#------------------------------------------------------------------------------ #$Date: 2017-10-13 01:08:28 +0100 (Fri, 13 Oct 2017) $ #$Revision: 201955 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/61/2006131.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_2006131 loop_ _publ_author_name 'Blake, Alexander J.' 'Pearson, Matthew' 'Sowerby, D. Bryan' 'Woodhead, Peter P.' _publ_section_title ; Bis(ethylxanthato)phenylantimony(III) ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 583 _journal_page_last 585 _journal_paper_doi 10.1107/S0108270197000620 _journal_volume 53 _journal_year 1997 _chemical_formula_iupac '[Sb (C6 H5) (C3 H5 O1 S2)2]' _chemical_formula_sum 'C12 H15 O2 S4 Sb' _chemical_formula_weight 441.23 _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' _audit_creation_method SHELXL _cell_angle_alpha 84.24(4) _cell_angle_beta 84.20(4) _cell_angle_gamma 77.85(5) _cell_formula_units_Z 2 _cell_length_a 5.795(4) _cell_length_b 9.059(4) _cell_length_c 16.081(7) _cell_measurement_reflns_used 31 _cell_measurement_temperature 150.0(2) _cell_measurement_theta_max 13 _cell_measurement_theta_min 12 _cell_volume 818.3(8) _computing_cell_refinement STADI-4 _computing_data_collection 'STADI-4 (Stoe & Cie, 1995a)' _computing_data_reduction 'X-RED (Stoe & Cie, 1995b)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material SHELXL93 _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 150.0(2) _diffrn_measurement_device 'Stoe Stadi-4 four-circle' _diffrn_measurement_method \w-2\q _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 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0179 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2879 _diffrn_reflns_theta_max 25.07 _diffrn_reflns_theta_min 2.54 _diffrn_standards_decay_% 'intensity variation: +-2.0%' _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.190 _exptl_absorpt_correction_T_max 0.636 _exptl_absorpt_correction_T_min 0.415 _exptl_absorpt_correction_type '\y scans (North, Phillips & Mathews, 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 436 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.29 _refine_diff_density_min -0.28 _refine_ls_extinction_coef 0.0012(2) _refine_ls_extinction_method SHELXL93 _refine_ls_goodness_of_fit_all 1.144 _refine_ls_goodness_of_fit_obs 1.118 _refine_ls_hydrogen_treatment 'H atoms: riding model' _refine_ls_matrix_type full _refine_ls_number_parameters 173 _refine_ls_number_reflns 2879 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.143 _refine_ls_restrained_S_obs 1.118 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_obs .0190 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.013)^2^+0.81P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0417 _refine_ls_wR_factor_obs .0392 _reflns_number_observed 2679 _reflns_number_total 2879 _reflns_observed_criterion >2sigma(I) _cod_data_source_file mu1305.cif _cod_data_source_block sbxane _cod_depositor_comments ; The following automatic conversions were performed: '_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (15 times). Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (15 times). '_geom_angle_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (26 times). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.013)^2^+0.81P] where P = (Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.013)^2^+0.81P] where P = (Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 818.3(9) _cod_database_code 2006131 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Sb .01901(10) .01467(9) .01758(10) -.00317(6) -.00065(6) -.00015(6) S1 .0172(3) .0279(4) .0231(4) -.0013(3) -.0021(3) -.0083(3) C1 .0217(14) .0144(12) .0213(14) -.0029(10) -.0002(11) -.0008(10) S2 .0178(3) .0240(3) .0307(4) -.0047(3) -.0019(3) -.0078(3) O1 .0204(9) .0286(10) .0203(10) .0007(8) -.0025(8) -.0086(8) C2 .0327(16) .0341(16) .0175(14) -.0077(12) -.0044(12) -.0078(12) C3 .0417(18) .0312(16) .0200(15) -.0076(13) .0009(13) -.0055(12) S3 .0209(3) .0245(3) .0190(3) .0000(3) -.0039(3) -.0041(3) C4 .0292(15) .0170(12) .0140(13) -.0021(11) -.0043(11) .0034(10) S4 .0232(4) .0278(4) .0227(4) -.0042(3) -.0002(3) -.0048(3) O2 .0246(10) .0242(10) .0218(10) -.0031(8) -.0031(8) -.0071(8) C5 .0335(16) .0278(15) .0210(15) -.0030(12) -.0009(12) -.0086(12) C6 .0438(18) .0335(16) .0231(15) -.0129(14) .0018(13) -.0118(12) C11 .0194(13) .0152(12) .0146(12) -.0010(10) .0017(10) -.0015(10) C12 .0194(13) .0190(13) .0229(14) -.0047(10) .0001(11) -.0045(10) C13 .0238(14) .0218(14) .0242(15) -.0003(11) -.0064(11) -.0003(11) C14 .0272(15) .0181(13) .0244(15) -.0011(11) -.0015(12) .0022(11) C15 .0262(15) .0170(13) .0293(15) -.0098(11) -.0033(12) -.0005(11) C16 .0219(14) .0222(13) .0196(14) -.0046(11) -.0046(11) -.0018(10) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Sb .36287(3) 1.441953(18) 1.180718(11) .01726(6) Uani d . 1 . Sb S1 -.00199(11) 1.54256(8) 1.27548(4) .02278(15) Uani d . 1 . S C1 .1519(5) 1.5882(3) 1.35281(16) .0194(5) Uani d . 1 . C S2 .44314(11) 1.55044(7) 1.35069(4) .02373(15) Uani d . 1 . S O1 .0045(3) 1.6570(2) 1.41250(11) .0234(4) Uani d . 1 . O C2 .1002(5) 1.6983(3) 1.48545(17) .0274(6) Uani d . 1 . C H2A .2115 1.7669 1.4679 .033 Uiso calc R 1 . H H2B .1854 1.6067 1.5168 .033 Uiso calc R 1 . H C3 -.1084(5) 1.7765(3) 1.53897(18) .0309(7) Uani d . 1 . C H3A -.0536 1.8053 1.5895 .046 Uiso calc R 1 . H H3B -.2182 1.7078 1.5550 .046 Uiso calc R 1 . H H3C -.1896 1.8675 1.5073 .046 Uiso calc R 1 . H S3 .03551(12) 1.38831(7) 1.10602(4) .02185(14) Uani d . 1 . S C4 .2300(5) 1.2935(3) 1.03015(16) .0206(6) Uani d . 1 . C S4 .51958(12) 1.27647(8) 1.02591(4) .02463(15) Uani d . 1 . S O2 .1117(3) 1.2373(2) .97855(11) .0234(4) Uani d . 1 . O C5 .2413(5) 1.1541(3) .90916(17) .0275(6) Uani d . 1 . C H5A .3758 1.0768 .9295 .033 Uiso calc R 1 . H H5B .3037 1.2241 .8656 .033 Uiso calc R 1 . H C6 .0684(6) 1.0801(3) .87426(18) .0324(7) Uani d . 1 . C H6A .1474 1.0229 .8272 .049 Uiso calc R 1 . H H6B -.0640 1.1579 .8548 .049 Uiso calc R 1 . H H6C .0086 1.0110 .9180 .049 Uiso calc R 1 . H C11 .4423(4) 1.2198(3) 1.24713(15) .0170(5) Uani d D 1 . C C12 .6380(4) 1.1859(3) 1.29380(16) .0203(5) Uani d D 1 . C H12 .7311 1.2598 1.2963 .024 Uiso calc R 1 . H C13 .6988(5) 1.0438(3) 1.33716(17) .0237(6) Uani d D 1 . C H13 .8321 1.0219 1.3695 .028 Uiso calc R 1 . H C14 .5659(5) .9345(3) 1.33341(17) .0241(6) Uani d D 1 . C H14 .6066 .8380 1.3632 .029 Uiso calc R 1 . H C15 .3730(5) .9679(3) 1.28563(17) .0234(6) Uani d D 1 . C H15 .2826 .8930 1.2820 .028 Uiso calc R 1 . H C16 .3101(5) 1.1092(3) 1.24303(16) .0210(5) Uani d D 1 . C H16 .1764 1.1307 1.2109 .025 Uiso calc R 1 . H 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' 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' 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_publ_flag S1 Sb S2 62.67(5) yes S1 Sb S3 77.52(6) yes S1 Sb S4 142.35(4) yes S2 Sb S3 139.68(3) yes S2 Sb S4 153.58(3) yes S3 Sb S4 64.96(5) yes S1 Sb C11 95.89(8) yes S2 Sb C11 83.30(8) yes S3 Sb C11 95.22(8) yes S4 Sb C11 84.95(8) yes Sb S1 C1 95.52(11) yes Sb S2 C1 78.29(10) yes Sb S3 C4 93.08(11) yes Sb S4 C4 78.48(10) yes Sb C11 C12 117.90(18) yes Sb C11 C16 122.99(19) yes O1 C1 S2 125.5(2) yes O1 C1 S1 111.11(19) yes S2 C1 S1 123.37(16) yes C1 O1 C2 119.4(2) yes O1 C2 C3 106.2(2) yes O2 C4 S4 126.2(2) yes O2 C4 S3 110.4(2) yes S4 C4 S3 123.41(16) yes C4 O2 C5 119.6(2) yes O2 C5 C6 106.5(2) yes C12 C11 C16 119.1(2) ? C11 C12 C13 120.3(2) ? C14 C13 C12 120.4(3) ? C15 C14 C13 119.1(2) ? C14 C15 C16 120.9(2) ? C15 C16 C11 120.2(2) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sb S1 . 2.5377(19) yes Sb S2 . 3.1051(15) yes Sb S3 . 2.4987(17) yes Sb S4 . 2.9981(16) yes Sb C11 . 2.163(3) yes S1 C1 . 1.731(3) yes C1 O1 . 1.330(3) yes C1 S2 . 1.648(3) yes O1 C2 . 1.460(3) yes C2 C3 . 1.502(4) yes S3 C4 . 1.738(3) yes C4 O2 . 1.328(3) yes C4 S4 . 1.648(3) yes O2 C5 . 1.462(3) yes C5 C6 . 1.496(4) yes C11 C12 . 1.387(4) ? C11 C16 . 1.394(4) ? C12 C13 . 1.395(4) ? C13 C14 . 1.386(4) ? C14 C15 . 1.384(4) ? C15 C16 . 1.385(4) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C11 Sb S1 C1 81.43(12) S3 Sb S1 C1 175.49(9) Sb S1 C1 O1 175.54(16) Sb S1 C1 S2 -4.24(17) S2 C1 O1 C2 -3.1(3) S1 C1 O1 C2 177.17(18) C1 O1 C2 C3 178.5(2) C11 Sb S3 C4 -80.44(11) S1 Sb S3 C4 -175.34(8) Sb S3 C4 O2 176.29(16) Sb S3 C4 S4 -2.96(16) S4 C4 O2 C5 -1.4(3) S3 C4 O2 C5 179.42(18) C4 O2 C5 C6 168.8(2) S3 Sb C11 C12 173.68(18) S1 Sb C11 C12 -108.36(19) S3 Sb C11 C16 -4.5(2) S1 Sb C11 C16 73.5(2) C16 C11 C12 C13 -1.1(4) Sb C11 C12 C13 -179.34(19) C11 C12 C13 C14 0.7(4) C12 C13 C14 C15 0.4(4) C13 C14 C15 C16 -1.0(4) C14 C15 C16 C11 0.6(4) C12 C11 C16 C15 0.5(4) Sb C11 C16 C15 178.64(19) loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 24728847