#------------------------------------------------------------------------------ #$Date: 2011-03-31 14:48:06 +0300 (Thu, 31 Mar 2011) $ #$Revision: 17004 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4315757.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4315757 loop_ _publ_author_name 'Vilma R. Bojan' 'Eduardo J. Fern\'andez' 'Antonio Laguna' 'Jos\'e M. L\'opez-de-Luzuriaga' 'Miguel Monge' 'M. Elena Olmos' 'Raquel C. Puelles' 'Cristian Silvestru' _publ_section_title ; Study of the Coordination Abilities of Stibine Ligands to Gold(I) ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 5530 _journal_page_last 5541 _journal_volume 49 _journal_year 2010 _chemical_compound_source 'synthesis as described' _chemical_formula_moiety 'C63 H63 Au Cl O4 Sb3' _chemical_formula_sum 'C63 H63 Au Cl O4 Sb3' _chemical_formula_weight 1481.8 _chemical_name_common rpVL815 _chemical_name_systematic ; ? ; _space_group_IT_number 205 _symmetry_cell_setting cubic _symmetry_Int_Tables_number 205 _symmetry_space_group_name_Hall '-P 2ac 2ab 3' _symmetry_space_group_name_H-M 'P a -3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_creation_date 2008-10-06T09:50:26-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 22.1544(3) _cell_length_b 22.1544(3) _cell_length_c 22.1544(3) _cell_measurement_reflns_used 4874 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 28.31 _cell_measurement_theta_min 2.76 _cell_measurement_wavelength 0.71073 _cell_volume 10873.8(3) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _diffrn_ambient_temperature 173(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_UB_11 0.416662E-1 _diffrn_orient_matrix_UB_12 -0.11759E-1 _diffrn_orient_matrix_UB_13 -0.127698E-1 _diffrn_orient_matrix_UB_21 0.37406E-2 _diffrn_orient_matrix_UB_22 -0.263423E-1 _diffrn_orient_matrix_UB_23 0.364624E-1 _diffrn_orient_matrix_UB_31 -0.169514E-1 _diffrn_orient_matrix_UB_32 -0.347164E-1 _diffrn_orient_matrix_UB_33 -0.233418E-1 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_unetI/netI 0.025 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 4519 _diffrn_reflns_theta_full 27.09 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_min 2.76 _diffrn_source 'Enraf Nonius FR590' _exptl_absorpt_coefficient_mu 4.262 _exptl_absorpt_correction_T_max 0.4865 _exptl_absorpt_correction_T_min 0.2398 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details Scalepack _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.81 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 5776 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.1 _refine_diff_density_max 4.813 _refine_diff_density_min -1.782 _refine_diff_density_rms 0.193 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_hydrogen_treatment riding _refine_ls_matrix_type full _refine_ls_number_parameters 220 _refine_ls_number_reflns 4009 _refine_ls_number_restraints 72 _refine_ls_restrained_S_all 1.154 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0514 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0762P)^2^+40.4056P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.126 _refine_ls_wR_factor_ref 0.141 _reflns_number_gt 3010 _reflns_number_total 4009 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic1003484_si_002_7.cif _[local]_cod_data_source_block vl815 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according to the built-in table from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_database_code 4315757 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 'y, z, x' '-y+1/2, -z, x+1/2' 'y+1/2, -z+1/2, -x' '-y, z+1/2, -x+1/2' 'z, x, y' '-z, x+1/2, -y+1/2' '-z+1/2, -x, y+1/2' 'z+1/2, -x+1/2, -y' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' '-y, -z, -x' 'y-1/2, z, -x-1/2' '-y-1/2, z-1/2, x' 'y, -z-1/2, x-1/2' '-z, -x, -y' 'z, -x-1/2, y-1/2' 'z-1/2, x, -y-1/2' '-z-1/2, x-1/2, y' 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 Au Au 0.159796(12) 0.159796(12) 0.159796(12) 0.02776(15) Uani 1 3 d S . . Sb Sb 0.22267(2) 0.18088(2) 0.06161(2) 0.02719(15) Uani 1 1 d . . . C1 C 0.2386(3) 0.2723(3) 0.0340(3) 0.0292(14) Uani 1 1 d DU . . C2 C 0.2123(3) 0.3010(3) -0.0158(3) 0.0353(15) Uani 1 1 d DU . . C3 C 0.2236(3) 0.3617(3) -0.0262(3) 0.0357(15) Uani 1 1 d DU . . H3 H 0.2061 0.3807 -0.0593 0.043 Uiso 1 1 calc R . . C4 C 0.2608(3) 0.3946(3) 0.0122(3) 0.0397(16) Uani 1 1 d DU . . C5 C 0.2878(3) 0.3660(3) 0.0608(4) 0.0408(17) Uani 1 1 d DU . . H5 H 0.3141 0.3875 0.0855 0.049 Uiso 1 1 calc R . . C6 C 0.2762(3) 0.3053(3) 0.0732(3) 0.0358(15) Uani 1 1 d DU . . C7 C 0.1705(4) 0.2691(4) -0.0577(4) 0.0454(19) Uani 1 1 d DU . . H7A H 0.1926 0.2392 -0.0801 0.068 Uiso 1 1 calc R . . H7B H 0.1529 0.2976 -0.0852 0.068 Uiso 1 1 calc R . . H7C H 0.1391 0.2497 -0.035 0.068 Uiso 1 1 calc R . . C8 C 0.2692(4) 0.4620(4) 0.0000(4) 0.049(2) Uani 1 1 d DU . . H8A H 0.231 0.4822 0.0033 0.073 Uiso 1 1 calc R . . H8B H 0.285 0.4676 -0.04 0.073 Uiso 1 1 calc R . . H8C H 0.2968 0.4786 0.0289 0.073 Uiso 1 1 calc R . . C9 C 0.3043(4) 0.2790(4) 0.1297(4) 0.0467(19) Uani 1 1 d DU . . H9A H 0.273 0.264 0.1557 0.07 Uiso 1 1 calc R . . H9B H 0.3267 0.3097 0.1504 0.07 Uiso 1 1 calc R . . H9C H 0.3308 0.2465 0.1188 0.07 Uiso 1 1 calc R . . C11 C 0.3111(3) 0.1446(3) 0.0534(3) 0.0285(14) Uani 1 1 d DU . . C12 C 0.3479(3) 0.1628(3) 0.0056(3) 0.0313(15) Uani 1 1 d DU . . H12 H 0.335 0.1926 -0.0211 0.038 Uiso 1 1 calc R . . C13 C 0.4039(3) 0.1357(3) -0.0014(3) 0.0356(15) Uani 1 1 d DU . . H13 H 0.4287 0.1473 -0.0333 0.043 Uiso 1 1 calc R . . C14 C 0.4231(3) 0.0924(3) 0.0377(3) 0.0353(15) Uani 1 1 d DU . . H14 H 0.4608 0.0748 0.0324 0.042 Uiso 1 1 calc R . . C15 C 0.3874(3) 0.0745(4) 0.0845(4) 0.0437(18) Uani 1 1 d DU . . H15 H 0.4008 0.0446 0.1108 0.052 Uiso 1 1 calc R . . C16 C 0.3306(3) 0.1011(3) 0.0933(3) 0.0355(16) Uani 1 1 d DU . . H16 H 0.3065 0.0895 0.1256 0.043 Uiso 1 1 calc R . . C21 C 0.1799(3) 0.1311(3) -0.0089(3) 0.0285(13) Uani 1 1 d DU . . C22 C 0.2082(3) 0.1126(3) -0.0616(3) 0.0336(15) Uani 1 1 d DU . . H22 H 0.2477 0.1249 -0.0689 0.04 Uiso 1 1 calc R . . C23 C 0.1797(3) 0.0767(3) -0.1032(3) 0.0372(16) Uani 1 1 d DU . . H23 H 0.1996 0.0644 -0.138 0.045 Uiso 1 1 calc R . . C24 C 0.1206(3) 0.0590(3) -0.0923(3) 0.0408(17) Uani 1 1 d DU . . H24 H 0.1005 0.0348 -0.1201 0.049 Uiso 1 1 calc R . . C25 C 0.0915(3) 0.0773(3) -0.0401(3) 0.0401(17) Uani 1 1 d DU . . H25 H 0.0519 0.0652 -0.0329 0.048 Uiso 1 1 calc R . . C26 C 0.1208(3) 0.1130(3) 0.0011(3) 0.0330(15) Uani 1 1 d DU . . H26 H 0.1009 0.1252 0.036 0.04 Uiso 1 1 calc R . . Cl Cl 0.31810(9) 0.18190(9) -0.18190(9) 0.0431(7) Uani 1 3 d S . . O1 O 0.2777(3) 0.1408(4) -0.2080(4) 0.083(2) Uani 1 1 d . . . O2 O 0.3552(4) 0.1448(4) -0.1448(4) 0.097(5) Uani 1 3 d S . . 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 Au 0.02776(15) 0.02776(15) 0.02776(15) 0.00109(10) 0.00109(10) 0.00109(10) Sb 0.0268(2) 0.0262(2) 0.0286(3) 0.00096(17) 0.00146(17) 0.00035(17) C1 0.025(3) 0.030(3) 0.033(3) -0.003(3) -0.001(3) 0.001(3) C2 0.031(4) 0.042(4) 0.032(4) -0.001(3) 0.002(3) 0.008(3) C3 0.032(4) 0.035(3) 0.040(4) 0.009(3) 0.003(3) 0.008(3) C4 0.034(4) 0.031(3) 0.053(5) 0.000(3) 0.007(3) 0.004(3) C5 0.037(4) 0.032(4) 0.053(5) 0.000(3) -0.004(3) -0.002(3) C6 0.041(4) 0.031(4) 0.036(4) 0.001(3) -0.001(3) 0.000(3) C7 0.059(5) 0.032(4) 0.046(5) -0.001(3) -0.014(4) 0.000(3) C8 0.048(5) 0.037(4) 0.061(5) 0.014(4) -0.009(4) -0.003(3) C9 0.054(5) 0.041(4) 0.045(4) -0.001(3) -0.013(4) -0.001(4) C11 0.024(3) 0.031(3) 0.030(3) -0.001(3) -0.002(3) 0.001(3) C12 0.032(4) 0.027(3) 0.035(4) 0.003(3) 0.001(3) 0.002(3) C13 0.027(3) 0.045(4) 0.035(4) -0.004(3) 0.002(3) 0.001(3) C14 0.026(3) 0.041(4) 0.039(4) -0.006(3) -0.002(3) 0.007(3) C15 0.047(4) 0.042(4) 0.043(4) 0.003(3) 0.002(3) 0.015(3) C16 0.032(4) 0.039(4) 0.036(4) 0.008(3) 0.002(3) -0.002(3) C21 0.032(3) 0.027(3) 0.027(3) 0.005(3) -0.001(3) 0.004(3) C22 0.032(4) 0.032(4) 0.036(4) -0.004(3) 0.001(3) 0.003(3) C23 0.042(4) 0.037(4) 0.033(4) -0.004(3) -0.001(3) 0.008(3) C24 0.046(4) 0.036(4) 0.040(4) -0.005(3) -0.010(3) -0.003(3) C25 0.035(4) 0.040(4) 0.045(4) 0.001(3) -0.005(3) -0.003(3) C26 0.033(3) 0.032(4) 0.033(4) -0.003(3) 0.000(3) 0.000(3) Cl 0.0431(7) 0.0431(7) 0.0431(7) -0.0038(9) 0.0038(9) -0.0038(9) O1 0.054(4) 0.100(6) 0.096(6) -0.038(5) -0.001(4) -0.022(4) O2 0.097(5) 0.097(5) 0.097(5) 0.023(5) -0.023(5) 0.023(5) 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Sb Au Sb 119.524(3) . 9 ? Sb Au Sb 119.524(3) . 5 ? Sb Au Sb 119.524(3) 9 5 ? C11 Sb C21 98.7(2) . . ? C11 Sb C1 100.4(2) . . ? C21 Sb C1 110.6(2) . . ? C11 Sb Au 119.54(16) . . ? C21 Sb Au 106.19(16) . . ? C1 Sb Au 119.42(17) . . ? C2 C1 C6 119.7(7) . . ? C2 C1 Sb 125.8(5) . . ? C6 C1 Sb 114.4(5) . . ? C3 C2 C1 119.7(7) . . ? C3 C2 C7 118.0(6) . . ? C1 C2 C7 122.2(7) . . ? C2 C3 C4 120.9(6) . . ? C5 C4 C3 119.4(7) . . ? C5 C4 C8 122.2(7) . . ? C3 C4 C8 118.4(7) . . ? C4 C5 C6 121.0(7) . . ? C5 C6 C1 119.2(7) . . ? C5 C6 C9 117.3(7) . . ? C1 C6 C9 123.5(6) . . ? C16 C11 C12 120.4(6) . . ? C16 C11 Sb 119.9(5) . . ? C12 C11 Sb 119.6(5) . . ? C13 C12 C11 118.9(6) . . ? C14 C13 C12 120.8(7) . . ? C13 C14 C15 120.5(7) . . ? C14 C15 C16 120.3(7) . . ? C11 C16 C15 119.0(7) . . ? C26 C21 C22 118.5(6) . . ? C26 C21 Sb 116.8(5) . . ? C22 C21 Sb 124.5(5) . . ? C23 C22 C21 121.8(7) . . ? C22 C23 C24 118.8(7) . . ? C25 C24 C23 120.2(7) . . ? C26 C25 C24 120.2(7) . . ? C25 C26 C21 120.5(7) . . ? O1 Cl O1 114.8(3) . 12 ? O1 Cl O1 114.8(3) . 6_554 ? O1 Cl O1 114.8(3) 12 6_554 ? O1 Cl O2 103.4(4) . . ? O1 Cl O2 103.4(4) 12 . ? O1 Cl O2 103.4(4) 6_554 . ? 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 Au Sb 2.6250(4) . ? Au Sb 2.6250(4) 9 ? Au Sb 2.6250(4) 5 ? Sb C11 2.125(7) . ? Sb C21 2.134(7) . ? Sb C1 2.145(7) . ? C1 C2 1.401(8) . ? C1 C6 1.408(9) . ? C2 C3 1.387(10) . ? C2 C7 1.491(11) . ? C3 C4 1.390(9) . ? C4 C5 1.386(9) . ? C4 C8 1.529(11) . ? C5 C6 1.395(9) . ? C6 C9 1.515(11) . ? C11 C16 1.378(9) . ? C11 C12 1.394(8) . ? C12 C13 1.389(9) . ? C13 C14 1.361(9) . ? C14 C15 1.363(9) . ? C15 C16 1.403(9) . ? C21 C26 1.386(8) . ? C21 C22 1.387(8) . ? C22 C23 1.372(9) . ? C23 C24 1.387(9) . ? C24 C25 1.384(10) . ? C25 C26 1.372(9) . ? Cl O1 1.402(7) . ? Cl O1 1.402(7) 12 ? Cl O1 1.402(7) 6_554 ? Cl O2 1.423(15) . ?