#------------------------------------------------------------------------------ #$Date: 2014-04-30 01:57:34 +0300 (Wed, 30 Apr 2014) $ #$Revision: 112250 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/51/57/1515779.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_1515779 loop_ _publ_author_name 'Yurkerwich, Kevin' 'Buccella, Daniela' 'Melnick, Jonathan G.' 'Parkin, Gerard' _publ_section_title ; Tris(2-mercapto-1-tert-butylimidazolyl)hydroborato gallium derivatives: synthesis of di- and trigallium compounds in a sulfur-rich coordination environment ; _journal_issue 2 _journal_name_full 'Chemical Science' _journal_page_first 210 _journal_paper_doi 10.1039/c0sc00145g _journal_volume 1 _journal_year 2010 _chemical_formula_sum 'C23 H36 B Cl11 Ga2 N6 S3' _chemical_formula_weight 1032.96 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _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 _audit_creation_method SHELXL-97 _cell_angle_alpha 98.2300(10) _cell_angle_beta 107.1550(10) _cell_angle_gamma 112.1170(10) _cell_formula_units_Z 2 _cell_length_a 11.0927(5) _cell_length_b 14.4146(7) _cell_length_c 16.1852(8) _cell_measurement_reflns_used 8686 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 28.26 _cell_measurement_theta_min 2.24 _cell_volume 2194.38(18) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 273(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0150 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 14599 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 1.59 _exptl_absorpt_coefficient_mu 2.066 _exptl_absorpt_correction_T_max 0.5762 _exptl_absorpt_correction_T_min 0.5762 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details sadabs _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1036 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _platon_squeeze_details ; The unit cell contains 4 chloroform molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _refine_diff_density_max 0.748 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.070 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 347 _refine_ls_number_reflns 8883 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.102 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0421 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0783P)^2^+0.7021P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1282 _refine_ls_wR_factor_ref 0.1342 _reflns_number_gt 7144 _reflns_number_total 8883 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c0sc00145g.txt _[local]_cod_data_source_block 2s10p _[local]_cod_cif_authors_sg_H-M P-1 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to /usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. '_exptl_absorpt_correction_type' value 'EMPIRICAL' changed to 'empirical' according to /usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius ; _cod_database_code 1515779 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Ga1 Ga -0.05255(3) 0.14903(2) 0.08940(2) 0.04187(11) Uani 1 1 d . Ga2 Ga 0.33459(4) 1.38445(3) 0.66105(3) 0.05706(13) Uani 1 1 d . S1 S -0.03699(8) 0.12436(7) 0.22737(6) 0.0568(2) Uani 1 1 d . S2 S 0.16614(7) 0.23678(5) 0.09011(5) 0.04347(17) Uani 1 1 d . S3 S -0.16307(7) 0.25439(6) 0.06783(5) 0.04287(17) Uani 1 1 d . Cl1 Cl -0.17512(9) 0.00253(7) -0.01719(7) 0.0697(3) Uani 1 1 d . Cl2 Cl 0.2451(2) 1.44868(16) 0.56148(12) 0.1302(6) Uani 1 1 d . Cl3 Cl 0.17081(13) 1.25445(11) 0.67712(10) 0.0985(4) Uani 1 1 d . Cl4 Cl 0.45910(13) 1.50347(10) 0.78987(8) 0.0918(4) Uani 1 1 d . Cl5 Cl 0.48116(13) 1.33761(9) 0.62416(8) 0.0784(3) Uani 1 1 d . B B 0.1388(3) 0.3913(3) 0.2615(2) 0.0430(7) Uani 1 1 d D H1 H 0.198(3) 0.4668(18) 0.3131(18) 0.052 Uiso 1 1 d D N11 N 0.1985(2) 0.31590(19) 0.29649(16) 0.0451(6) Uani 1 1 d . C11 C 0.1388(3) 0.2122(2) 0.29003(19) 0.0454(7) Uani 1 1 d . N12 N 0.2374(3) 0.1882(2) 0.34023(16) 0.0489(6) Uani 1 1 d . C12 C 0.3388(3) 0.3565(3) 0.3521(2) 0.0512(7) Uani 1 1 d . H12A H 0.4054 0.4257 0.3682 0.061 Uiso 1 1 calc R C13 C 0.3621(3) 0.2795(3) 0.3785(2) 0.0537(8) Uani 1 1 d . H13A H 0.4480 0.2859 0.4165 0.064 Uiso 1 1 calc R C14 C 0.2181(4) 0.0839(3) 0.3565(3) 0.0625(9) Uani 1 1 d . C15 C 0.1696(6) 0.0040(4) 0.2684(3) 0.0830(13) Uani 1 1 d . H15A H 0.0792 -0.0055 0.2294 0.124 Uiso 1 1 calc R H15B H 0.1624 -0.0613 0.2793 0.124 Uiso 1 1 calc R H15C H 0.2361 0.0276 0.2403 0.124 Uiso 1 1 calc R C16 C 0.3607(5) 0.0962(4) 0.4198(3) 0.0834(13) Uani 1 1 d . H16A H 0.3920 0.1471 0.4762 0.125 Uiso 1 1 calc R H16B H 0.4286 0.1189 0.3925 0.125 Uiso 1 1 calc R H16C H 0.3507 0.0303 0.4304 0.125 Uiso 1 1 calc R C17 C 0.1171(5) 0.0561(4) 0.4047(3) 0.0852(13) Uani 1 1 d . H17A H 0.0272 0.0483 0.3665 0.128 Uiso 1 1 calc R H17B H 0.1533 0.1107 0.4596 0.128 Uiso 1 1 calc R H17C H 0.1068 -0.0084 0.4186 0.128 Uiso 1 1 calc R N21 N 0.1638(2) 0.41526(18) 0.17550(16) 0.0398(5) Uani 1 1 d . C21 C 0.1692(3) 0.3596(2) 0.10377(19) 0.0373(6) Uani 1 1 d . N22 N 0.1805(2) 0.41613(19) 0.04388(16) 0.0420(5) Uani 1 1 d . C22 C 0.1736(3) 0.5089(2) 0.1614(2) 0.0503(7) Uani 1 1 d . H22A H 0.1731 0.5623 0.2008 0.060 Uiso 1 1 calc R C23 C 0.1841(4) 0.5101(2) 0.0807(2) 0.0510(7) Uani 1 1 d . H23A H 0.1923 0.5644 0.0545 0.061 Uiso 1 1 calc R C24 C 0.1830(3) 0.3837(3) -0.0492(2) 0.0516(7) Uani 1 1 d . C25 C 0.0437(4) 0.2910(4) -0.1084(2) 0.0721(11) Uani 1 1 d . H25A H -0.0317 0.3097 -0.1120 0.108 Uiso 1 1 calc R H25B H 0.0317 0.2335 -0.0830 0.108 Uiso 1 1 calc R H25C H 0.0429 0.2710 -0.1679 0.108 Uiso 1 1 calc R C26 C 0.3088(4) 0.3607(4) -0.0394(3) 0.0662(10) Uani 1 1 d . H26A H 0.3106 0.3400 -0.0980 0.099 Uiso 1 1 calc R H26B H 0.3012 0.3052 -0.0118 0.099 Uiso 1 1 calc R H26C H 0.3939 0.4223 -0.0024 0.099 Uiso 1 1 calc R C27 C 0.2003(5) 0.4751(4) -0.0891(3) 0.0760(11) Uani 1 1 d . H27A H 0.1216 0.4906 -0.0954 0.114 Uiso 1 1 calc R H27B H 0.2046 0.4571 -0.1473 0.114 Uiso 1 1 calc R H27C H 0.2856 0.5354 -0.0498 0.114 Uiso 1 1 calc R N31 N -0.0188(3) 0.3533(2) 0.24989(16) 0.0451(6) Uani 1 1 d . C31 C -0.1422(3) 0.2963(2) 0.17955(19) 0.0400(6) Uani 1 1 d . N32 N -0.2481(3) 0.2773(2) 0.21036(17) 0.0485(6) Uani 1 1 d . C32 C -0.0488(4) 0.3705(3) 0.3252(2) 0.0645(10) Uani 1 1 d . H32A H 0.0173 0.4081 0.3833 0.077 Uiso 1 1 calc R C33 C -0.1879(4) 0.3249(3) 0.3018(2) 0.0651(10) Uani 1 1 d . H33A H -0.2356 0.3252 0.3403 0.078 Uiso 1 1 calc R C34 C -0.4036(3) 0.2070(3) 0.1578(2) 0.0528(8) Uani 1 1 d . C35 C -0.4797(4) 0.2083(4) 0.2227(3) 0.0754(11) Uani 1 1 d . H35A H -0.4686 0.2778 0.2440 0.113 Uiso 1 1 calc R H35B H -0.4402 0.1864 0.2730 0.113 Uiso 1 1 calc R H35C H -0.5779 0.1614 0.1918 0.113 Uiso 1 1 calc R C36 C -0.4222(4) 0.0964(3) 0.1248(3) 0.0699(11) Uani 1 1 d . H36A H -0.3738 0.0949 0.0846 0.105 Uiso 1 1 calc R H36B H -0.5206 0.0500 0.0933 0.105 Uiso 1 1 calc R H36C H -0.3841 0.0745 0.1754 0.105 Uiso 1 1 calc R C37 C -0.4608(4) 0.2480(3) 0.0826(3) 0.0629(9) Uani 1 1 d . H37A H -0.4462 0.3178 0.1073 0.094 Uiso 1 1 calc R H37B H -0.5597 0.2037 0.0507 0.094 Uiso 1 1 calc R H37C H -0.4131 0.2486 0.0417 0.094 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 Ga1 0.03442(16) 0.03257(17) 0.04753(19) 0.00516(13) 0.00764(13) 0.01191(13) Ga2 0.0603(2) 0.0528(2) 0.0544(2) 0.01654(17) 0.01615(17) 0.02522(18) S1 0.0431(4) 0.0476(4) 0.0590(5) 0.0234(4) 0.0078(3) 0.0052(3) S2 0.0400(3) 0.0341(3) 0.0578(4) 0.0124(3) 0.0176(3) 0.0188(3) S3 0.0418(4) 0.0498(4) 0.0373(3) 0.0078(3) 0.0117(3) 0.0248(3) Cl1 0.0448(4) 0.0463(4) 0.0852(6) -0.0166(4) 0.0072(4) 0.0131(3) Cl2 0.1522(14) 0.1486(15) 0.1151(11) 0.0754(11) 0.0265(10) 0.0971(13) Cl3 0.0710(6) 0.0820(8) 0.1212(10) 0.0385(7) 0.0298(6) 0.0141(6) Cl4 0.0821(7) 0.0910(8) 0.0726(6) -0.0108(6) 0.0320(5) 0.0187(6) Cl5 0.0963(7) 0.0773(7) 0.0789(6) 0.0225(5) 0.0440(6) 0.0477(6) B 0.0399(15) 0.0389(16) 0.0365(15) 0.0027(13) 0.0090(12) 0.0107(13) N11 0.0364(12) 0.0419(13) 0.0416(12) 0.0123(10) 0.0057(10) 0.0087(10) C11 0.0422(14) 0.0440(16) 0.0396(14) 0.0146(12) 0.0097(12) 0.0121(12) N12 0.0504(14) 0.0503(15) 0.0405(13) 0.0178(11) 0.0114(11) 0.0196(12) C12 0.0397(15) 0.0553(18) 0.0433(16) 0.0090(14) 0.0109(12) 0.0110(14) C13 0.0445(16) 0.063(2) 0.0427(16) 0.0145(14) 0.0081(13) 0.0194(15) C14 0.073(2) 0.060(2) 0.058(2) 0.0293(17) 0.0199(17) 0.0334(18) C15 0.102(3) 0.063(2) 0.073(3) 0.018(2) 0.015(2) 0.039(2) C16 0.094(3) 0.073(3) 0.073(3) 0.026(2) 0.006(2) 0.045(2) C17 0.097(3) 0.088(3) 0.092(3) 0.061(3) 0.049(3) 0.040(3) N21 0.0366(11) 0.0349(12) 0.0452(12) 0.0104(10) 0.0138(9) 0.0148(9) C21 0.0337(12) 0.0314(13) 0.0445(14) 0.0086(11) 0.0136(11) 0.0140(10) N22 0.0444(12) 0.0414(13) 0.0475(13) 0.0174(10) 0.0221(10) 0.0211(11) C22 0.0578(18) 0.0370(15) 0.0616(19) 0.0137(13) 0.0266(15) 0.0239(14) C23 0.0621(19) 0.0398(16) 0.0625(19) 0.0222(14) 0.0303(16) 0.0263(14) C24 0.0559(18) 0.066(2) 0.0493(17) 0.0241(15) 0.0280(14) 0.0346(16) C25 0.067(2) 0.093(3) 0.0465(19) 0.0166(19) 0.0149(16) 0.032(2) C26 0.067(2) 0.095(3) 0.066(2) 0.032(2) 0.0384(18) 0.053(2) C27 0.103(3) 0.094(3) 0.073(2) 0.054(2) 0.054(2) 0.061(3) N31 0.0423(12) 0.0451(13) 0.0374(12) 0.0036(10) 0.0124(10) 0.0137(11) C31 0.0393(14) 0.0397(14) 0.0420(14) 0.0107(11) 0.0152(11) 0.0188(12) N32 0.0420(13) 0.0547(15) 0.0469(14) 0.0122(12) 0.0201(11) 0.0179(12) C32 0.0554(19) 0.075(2) 0.0425(17) 0.0019(16) 0.0190(14) 0.0124(17) C33 0.0545(19) 0.084(3) 0.0441(17) 0.0061(17) 0.0252(15) 0.0178(18) C34 0.0384(15) 0.0567(19) 0.0636(19) 0.0211(15) 0.0190(14) 0.0204(14) C35 0.052(2) 0.100(3) 0.078(3) 0.032(2) 0.0342(19) 0.028(2) C36 0.0448(17) 0.052(2) 0.103(3) 0.019(2) 0.0231(19) 0.0161(15) C37 0.0523(18) 0.067(2) 0.077(2) 0.0250(19) 0.0228(17) 0.0334(17) 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' B B 0.0013 0.0007 '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' Ga Ga 0.2307 1.6083 '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 Cl1 Ga1 S2 112.20(4) Cl1 Ga1 S1 111.52(4) S2 Ga1 S1 109.95(3) Cl1 Ga1 S3 109.19(3) S2 Ga1 S3 107.32(3) S1 Ga1 S3 106.41(3) Cl2 Ga2 Cl4 110.06(7) Cl2 Ga2 Cl3 110.96(7) Cl4 Ga2 Cl3 108.91(6) Cl2 Ga2 Cl5 109.67(7) Cl4 Ga2 Cl5 105.56(5) Cl3 Ga2 Cl5 111.53(6) C11 S1 Ga1 99.28(10) C21 S2 Ga1 97.14(9) C31 S3 Ga1 96.67(10) H1 B N21 104.6(18) H1 B N11 107.4(18) N21 B N11 113.6(3) H1 B N31 106.5(18) N21 B N31 112.5(2) N11 B N31 111.6(3) C11 N11 C12 107.1(3) C11 N11 B 133.6(2) C12 N11 B 119.1(3) N12 C11 N11 109.1(2) N12 C11 S1 125.3(2) N11 C11 S1 125.6(2) C11 N12 C13 107.0(3) C11 N12 C14 127.7(3) C13 N12 C14 125.2(3) C13 C12 N11 108.2(3) C12 C13 N12 108.7(3) C15 C14 N12 109.6(3) C15 C14 C17 113.7(4) N12 C14 C17 107.9(3) C15 C14 C16 109.2(4) N12 C14 C16 108.3(3) C17 C14 C16 107.9(4) C21 N21 C22 108.0(2) C21 N21 B 133.8(2) C22 N21 B 118.0(2) N21 C21 N22 108.6(2) N21 C21 S2 126.1(2) N22 C21 S2 125.2(2) C21 N22 C23 107.5(2) C21 N22 C24 128.0(2) C23 N22 C24 124.5(3) C23 C22 N21 108.2(3) C22 C23 N22 107.6(3) C25 C24 C27 109.2(3) C25 C24 C26 113.0(3) C27 C24 C26 108.7(3) C25 C24 N22 108.6(3) C27 C24 N22 108.0(3) C26 C24 N22 109.2(3) C31 N31 C32 107.3(3) C31 N31 B 133.9(2) C32 N31 B 118.6(2) N31 C31 N32 108.6(2) N31 C31 S3 125.8(2) N32 C31 S3 125.6(2) C31 N32 C33 107.5(3) C31 N32 C34 127.4(3) C33 N32 C34 124.8(3) C33 C32 N31 109.1(3) C32 C33 N32 107.6(3) C37 C34 N32 110.3(3) C37 C34 C36 113.2(3) N32 C34 C36 108.1(3) C37 C34 C35 108.6(3) N32 C34 C35 107.8(3) C36 C34 C35 108.7(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ga1 Cl1 2.1669(8) Ga1 S2 2.2702(8) Ga1 S1 2.2780(9) Ga1 S3 2.2876(8) Ga2 Cl2 2.1482(13) Ga2 Cl4 2.1659(11) Ga2 Cl3 2.1759(13) Ga2 Cl5 2.1770(12) S1 C11 1.744(3) S2 C21 1.739(3) S3 C31 1.739(3) B H1 1.091(18) B N21 1.557(4) B N11 1.561(4) B N31 1.565(4) N11 C11 1.361(4) N11 C12 1.383(4) C11 N12 1.348(4) N12 C13 1.386(4) N12 C14 1.510(4) C12 C13 1.330(5) C14 C15 1.504(6) C14 C17 1.514(6) C14 C16 1.538(6) N21 C21 1.344(4) N21 C22 1.370(4) C21 N22 1.356(4) N22 C23 1.381(4) N22 C24 1.523(4) C22 C23 1.348(5) C24 C25 1.516(5) C24 C27 1.522(5) C24 C26 1.522(5) N31 C31 1.346(4) N31 C32 1.368(4) C31 N32 1.359(4) N32 C33 1.374(4) N32 C34 1.516(4) C32 C33 1.333(5) C34 C37 1.505(5) C34 C36 1.521(5) C34 C35 1.531(5) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.499 0.001 0.500 684 228 ' '