) Cu1 0.0528(5) 0.0556(5) 0.0388(4) -0.0223(4) 0.0032(4) -0.0074(4) Cu2 0.0566(5) 0.0563(5) 0.0360(4) -0.0268(4) -0.0124(4) -0.0030(4) Cu3 0.0561(5) 0.0440(5) 0.0516(5) -0.0244(4) -0.0020(4) -0.0051(4) S1 0.0697(11) 0.0397(9) 0.0373(8) -0.0219(9) -0.0098(8) -0.0015(7) S2 0.0565(10) 0.0523(10) 0.0390(9) -0.0208(9) -0.0025(7) -0.0096(7) S3 0.0509(9) 0.0484(10) 0.0339(8) -0.0215(8) -0.0042(7) 0.0001(7) I1 0.0897(4) 0.0651(3) 0.0493(3) -0.0499(3) 0.0082(2) -0.0130(2) O1 0.062(3) 0.091(4) 0.057(3) -0.052(3) 0.004(2) -0.005(3) C1 0.076(5) 0.096(6) 0.041(4) -0.048(5) -0.017(4) 0.001(4) C2 0.059(5) 0.099(6) 0.065(5) -0.051(5) -0.024(4) 0.014(5) C3 0.040(4) 0.088(6) 0.072(5) -0.026(4) -0.004(4) 0.013(5) C4 0.051(4) 0.056(5) 0.057(4) -0.010(4) 0.001(3) 0.000(4) C5 0.040(4) 0.045(4) 0.042(4) -0.013(3) -0.005(3) 0.006(3) C6 0.051(4) 0.038(4) 0.035(3) -0.008(3) -0.004(3) -0.003(3) C7 0.075(5) 0.059(5) 0.048(4) -0.019(4) -0.006(4) -0.004(4) C8 0.104(7) 0.072(6) 0.054(5) -0.018(5) -0.020(5) -0.022(4) C9 0.077(6) 0.053(5) 0.070(5) -0.013(4) -0.028(5) -0.016(4) C10 0.063(5) 0.046(4) 0.058(4) -0.021(4) -0.018(4) -0.002(3) N1 0.048(3) 0.066(4) 0.038(3) -0.028(3) -0.005(2) -0.005(3) N2 0.045(3) 0.038(3) 0.041(3) -0.011(2) -0.008(2) -0.003(2) C11 0.064(5) 0.073(5) 0.049(4) -0.043(4) -0.002(3) -0.009(4) C12 0.070(5) 0.068(5) 0.062(5) -0.038(4) 0.013(4) -0.016(4) C13 0.079(6) 0.068(5) 0.054(5) -0.026(5) 0.013(4) 0.008(4) C14 0.052(4) 0.069(5) 0.041(4) -0.019(4) -0.014(3) 0.001(3) C15 0.042(3) 0.045(4) 0.035(3) -0.016(3) -0.002(3) -0.006(3) C16 0.047(4) 0.041(4) 0.040(4) -0.014(3) -0.008(3) -0.009(3) C17 0.052(4) 0.063(5) 0.052(4) -0.025(4) -0.016(3) -0.009(3) C18 0.050(4) 0.074(5) 0.071(5) -0.028(4) -0.016(4) -0.023(4) C19 0.046(4) 0.067(5) 0.072(5) -0.031(4) 0.006(4) -0.025(4) C20 0.049(4) 0.070(5) 0.050(4) -0.032(4) 0.005(3) -0.016(4) N3 0.048(3) 0.052(3) 0.039(3) -0.026(3) -0.003(2) -0.009(2) N4 0.045(3) 0.054(3) 0.037(3) -0.026(3) -0.001(2) -0.009(2) 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 _geom_angle_publ_flag O1 W1 S1 110.80(18) yes O1 W1 S3 110.76(16) yes S1 W1 S3 108.07(6) yes O1 W1 S2 110.50(18) yes S1 W1 S2 108.58(6) yes S3 W1 S2 108.03(6) yes O1 W1 Cu3 131.77(18) ? S1 W1 Cu3 117.43(5) ? S3 W1 Cu3 54.22(5) ? S2 W1 Cu3 54.12(4) ? O1 W1 Cu2 124.40(16) ? S1 W1 Cu2 54.28(5) ? S3 W1 Cu2 124.84(5) ? S2 W1 Cu2 54.39(5) ? Cu3 W1 Cu2 85.99(3) ? O1 W1 Cu1 126.51(17) ? S1 W1 Cu1 53.66(5) ? S3 W1 Cu1 54.42(5) ? S2 W1 Cu1 122.99(5) ? Cu3 W1 Cu1 84.69(3) ? Cu2 W1 Cu1 89.58(3) ? N1 Cu1 N2 79.5(2) yes N1 Cu1 S1 121.81(15) yes N2 Cu1 S1 124.53(15) yes N1 Cu1 S3 112.81(16) yes N2 Cu1 S3 108.65(14) yes S1 Cu1 S3 107.24(7) yes N1 Cu1 W1 141.09(16) ? N2 Cu1 W1 137.72(15) ? S1 Cu1 W1 53.71(5) ? S3 Cu1 W1 53.54(4) ? N4 Cu2 N3 79.56(19) ?yes N4 Cu2 S1 129.03(16) yes N3 Cu2 S1 107.22(14) yes N4 Cu2 S2 116.21(16) yes N3 Cu2 S2 113.02(15) yes S1 Cu2 S2 107.27(6) yes N4 Cu2 W1 157.25(14) ? N3 Cu2 W1 122.70(13) ? S1 Cu2 W1 53.56(5) ? S2 Cu2 W1 53.80(4) ? S2 Cu3 S3 107.67(6) yes S2 Cu3 I1 127.99(5) yes S3 Cu3 I1 124.34(5) yes S2 Cu3 W1 54.11(5) ? S3 Cu3 W1 53.86(4) ? I1 Cu3 W1 174.48(4) ? Cu1 S1 W1 72.64(5) ? Cu1 S1 Cu2 112.27(7) ? W1 S1 Cu2 72.16(6) ? W1 S2 Cu3 71.76(5) ? W1 S2 Cu2 71.80(6) ? Cu3 S2 Cu2 105.89(7) ? W1 S3 Cu3 71.92(5) ? W1 S3 Cu1 72.04(5) ? Cu3 S3 Cu1 104.11(7) ? N1 C1 C2 123.3(7) ? N1 C1 H1 118.3 ? C2 C1 H1 118.3 ? C3 C2 C1 117.6(7) ? C3 C2 H2 121.2 ? C1 C2 H2 121.2 ? C2 C3 C4 120.5(7) ? C2 C3 H3 119.8 ? C4 C3 H3 119.8 ? C3 C4 C5 118.4(7) ? C3 C4 H4 120.8 ? C5 C4 H4 120.8 ? N1 C5 C4 121.8(6) ? N1 C5 C6 115.7(5) ? C4 C5 C6 122.5(6) ? N2 C6 C7 121.2(6) ? N2 C6 C5 115.5(5) ? C7 C6 C5 123.3(6) ? C8 C7 C6 119.0(7) ? C8 C7 H7 120.5 ? C6 C7 H7 120.5 ? C7 C8 C9 119.3(8) ? C7 C8 H8 120.3 ? C9 C8 H8 120.3 ? C8 C9 C10 119.1(8) ? C8 C9 H9 120.4 ? C10 C9 H9 120.4 ? N2 C10 C9 122.4(7) ? N2 C10 H10 118.8 ? C9 C10 H10 118.8 ? C5 N1 C1 118.4(6) ? C5 N1 Cu1 114.9(4) ? C1 N1 Cu1 126.4(5) ? C10 N2 C6 119.0(6) ? C10 N2 Cu1 126.9(5) ? C6 N2 Cu1 113.8(4) ? N3 C11 C12 124.4(7) ? N3 C11 H11 117.8 ? C12 C11 H11 117.8 ? C11 C12 C13 119.0(7) ? C11 C12 H12 120.5 ? C13 C12 H12 120.5 ? C12 C13 C14 118.3(7) ? C12 C13 H13 120.8 ? C14 C13 H13 120.8 ? C13 C14 C15 120.3(6) ? C13 C14 H14 119.9 ? C15 C14 H14 119.9 ? N3 C15 C14 120.0(5) ? N3 C15 C16 115.1(5) ? C14 C15 C16 124.9(6) ? N4 C16 C17 121.9(6) ? N4 C16 C15 116.5(5) ? C17 C16 C15 121.6(6) ? C18 C17 C16 118.3(6) ? C18 C17 H17 120.8 ? C16 C17 H17 120.8 ? C19 C18 C17 120.1(6) ? C19 C18 H18 119.9 ? C17 C18 H18 119.9 ? C18 C19 C20 118.5(6) ? C18 C19 H19 120.7 ? C20 C19 H19 120.7 ? N4 C20 C19 123.0(6) ? N4 C20 H20 118.5 ? C19 C20 H20 118.5 ? C11 N3 C15 118.0(5) ? C11 N3 Cu2 128.5(4) ? C15 N3 Cu2 113.5(4) ? C20 N4 C16 118.2(5) ? C20 N4 Cu2 126.6(4) ? C16 N4 Cu2 114.8(4) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag W1 O1 1.717(4) yes W1 S1 2.2531(18) yes W1 S3 2.2556(15) yes W1 S2 2.2649(17) yes W1 Cu3 2.6551(8) yes W1 Cu2 2.6662(8) yes W1 Cu1 2.6680(9) yes Cu1 N1 2.057(5) yes Cu1 N2 2.076(5) yes Cu1 S1 2.2517(17) yes Cu1 S3 2.2810(19) yes Cu2 N4 2.037(5) yes Cu2 N3 2.099(5) yes Cu2 S1 2.2741(18) yes Cu2 S2 2.2818(19) yes Cu3 S2 2.2650(17) yes Cu3 S3 2.2658(18) yes Cu3 I1 2.4435(9) yes C1 N1 1.336(8) ? C1 C2 1.384(10) ? C1 H1 0.9300 ? C2 C3 1.363(11) ? C2 H2 0.9300 ? C3 C4 1.373(10) ? C3 H3 0.9300 ? C4 C5 1.391(9) ? C4 H4 0.9300 ? C5 N1 1.331(8) ? C5 C6 1.487(9) ? C6 N2 1.347(8) ? C6 C7 1.396(9) ? C7 C8 1.369(11) ? C7 H7 0.9300 ? C8 C9 1.372(11) ? C8 H8 0.9300 ? C9 C10 1.379(10) ? C9 H9 0.9300 ? C10 N2 1.328(8) ? C10 H10 0.9300 ? C11 N3 1.336(8) ? C11 C12 1.337(9) ? C11 H11 0.9300 ? C12 C13 1.369(10) ? C12 H12 0.9300 ? C13 C14 1.377(10) ? C13 H13 0.9300 ? C14 C15 1.388(8) ? C14 H14 0.9300 ? C15 N3 1.350(7) ? C15 C16 1.473(8) ? C16 N4 1.345(7) ? C16 C17 1.390(8) ? C17 C18 1.377(9) ? C17 H17 0.9300 ? C18 C19 1.350(10) ? C18 H18 0.9300 ? C19 C20 1.386(9) ? C19 H19 0.9300 ? C20 N4 1.326(8) ? C20 H20 0.9300 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C2 H2 O1 1_455 0.93 2.57 3.202(9) 126