#------------------------------------------------------------------------------ #$Date: 2011-03-31 14:48:06 +0300 (Thu, 31 Mar 2011) $ #$Revision: 17004 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4315754.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_4315754 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_absolute_configuration unk _chemical_compound_source 'synthesis as described' _chemical_formula_moiety 'C54 H66 Au Cl O4 Sb2' _chemical_formula_sum 'C54 H66 Au Cl O4 Sb2' _chemical_formula_weight 1254.98 _chemical_name_common 'VL23 (CHCl3/Et2O)' _chemical_name_systematic ; ? ; _space_group_IT_number 152 _symmetry_cell_setting trigonal _symmetry_Int_Tables_number 152 _symmetry_space_group_name_Hall 'P 31 2"' _symmetry_space_group_name_H-M 'P 31 2 1' _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 2010-02-03T12:06:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 3 _cell_length_a 15.2038(3) _cell_length_b 15.2038(3) _cell_length_c 19.1083(4) _cell_measurement_reflns_used 9845 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.47 _cell_measurement_theta_min 2.63 _cell_measurement_wavelength 0.71073 _cell_volume 3825.22(13) _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 0.582895E-1 _diffrn_orient_matrix_UB_12 0.321537E-1 _diffrn_orient_matrix_UB_13 0.334633E-1 _diffrn_orient_matrix_UB_21 0.48455E-1 _diffrn_orient_matrix_UB_22 0.270442E-1 _diffrn_orient_matrix_UB_23 -0.402361E-1 _diffrn_orient_matrix_UB_31 -0.4751E-2 _diffrn_orient_matrix_UB_32 0.632683E-1 _diffrn_orient_matrix_UB_33 0.1926E-3 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1071 _diffrn_reflns_av_unetI/netI 0.0641 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 47807 _diffrn_reflns_theta_full 27.47 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_min 2.63 _diffrn_source 'Enraf Nonius FR590' _exptl_absorpt_coefficient_mu 4.016 _exptl_absorpt_correction_T_max 0.7496 _exptl_absorpt_correction_T_min 0.5832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_description neddle _exptl_crystal_F_000 1860 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.206 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.149 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.019(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment riding _refine_ls_matrix_type full _refine_ls_number_parameters 290 _refine_ls_number_reflns 5846 _refine_ls_number_restraints 96 _refine_ls_restrained_S_all 1.032 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0389 _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^)+(0.0188P)^2^+7.4277P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.0647 _reflns_number_gt 4998 _reflns_number_total 5846 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic1003484_si_002_4.cif _[local]_cod_data_source_block ele91 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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 4315754 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' 'y, x, -z' '-x+y, -x, z+2/3' '-x, -x+y, -z+1/3' 'x-y, -y, -z+2/3' 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 0.48287(2) 0.48287(2) 0 0.01471(8) Uani 1 2 d S . . Sb Sb 0.53392(3) 0.41135(3) 0.105396(18) 0.01347(9) Uani 1 1 d . . . C1 C 0.6485(4) 0.5331(4) 0.1662(3) 0.0139(12) Uani 1 1 d DU . . C2 C 0.7310(4) 0.6086(4) 0.1291(3) 0.0188(11) Uani 1 1 d DU . . C3 C 0.7994(5) 0.6964(4) 0.1646(3) 0.0236(13) Uani 1 1 d DU . . H3 H 0.8554 0.7461 0.1405 0.028 Uiso 1 1 calc R . . C4 C 0.7874(5) 0.7128(5) 0.2342(3) 0.0258(14) Uani 1 1 d DU . . C5 C 0.7055(5) 0.6365(5) 0.2702(3) 0.0241(14) Uani 1 1 d DU . . H5 H 0.6969 0.6462 0.3172 0.029 Uiso 1 1 calc R . . C6 C 0.6361(4) 0.5463(4) 0.2383(3) 0.0150(12) Uani 1 1 d DU . . C7 C 0.7476(4) 0.6008(4) 0.0518(3) 0.0213(13) Uani 1 1 d DU . . H7A H 0.7293 0.5322 0.0406 0.032 Uiso 1 1 calc R . . H7B H 0.8178 0.6455 0.0405 0.032 Uiso 1 1 calc R . . H7C H 0.7061 0.62 0.0252 0.032 Uiso 1 1 calc R . . C8 C 0.8619(6) 0.8108(5) 0.2703(4) 0.048(2) Uani 1 1 d DU . . H8A H 0.9267 0.8145 0.2741 0.072 Uiso 1 1 calc R . . H8B H 0.8373 0.8126 0.3162 0.072 Uiso 1 1 calc R . . H8C H 0.8692 0.8674 0.2435 0.072 Uiso 1 1 calc R . . C9 C 0.5531(5) 0.4659(5) 0.2833(3) 0.0222(14) Uani 1 1 d DU . . H9A H 0.5669 0.4852 0.3317 0.033 Uiso 1 1 calc R . . H9B H 0.5507 0.4022 0.2764 0.033 Uiso 1 1 calc R . . H9C H 0.489 0.4592 0.2705 0.033 Uiso 1 1 calc R . . C11 C 0.5789(4) 0.3105(4) 0.0604(2) 0.0141(11) Uani 1 1 d DU . . C12 C 0.6737(4) 0.3181(4) 0.0710(2) 0.0165(12) Uani 1 1 d DU . . C13 C 0.6964(5) 0.2533(4) 0.0334(3) 0.0204(12) Uani 1 1 d DU . . H13 H 0.759 0.2577 0.0401 0.024 Uiso 1 1 calc R . . C14 C 0.6287(4) 0.1827(4) -0.0137(3) 0.0213(13) Uani 1 1 d DU . . C15 C 0.5349(5) 0.1752(4) -0.0218(3) 0.0206(13) Uani 1 1 d DU . . H15 H 0.4885 0.1271 -0.0527 0.025 Uiso 1 1 calc R . . C16 C 0.5072(4) 0.2368(4) 0.0145(3) 0.0180(13) Uani 1 1 d DU . . C17 C 0.7485(4) 0.3856(5) 0.1252(3) 0.0216(13) Uani 1 1 d DU . . H17A H 0.7879 0.4531 0.1068 0.032 Uiso 1 1 calc R . . H17B H 0.7928 0.3599 0.1373 0.032 Uiso 1 1 calc R . . H17C H 0.7127 0.387 0.1662 0.032 Uiso 1 1 calc R . . C18 C 0.6561(5) 0.1141(5) -0.0541(3) 0.0289(16) Uani 1 1 d DU . . H18A H 0.5966 0.0618 -0.0769 0.043 Uiso 1 1 calc R . . H18B H 0.6824 0.0838 -0.0225 0.043 Uiso 1 1 calc R . . H18C H 0.7067 0.1533 -0.0886 0.043 Uiso 1 1 calc R . . C19 C 0.3984(4) 0.2142(5) 0.0074(3) 0.0217(13) Uani 1 1 d DU . . H19A H 0.3606 0.179 0.0483 0.032 Uiso 1 1 calc R . . H19B H 0.3679 0.1725 -0.0331 0.032 Uiso 1 1 calc R . . H19C H 0.3978 0.2767 0.0023 0.032 Uiso 1 1 calc R . . C21 C 0.4045(5) 0.3139(4) 0.1675(3) 0.0167(11) Uani 1 1 d DU . . C22 C 0.3885(4) 0.2209(4) 0.1927(2) 0.0157(11) Uani 1 1 d DU . . C23 C 0.2933(4) 0.1503(4) 0.2185(3) 0.0189(13) Uani 1 1 d DU . . H23 H 0.2833 0.0889 0.236 0.023 Uiso 1 1 calc R . . C24 C 0.2126(4) 0.1693(4) 0.2189(3) 0.0211(13) Uani 1 1 d DU . . C25 C 0.2323(4) 0.2650(5) 0.1982(3) 0.0203(12) Uani 1 1 d DU . . H25 H 0.1806 0.2807 0.2013 0.024 Uiso 1 1 calc R . . C26 C 0.3264(4) 0.3380(4) 0.1730(3) 0.0169(13) Uani 1 1 d DU . . C27 C 0.4700(5) 0.1906(5) 0.1953(3) 0.0254(15) Uani 1 1 d DU . . H27A H 0.4549 0.1426 0.2324 0.038 Uiso 1 1 calc R . . H27B H 0.5349 0.2498 0.2037 0.038 Uiso 1 1 calc R . . H27C H 0.4715 0.1604 0.1516 0.038 Uiso 1 1 calc R . . C28 C 0.1084(5) 0.0894(5) 0.2422(3) 0.0331(16) Uani 1 1 d DU . . H28A H 0.0855 0.0298 0.2138 0.05 Uiso 1 1 calc R . . H28B H 0.0623 0.1149 0.2374 0.05 Uiso 1 1 calc R . . H28C H 0.1109 0.0726 0.2903 0.05 Uiso 1 1 calc R . . C29 C 0.3426(5) 0.4411(4) 0.1555(3) 0.0204(13) Uani 1 1 d DU . . H29A H 0.2816 0.443 0.1651 0.031 Uiso 1 1 calc R . . H29B H 0.3594 0.455 0.1068 0.031 Uiso 1 1 calc R . . H29C H 0.3971 0.4914 0.1834 0.031 Uiso 1 1 calc R . . Cl Cl 0.69476(17) 0.69476(17) 0.5 0.0319(6) Uani 1 2 d S . . O1 O 0.7391(5) 0.7652(5) 0.4423(2) 0.0614(16) Uani 1 1 d . . . O2 O 0.6900(5) 0.6057(4) 0.4811(4) 0.085(2) 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 Au 0.01614(13) 0.01614(13) 0.01344(14) 0.00102(7) -0.00102(7) 0.00925(15) Sb 0.0149(2) 0.0147(2) 0.01239(18) 0.00104(16) 0.00015(16) 0.00860(17) C1 0.008(3) 0.015(3) 0.016(3) -0.004(2) -0.003(2) 0.005(2) C2 0.018(3) 0.018(3) 0.023(3) 0.001(3) 0.000(2) 0.011(3) C3 0.021(4) 0.016(3) 0.029(3) 0.007(3) -0.002(3) 0.006(3) C4 0.027(4) 0.022(3) 0.026(3) -0.002(3) -0.011(3) 0.010(3) C5 0.032(4) 0.027(3) 0.016(3) -0.002(3) -0.010(3) 0.017(3) C6 0.013(3) 0.020(3) 0.018(3) -0.003(2) -0.005(2) 0.012(2) C7 0.021(3) 0.019(3) 0.020(3) 0.005(3) 0.004(3) 0.007(3) C8 0.046(5) 0.033(4) 0.040(5) -0.007(4) -0.008(4) 0.002(4) C9 0.024(3) 0.031(3) 0.016(3) -0.001(3) 0.002(3) 0.017(3) C11 0.017(3) 0.014(3) 0.016(3) 0.000(2) -0.001(2) 0.011(3) C12 0.022(3) 0.018(3) 0.014(3) 0.006(2) 0.003(2) 0.012(3) C13 0.024(3) 0.021(3) 0.019(3) 0.009(2) 0.008(3) 0.014(3) C14 0.034(4) 0.015(3) 0.014(3) 0.006(2) 0.012(3) 0.011(3) C15 0.026(3) 0.012(3) 0.019(3) 0.002(2) 0.005(3) 0.006(3) C16 0.022(3) 0.021(3) 0.011(3) 0.004(2) 0.003(2) 0.011(3) C17 0.020(3) 0.029(4) 0.023(3) -0.001(3) -0.001(2) 0.017(3) C18 0.034(4) 0.023(4) 0.027(4) 0.002(3) 0.012(3) 0.012(3) C19 0.019(3) 0.021(3) 0.021(3) -0.001(3) 0.002(2) 0.008(3) C21 0.019(3) 0.019(3) 0.014(3) -0.001(2) 0.000(3) 0.011(3) C22 0.023(3) 0.019(3) 0.009(3) -0.007(2) -0.001(2) 0.014(3) C23 0.031(3) 0.013(3) 0.015(3) 0.001(2) 0.004(2) 0.013(2) C24 0.021(3) 0.021(3) 0.016(3) -0.005(2) 0.001(3) 0.006(3) C25 0.018(3) 0.027(3) 0.019(3) 0.000(3) -0.001(3) 0.013(3) C26 0.018(3) 0.023(3) 0.013(3) -0.006(2) -0.001(2) 0.013(3) C27 0.033(4) 0.031(4) 0.021(3) 0.017(3) 0.015(3) 0.023(3) C28 0.028(3) 0.033(4) 0.035(4) -0.002(3) 0.010(3) 0.012(3) C29 0.021(3) 0.022(3) 0.023(3) -0.002(3) 0.002(3) 0.014(3) Cl 0.0448(12) 0.0448(12) 0.0253(12) 0.0001(5) -0.0001(5) 0.0368(13) O1 0.097(5) 0.067(4) 0.032(3) 0.008(3) -0.006(3) 0.050(4) O2 0.117(6) 0.032(4) 0.113(6) 0.004(3) 0.034(4) 0.041(4) 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 173.10(2) 3 . ? C21 Sb C1 111.53(18) . . ? C21 Sb C11 103.82(19) . . ? C1 Sb C11 115.02(19) . . ? C21 Sb Au 111.02(14) . . ? C1 Sb Au 110.15(14) . . ? C11 Sb Au 104.98(13) . . ? C2 C1 C6 120.3(5) . . ? C2 C1 Sb 116.2(4) . . ? C6 C1 Sb 122.8(4) . . ? C3 C2 C1 118.3(5) . . ? C3 C2 C7 118.5(5) . . ? C1 C2 C7 123.2(5) . . ? C4 C3 C2 122.6(6) . . ? C3 C4 C5 118.0(6) . . ? C3 C4 C8 120.9(6) . . ? C5 C4 C8 121.0(5) . . ? C6 C5 C4 122.1(6) . . ? C5 C6 C1 118.5(5) . . ? C5 C6 C9 117.8(5) . . ? C1 C6 C9 123.7(5) . . ? C12 C11 C16 120.7(5) . . ? C12 C11 Sb 124.4(4) . . ? C16 C11 Sb 114.8(4) . . ? C13 C12 C11 118.3(5) . . ? C13 C12 C17 117.9(5) . . ? C11 C12 C17 123.6(5) . . ? C14 C13 C12 122.2(6) . . ? C15 C14 C13 118.2(5) . . ? C15 C14 C18 121.0(5) . . ? C13 C14 C18 120.8(5) . . ? C14 C15 C16 122.4(5) . . ? C15 C16 C11 118.1(5) . . ? C15 C16 C19 117.7(5) . . ? C11 C16 C19 123.9(5) . . ? C22 C21 C26 119.7(5) . . ? C22 C21 Sb 121.9(4) . . ? C26 C21 Sb 117.6(4) . . ? C21 C22 C23 119.4(5) . . ? C21 C22 C27 124.2(5) . . ? C23 C22 C27 116.4(5) . . ? C22 C23 C24 121.8(5) . . ? C25 C24 C23 117.7(5) . . ? C25 C24 C28 121.3(5) . . ? C23 C24 C28 121.0(5) . . ? C26 C25 C24 122.2(5) . . ? C25 C26 C21 118.9(5) . . ? C25 C26 C29 118.6(5) . . ? C21 C26 C29 122.5(5) . . ? O2 Cl O2 117.2(6) . 3_556 ? O2 Cl O1 108.8(4) . 3_556 ? O2 Cl O1 107.8(3) 3_556 3_556 ? O2 Cl O1 107.8(3) . . ? O2 Cl O1 108.8(4) 3_556 . ? O1 Cl O1 105.8(5) 3_556 . ? 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 2.5855(3) 3 ? Au Sb 2.5855(3) . ? Sb C21 2.136(6) . ? Sb C1 2.142(5) . ? Sb C11 2.146(6) . ? C1 C2 1.398(7) . ? C1 C6 1.418(7) . ? C2 C3 1.391(8) . ? C2 C7 1.513(7) . ? C3 C4 1.383(7) . ? C4 C5 1.387(8) . ? C4 C8 1.514(9) . ? C5 C6 1.384(7) . ? C6 C9 1.511(8) . ? C11 C12 1.401(7) . ? C11 C16 1.412(7) . ? C12 C13 1.396(7) . ? C12 C17 1.500(8) . ? C13 C14 1.385(7) . ? C14 C15 1.382(8) . ? C14 C18 1.513(8) . ? C15 C16 1.390(7) . ? C16 C19 1.518(8) . ? C21 C22 1.395(7) . ? C21 C26 1.411(7) . ? C22 C23 1.392(7) . ? C22 C27 1.522(8) . ? C23 C24 1.394(7) . ? C24 C25 1.389(7) . ? C24 C28 1.502(8) . ? C25 C26 1.387(7) . ? C26 C29 1.498(8) . ? Cl O2 1.368(5) . ? Cl O2 1.368(5) 3_556 ? Cl O1 1.447(6) 3_556 ? Cl O1 1.447(6) . ?