#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/25/2012536.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_2012536 loop_ _publ_author_name 'Razak, Ibrahim Abdul' 'Usman, Anwar' 'Fun, Hoong-Kun' 'Yamin, Bohari M.' 'Keat, Goh Wooi' _publ_section_title ; Dichlorobis(trimethylenethiourea-\kS)antimony(III) chloride ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m122 _journal_page_last m123 _journal_paper_doi 10.1107/S0108270101020911 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Sb Cl2 (C4 H8 N2 S)2] Cl' _chemical_formula_moiety 'C8 H16 Cl2 N4 S2 Sb 1+, Cl 1-' _chemical_formula_sum 'C8 H16 Cl3 N4 S2 Sb' _chemical_formula_weight 460.47 _chemical_melting_point 480 _chemical_name_systematic ; Dichlorobis(trimethylenethiourea-S)antimony(III) chloride ; _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 71.3580(10) _cell_angle_beta 84.2520(10) _cell_angle_gamma 73.6120(10) _cell_formula_units_Z 2 _cell_length_a 7.5103(4) _cell_length_b 10.3304(5) _cell_length_c 12.1206(6) _cell_measurement_reflns_used 5944 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.35 _cell_measurement_theta_min 1.77 _cell_volume 854.78(7) _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_data_reduction SAINT _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990) ; _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 8.33 _diffrn_measured_fraction_theta_full .991 _diffrn_measured_fraction_theta_max .991 _diffrn_measurement_device_type 'Siemens SMART CCD area-detector' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0688 _diffrn_reflns_av_sigmaI/netI .1091 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4916 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 1.77 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 2.316 _exptl_absorpt_correction_T_max .7375 _exptl_absorpt_correction_T_min .6545 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.789 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 452 _exptl_crystal_size_max .20 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .14 _refine_diff_density_max 1.550 _refine_diff_density_min -1.785 _refine_ls_extinction_coef .054(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 164 _refine_ls_number_reflns 2981 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.085 _refine_ls_R_factor_all .0647 _refine_ls_R_factor_gt .0580 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0841P)^2^+0.1942P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .1537 _refine_ls_wR_factor_ref .1578 _reflns_number_gt 2799 _reflns_number_total 2981 _reflns_threshold_expression I>2\s(I) _cod_data_source_file tr1006.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value '480K' was changed to '480' - the value should be numeric and without a unit designator. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_chemical_melting_point' value '480K' was changed to '480' - the value should be numeric and without a unit designator. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2012536 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _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 _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Sb1 .47852(4) .44234(3) .19963(3) .0272(3) Uani d . 1 . . Sb Cl1 .4838(2) .18669(15) .29632(14) .0460(4) Uani d . 1 . . Cl Cl2 .3689(2) .72354(15) .10677(14) .0461(4) Uani d . 1 . . Cl Cl3 .7829(2) .4118(2) .35724(15) .0479(4) Uani d . 1 . . Cl S1 .26511(19) .51998(14) .34993(11) .0341(4) Uani d . 1 . . S S2 .2109(2) .48201(15) .06763(13) .0375(4) Uani d . 1 . . S N1 .1543(7) .3125(6) .5067(4) .0413(12) Uani d . 1 . . N H1A .0530 .3510 .4680 .050 Uiso calc R 1 . . H N2 .4532(6) .3148(5) .5265(4) .0358(11) Uani d . 1 . . N H2A .5421 .3542 .5007 .043 Uiso calc R 1 . . H N3 .2613(8) .2301(6) .0380(4) .0448(13) Uani d . 1 . . N H3A .3356 .2599 -.0168 .054 Uiso calc R 1 . . H N4 .0529(7) .2768(6) .1814(5) .0429(12) Uani d . 1 . . N H4A -.0075 .3366 .2165 .051 Uiso calc R 1 . . H C1 .2965(7) .3667(6) .4709(4) .0299(11) Uani d . 1 . . C C2 .4834(10) .1917(7) .6314(6) .0508(16) Uani d . 1 . . C H2B .5696 .1990 .6822 .061 Uiso calc R 1 . . H H2C .5362 .1056 .6102 .061 Uiso calc R 1 . . H C3 .3020(12) .1866(8) .6930(6) .058(2) Uani d . 1 . . C H3B .2569 .2670 .7226 .070 Uiso calc R 1 . . H H3C .3184 .1007 .7586 .070 Uiso calc R 1 . . H C4 .1618(10) .1896(8) .6098(6) .0548(18) Uani d . 1 . . C H4B .1985 .1033 .5877 .066 Uiso calc R 1 . . H H4C .0405 .1962 .6471 .066 Uiso calc R 1 . . H C5 .1724(7) .3149(6) .1001(4) .0311(11) Uani d . 1 . . C C6 .0166(12) .1354(9) .2161(8) .067(2) Uani d . 1 . . C H6A .0922 .0730 .2826 .081 Uiso calc R 1 . . H H6B -.1127 .1439 .2389 .081 Uiso calc R 1 . . H C7 .0592(13) .0744(9) .1201(9) .077(3) Uani d . 1 . . C H7A -.0404 .1201 .0640 .093 Uiso calc R 1 . . H H7B .0633 -.0254 .1500 .093 Uiso calc R 1 . . H C8 .2382(13) .0891(8) .0592(8) .068(3) Uani d . 1 . . C H8A .3400 .0196 .1061 .082 Uiso calc R 1 . . H H8B .2422 .0701 -.0145 .082 Uiso calc R 1 . . H 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 Sb1 .0260(3) .0231(3) .0318(3) -.00468(19) .00005(18) -.0094(2) Cl1 .0568(10) .0221(7) .0557(9) -.0049(6) -.0151(7) -.0078(6) Cl2 .0515(10) .0259(7) .0568(9) -.0125(7) .0074(7) -.0075(6) Cl3 .0249(8) .0723(11) .0598(10) -.0116(7) .0029(6) -.0403(9) S1 .0322(8) .0289(7) .0337(7) .0006(6) .0011(6) -.0075(6) S2 .0456(9) .0260(7) .0404(8) -.0052(6) -.0173(6) -.0082(6) N1 .029(3) .042(3) .048(3) -.011(2) -.002(2) -.006(2) N2 .030(3) .036(3) .038(2) -.008(2) -.0100(19) -.005(2) N3 .054(3) .046(3) .046(3) -.021(3) .014(2) -.026(2) N4 .045(3) .035(3) .053(3) -.013(2) .005(2) -.019(2) C1 .026(3) .032(3) .033(3) -.009(2) .001(2) -.013(2) C2 .066(4) .037(3) .050(3) -.017(3) -.021(3) -.007(3) C3 .084(6) .039(4) .040(3) -.014(4) -.001(4) .001(3) C4 .054(4) .046(4) .058(4) -.021(3) .014(3) -.005(3) C5 .031(3) .036(3) .032(3) -.006(2) -.006(2) -.019(2) C6 .062(5) .052(4) .096(6) -.030(4) .021(4) -.027(4) C7 .082(6) .050(5) .113(7) -.036(5) .017(5) -.032(5) C8 .097(7) .043(4) .082(5) -.034(4) .038(5) -.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 .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -.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 Sb1 Cl1 92.41(5) yes S1 Sb1 Cl2 76.62(5) yes S1 Sb1 S2 92.59(5) yes S2 Sb1 Cl2 76.18(5) yes Cl1 Sb1 S2 92.43(5) yes Cl1 Sb1 Cl2 163.60(6) yes C1 S1 Sb1 104.01(18) yes C5 S2 Sb1 104.18(18) yes C1 N1 C4 122.6(5) ? C1 N1 H1A 118.7 ? C4 N1 H1A 118.7 ? C1 N2 C2 122.4(5) ? C1 N2 H2A 118.8 ? C2 N2 H2A 118.8 ? C5 N3 C8 122.7(5) ? C5 N3 H3A 118.7 ? C8 N3 H3A 118.7 ? C5 N4 C6 123.1(5) ? C5 N4 H4A 118.4 ? C6 N4 H4A 118.4 ? N2 C1 N1 121.8(5) ? N2 C1 S1 120.1(4) ? N1 C1 S1 117.9(4) ? N2 C2 C3 109.0(5) ? N2 C2 H2B 109.9 ? C3 C2 H2B 109.9 ? N2 C2 H2C 109.9 ? C3 C2 H2C 109.9 ? H2B C2 H2C 108.3 ? C2 C3 C4 109.8(6) ? C2 C3 H3B 109.7 ? C4 C3 H3B 109.7 ? C2 C3 H3C 109.7 ? C4 C3 H3C 109.7 ? H3B C3 H3C 108.2 ? N1 C4 C3 108.3(6) ? N1 C4 H4B 110.0 ? C3 C4 H4B 110.0 ? N1 C4 H4C 110.0 ? C3 C4 H4C 110.0 ? H4B C4 H4C 108.4 ? N4 C5 N3 121.1(5) ? N4 C5 S2 120.0(4) ? N3 C5 S2 118.9(4) ? C7 C6 N4 110.7(6) ? C7 C6 H6A 109.5 ? N4 C6 H6A 109.5 ? C7 C6 H6B 109.5 ? N4 C6 H6B 109.5 ? H6A C6 H6B 108.1 ? C6 C7 C8 113.8(7) ? C6 C7 H7A 108.8 ? C8 C7 H7A 108.8 ? C6 C7 H7B 108.8 ? C8 C7 H7B 108.8 ? H7A C7 H7B 107.7 ? N3 C8 C7 111.7(6) ? N3 C8 H8A 109.3 ? C7 C8 H8A 109.3 ? N3 C8 H8B 109.3 ? C7 C8 H8B 109.3 ? H8A C8 H8B 107.9 ? 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 Sb1 S1 . 2.4810(10) yes Sb1 S2 . 2.555(2) yes Sb1 Cl1 . 2.5140(10) yes Sb1 Cl2 . 2.670(2) yes S1 C1 . 1.757(5) yes S2 C5 . 1.745(6) yes N1 C1 . 1.316(7) yes N1 C4 . 1.462(8) yes N1 H1A . .8600 ? N2 C1 . 1.303(7) yes N2 C2 . 1.465(8) yes N2 H2A . .8600 ? N3 C5 . 1.330(7) yes N3 C8 . 1.453(9) yes N3 H3A . .8600 ? N4 C5 . 1.306(7) yes N4 C6 . 1.481(9) yes N4 H4A . .8600 ? C2 C3 . 1.492(11) yes C2 H2B . .9700 ? C2 H2C . .9700 ? C3 C4 . 1.517(11) yes C3 H3B . .9700 ? C3 H3C . .9700 ? C4 H4B . .9700 ? C4 H4C . .9700 ? C6 C7 . 1.461(13) yes C6 H6A . .9700 ? C6 H6B . .9700 ? C7 C8 . 1.490(12) yes C7 H7A . .9700 ? C7 H7B . .9700 ? C8 H8A . .9700 ? C8 H8B . .9700 ? 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 _geom_hbond_publ_flag N1 H1A Cl3 1_455 .86 2.37 3.213(6) 169 yes N2 H2A Cl3 1_555 .86 2.44 3.227(5) 152 yes N3 H3A Cl2 2_665 .86 2.40 3.203(6) 156 yes N4 H4A Cl3 1_455 .86 2.37 3.168(6) 155 yes 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 Cl1 Sb1 S1 C1 22.28(19) S2 Sb1 S1 C1 114.82(19) Cl2 Sb1 S1 C1 -170.04(19) S1 Sb1 S2 C5 -96.33(19) Cl1 Sb1 S2 C5 -3.81(19) Cl2 Sb1 S2 C5 -171.87(19) C2 N2 C1 N1 .9(9) C2 N2 C1 S1 176.8(4) C4 N1 C1 N2 -.9(9) C4 N1 C1 S1 -176.9(5) Sb1 S1 C1 N2 68.2(5) Sb1 S1 C1 N1 -115.7(4) C1 N2 C2 C3 -28.5(8) N2 C2 C3 C4 54.1(7) C1 N1 C4 C3 27.9(9) C2 C3 C4 N1 -53.7(8) C6 N4 C5 N3 4.2(10) C6 N4 C5 S2 -178.2(5) C8 N3 C5 N4 -2.6(10) C8 N3 C5 S2 179.8(6) Sb1 S2 C5 N4 91.1(5) Sb1 S2 C5 N3 -91.3(5) C5 N4 C6 C7 -25.8(10) N4 C6 C7 C8 44.9(11) C5 N3 C8 C7 22.5(11) C6 C7 C8 N3 -44.0(12)