#------------------------------------------------------------------------------ #$Date: 2017-10-13 01:08:28 +0100 (Fri, 13 Oct 2017) $ #$Revision: 201955 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/72/2007221.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_2007221 loop_ _publ_author_name ' Webster, Michael' _publ_section_title ; Dibromotriphenylantimony(V), a Second Polymorph ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 570 _journal_page_last 572 _journal_paper_doi 10.1107/S0108270197018040 _journal_volume 54 _journal_year 1998 _chemical_formula_iupac '[Sb Br2 (C6 H5)3]' _chemical_formula_moiety 'C18 H15 Br2 Sb ' _chemical_formula_structural '[(C6H5)3SbBr2]' _chemical_formula_sum 'C18 H15 Br2 Sb' _chemical_formula_weight 512.87 _chemical_name_systematic ; dibromotriphenylantimony(V) ; _space_group_IT_number 7 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P -2ya' _symmetry_space_group_name_H-M 'P 1 a 1' _audit_creation_method SHELXL-97 _cell_angle_alpha 90 _cell_angle_beta 118.10(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.714(4) _cell_length_b 10.159(3) _cell_length_c 14.006(2) _cell_measurement_reflns_used 20 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 21.1 _cell_measurement_theta_min 18.9 _cell_volume 1721.3(8) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988) ; _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1995)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device 'Rigaku AFC7S' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed xray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0739 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 3359 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_min 2.60 _diffrn_standards_decay_% 1.0 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 6.236 _exptl_absorpt_correction_T_max 0.535 _exptl_absorpt_correction_T_min 0.306 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '\y scan (North et al., 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_meas ? _exptl_crystal_description plate _exptl_crystal_F_000 976.00 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _refine_diff_density_max 1.803 _refine_diff_density_min -2.767 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment 'H atoms riding' _refine_ls_matrix_type full _refine_ls_number_parameters 379 _refine_ls_number_reflns 3172 _refine_ls_number_restraints 74 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.088 _refine_ls_R_factor_gt 0.051 _refine_ls_shift/su_max 0.100 _refine_ls_shift/su_mean 0.023 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1008P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.148 _reflns_number_gt 2310 _reflns_number_total 3172 _reflns_threshold_expression I>2\s(I) _cod_data_source_file cf1211.cif _cod_data_source_block Ph3SbBr2 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.1008P)^2^] 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^)+(0.1008P)^2^] 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 1721.3(9) _cod_original_sg_symbol_H-M 'P a' _cod_original_formula_sum 'C18 H15 Br2 Sb ' _cod_database_code 2007221 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+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 .01151(9) .37044(13) .51174(9) .0217(3) Uani d . 1 . . Sb Sb2 -.00131(10) .09125(13) -.00204(10) .0230(3) Uani d . 1 . . Sb Br1 .08386(18) .6048(2) .49466(18) .0357(6) Uani d . 1 . . Br Br2 -.06475(16) .13350(19) .51357(16) .0337(5) Uani d . 1 . . Br Br3 .05728(17) -.1384(2) -.04694(17) .0332(5) Uani d . 1 . . Br Br4 -.06272(16) .3197(2) .04430(16) .0309(5) Uani d . 1 . . Br C1 .0148(15) .4199(18) .6614(13) .022(3) Uani d U 1 . . C C2 .1029(15) .500(2) .7351(14) .027(4) Uani d U 1 . . C H2 .1594 .5296 .7193 .032 Uiso calc R 1 . . H C3 .103(2) .5321(19) .8285(17) .039(4) Uani d U 1 . . C H3 .1616 .5860 .8785 .047 Uiso calc R 1 . . H C4 .026(2) .492(2) .8548(14) .042(5) Uani d U 1 . . C H4 .0293 .5172 .9219 .050 Uiso calc R 1 . . H C5 -.063(2) .412(2) .7799(17) .036(4) Uani d U 1 . . C H5 -.1187 .3818 .7960 .043 Uiso calc R 1 . . H C6 -.0645(17) .3790(19) .6837(15) .031(4) Uani d U 1 . . C H6 -.1231 .3264 .6326 .037 Uiso calc R 1 . . H C7 -.1329(15) .3990(18) .3671(14) .025(4) Uani d U 1 . . C C8 -.2238(17) .459(2) .3722(17) .040(5) Uani d U 1 . . C H8 -.2163 .4904 .4393 .048 Uiso calc R 1 . . H C9 -.3234(17) .472(2) .2786(16) .035(5) Uani d U 1 . . C H9 -.3836 .5142 .2816 .042 Uiso calc R 1 . . H C10 -.3372(16) .423(2) .1798(16) .033(4) Uani d U 1 . . C H10 -.4063 .4288 .1160 .040 Uiso calc R 1 . . H C11 -.2461(16) .3657(19) .1785(15) .032(4) Uani d U 1 . . C H11 -.2527 .3307 .1128 .039 Uiso calc R 1 . . H C12 -.1473(19) .359(2) .2704(16) .040(5) Uani d U 1 . . C H12 -.0855 .3245 .2656 .048 Uiso calc R 1 . . H C13 .1547(14) .2920(18) .5131(14) .024(4) Uani d U 1 . . C C14 .1494(16) .215(2) .4295(15) .032(4) Uani d U 1 . . C H14 .0798 .1898 .3715 .039 Uiso calc R 1 . . H C15 .2487(19) .173(2) .4314(18) .037(5) Uani d U 1 . . C H15 .2471 .1240 .3729 .045 Uiso calc R 1 . . H C16 .3495(19) .205(2) .5217(19) .044(5) Uani d U 1 . . C H16 .4172 .1753 .5260 .053 Uiso calc R 1 . . H C17 .3499(18) .278(2) .6028(19) .047(5) Uani d U 1 . . C H17 .4191 .2975 .6635 .056 Uiso calc R 1 . . H C18 .2557(17) .326(2) .6023(17) .037(4) Uani d U 1 . . C H18 .2589 .3795 .6594 .044 Uiso calc R 1 . . H C19 -.0015(16) .0095(19) .1382(14) .027(4) Uani d U 1 . . C C20 -.0869(14) .0349(17) .1573(14) .023(4) Uani d U 1 . . C H20 -.1461 .0891 .1090 .028 Uiso calc R 1 . . H C21 -.0884(18) -.018(2) .2480(17) .036(4) Uani d U 1 . . C H21 -.1482 -.0021 .2627 .043 Uiso calc R 1 . . H C22 .001(2) -.096(2) .3166(16) .043(5) Uani d U 1 . . C H22 .0035 -.1314 .3807 .052 Uiso calc R 1 . . H C23 .084(2) -.122(2) .2928(17) .051(6) Uani d U 1 . . C H23 .1439 -.1753 .3405 .061 Uiso calc R 1 . . H C24 .0817(17) -.075(2) .2041(16) .037(5) Uani d U 1 . . C H24 .1379 -.0983 .1859 .045 Uiso calc R 1 . . H C25 -.1445(16) .0904(19) -.1541(14) .026(4) Uani d U 1 . . C C26 -.2456(15) .1266(18) -.1624(16) .028(4) Uani d U 1 . . C H26 -.2503 .1527 -.0996 .033 Uiso calc R 1 . . H C27 -.3377(19) .125(2) -.2600(18) .040(5) Uani d U 1 . . C H27 -.4064 .1502 -.2644 .048 Uiso calc R 1 . . H C28 -.3348(16) .0871(19) -.3528(16) .031(4) Uani d U 1 . . C H28 -.4004 .0837 -.4203 .037 Uiso calc R 1 . . H C29 -.2317(15) .0537(19) -.3451(14) .027(4) Uani d U 1 . . C H29 -.2263 .0315 -.4084 .033 Uiso calc R 1 . . H C30 -.1379(18) .053(2) -.2449(14) .035(5) Uani d U 1 . . C H30 -.0689 .0273 -.2392 .043 Uiso calc R 1 . . H C31 .1430(14) .1768(18) .0085(16) .026(4) Uani d U 1 . . C C32 .2096(17) .255(3) .1008(19) .050(6) Uani d U 1 . . C H32 .1903 .2681 .1570 .060 Uiso calc R 1 . . H C33 .3047(19) .311(2) .105(2) .060(7) Uani d U 1 . . C H33 .3493 .3659 .1647 .073 Uiso calc R 1 . . H C34 .335(3) .290(3) .030(3) .080(9) Uani d U 1 . . C H34 .4035 .3238 .0397 .096 Uiso calc R 1 . . H C35 .268(2) .220(3) -.062(2) .057(6) Uani d U 1 . . C H35 .2865 .2121 -.1196 .069 Uiso calc R 1 . . H C36 .174(2) .161(2) -.070(2) .047(5) Uani d U 1 . . C H36 .1296 .1075 -.1311 .057 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 .0246(7) .0131(6) .0281(6) .0014(6) .0130(5) -.0002(5) Sb2 .0262(7) .0130(6) .0311(6) .0011(6) .0145(5) .0003(6) Br1 .0477(14) .0143(11) .0542(13) -.0023(10) .0313(11) .0030(9) Br2 .0424(12) .0133(11) .0515(12) -.0046(9) .0271(10) -.0017(9) Br3 .0434(13) .0142(10) .0502(12) .0028(9) .0288(11) -.0003(9) Br4 .0398(12) .0155(11) .0435(11) .0000(9) .0248(10) -.0026(8) C1 .027(9) .020(10) .024(8) .012(7) .016(7) .004(6) C2 .022(8) .026(10) .033(8) .007(7) .013(7) .012(7) C3 .059(12) .013(10) .039(9) .001(9) .017(9) -.005(8) C4 .075(14) .039(13) .017(8) .016(10) .027(9) .002(7) C5 .059(12) .020(11) .043(10) .017(8) .037(9) .015(8) C6 .040(10) .020(11) .032(9) -.012(8) .016(8) .000(7) C7 .022(8) .011(9) .030(7) .000(7) .002(7) .005(7) C8 .032(10) .045(14) .036(8) .011(10) .011(7) -.006(10) C9 .028(8) .033(13) .044(9) .009(9) .016(7) .005(9) C10 .027(8) .032(12) .035(8) -.006(8) .011(8) .001(8) C11 .041(10) .020(11) .031(8) -.009(9) .013(7) -.012(8) C12 .044(9) .045(15) .033(8) .015(11) .018(7) .004(9) C13 .027(7) .013(9) .033(9) .008(7) .015(7) .001(7) C14 .031(8) .044(13) .027(9) -.005(9) .018(7) -.005(8) C15 .044(10) .031(13) .050(10) .009(9) .032(8) .002(9) C16 .036(8) .044(14) .064(13) .001(10) .032(8) .011(10) C17 .033(8) .019(11) .064(12) -.004(9) .003(9) -.003(9) C18 .038(9) .022(11) .041(10) -.006(9) .010(7) -.001(8) C19 .038(10) .013(9) .029(9) -.003(7) .015(7) .002(7) C20 .020(8) .010(9) .033(8) -.002(7) .007(7) .008(7) C21 .049(11) .012(11) .065(13) -.005(8) .043(10) .001(8) C22 .075(15) .019(11) .032(10) -.002(10) .022(9) .002(8) C23 .065(14) .032(13) .036(10) .021(12) .008(10) .005(8) C24 .029(9) .035(13) .038(10) .011(8) .008(8) -.010(8) C25 .029(7) .017(10) .025(7) -.005(8) .005(7) .002(7) C26 .029(8) .010(9) .042(8) .001(8) .014(7) .013(7) C27 .038(9) .029(12) .045(10) .008(10) .014(7) -.005(9) C28 .030(8) .016(10) .039(8) .005(8) .011(8) .012(8) C29 .029(8) .025(11) .022(7) -.007(8) .007(6) .000(7) C30 .035(9) .033(12) .028(8) .008(10) .006(6) -.004(8) C31 .018(8) .007(9) .051(10) .000(7) .014(7) -.001(7) C32 .030(11) .041(15) .067(13) -.006(10) .013(10) -.014(11) C33 .032(11) .026(14) .108(18) -.012(9) .021(12) -.021(13) C34 .074(18) .027(15) .17(3) -.008(13) .079(18) -.023(17) C35 .042(13) .048(16) .101(16) .013(10) .050(13) .021(12) C36 .064(14) .022(13) .077(14) -.004(10) .051(12) .002(10) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C' H 0.0000 0.0000 'International Tables Vol C' Sb -0.5866 1.5461 'International Tables Vol C' Br -0.2901 2.4595 'International Tables Vol C' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 5 -2 -5 5 2 -5 0 0 -6 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 C7 Sb1 C13 121.1(7) y C7 Sb1 C1 119.6(7) y C13 Sb1 C1 119.4(7) y C7 Sb1 Br2 86.4(5) y C13 Sb1 Br2 91.5(5) y C1 Sb1 Br2 91.8(5) y C7 Sb1 Br1 90.7(5) y C13 Sb1 Br1 87.3(5) y C1 Sb1 Br1 92.4(5) y Br2 Sb1 Br1 175.74(9) y C31 Sb2 C25 118.1(8) y C31 Sb2 C19 120.4(7) y C25 Sb2 C19 121.6(7) y C31 Sb2 Br3 90.0(5) y C25 Sb2 Br3 89.9(5) y C19 Sb2 Br3 90.5(5) y C31 Sb2 Br4 91.0(5) y C25 Sb2 Br4 89.9(5) y C19 Sb2 Br4 88.7(5) y Br3 Sb2 Br4 178.91(9) y C6 C1 C2 121.2(17) ? C6 C1 Sb1 121.0(14) ? C2 C1 Sb1 117.8(13) ? C3 C2 C1 117.3(19) ? C4 C3 C2 124(2) ? C3 C4 C5 118.5(18) ? C6 C5 C4 119(2) ? C1 C6 C5 120.8(19) ? C12 C7 C8 117.9(18) ? C12 C7 Sb1 124.3(16) ? C8 C7 Sb1 117.8(14) ? C9 C8 C7 119.3(19) ? C8 C9 C10 121(2) ? C11 C10 C9 117.4(18) ? C12 C11 C10 120.6(19) ? C7 C12 C11 123(2) ? C14 C13 C18 122.1(18) ? C14 C13 Sb1 121.9(14) ? C18 C13 Sb1 116.0(14) ? C13 C14 C15 119.2(19) ? C16 C15 C14 119(2) ? C17 C16 C15 120(2) ? C16 C17 C18 124(2) ? C17 C18 C13 117(2) ? C20 C19 C24 120.8(18) ? C20 C19 Sb2 119.2(14) ? C24 C19 Sb2 119.9(16) ? C19 C20 C21 119.7(18) ? C20 C21 C22 118(2) ? C23 C22 C21 120(2) ? C24 C23 C22 121(2) ? C23 C24 C19 120(2) ? C30 C25 C26 119.8(18) ? C30 C25 Sb2 120.1(15) ? C26 C25 Sb2 120.2(14) ? C27 C26 C25 120(2) ? C26 C27 C28 122(2) ? C27 C28 C29 118.1(19) ? C30 C29 C28 119.8(19) ? C25 C30 C29 120(2) ? C36 C31 C32 119(2) ? C36 C31 Sb2 122.2(15) ? C32 C31 Sb2 118.3(16) ? C33 C32 C31 117(2) ? C34 C33 C32 123(3) ? C33 C34 C35 121(3) ? C34 C35 C36 119(3) ? C31 C36 C35 121(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 Sb1 Br1 . 2.634(3) y Sb1 Br2 . 2.629(2) y Sb1 C1 . 2.135(16) y Sb1 C7 . 2.082(17) y Sb1 C13 . 2.111(17) y Sb2 Br3 . 2.638(3) y Sb2 Br4 . 2.652(2) y Sb2 C19 . 2.134(18) y Sb2 C25 . 2.110(17) y Sb2 C31 . 2.102(18) y C1 C6 . 1.33(3) ? C1 C2 . 1.42(3) ? C2 C3 . 1.35(3) ? C3 C4 . 1.34(3) ? C4 C5 . 1.43(3) ? C5 C6 . 1.38(3) ? C7 C12 . 1.34(3) ? C7 C8 . 1.42(3) ? C8 C9 . 1.38(3) ? C9 C10 . 1.40(3) ? C10 C11 . 1.39(3) ? C11 C12 . 1.36(3) ? C13 C14 . 1.38(3) ? C13 C18 . 1.40(3) ? C14 C15 . 1.41(3) ? C15 C16 . 1.40(3) ? C16 C17 . 1.36(3) ? C17 C18 . 1.38(3) ? C19 C20 . 1.34(3) ? C19 C24 . 1.38(3) ? C20 C21 . 1.39(3) ? C21 C22 . 1.39(3) ? C22 C23 . 1.35(3) ? C23 C24 . 1.32(3) ? C25 C30 . 1.37(3) ? C25 C26 . 1.38(3) ? C26 C27 . 1.36(3) ? C27 C28 . 1.37(3) ? C28 C29 . 1.41(3) ? C29 C30 . 1.39(2) ? C31 C36 . 1.36(3) ? C31 C32 . 1.42(3) ? C32 C33 . 1.40(3) ? C33 C34 . 1.32(4) ? C34 C35 . 1.38(4) ? C35 C36 . 1.39(3) ? 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 _geom_torsion_publ_flag Br1 Sb1 C1 C2 -37.6(14) y Br1 Sb1 C1 C6 141.1(15) ? Br1 Sb1 C7 C8 -89.2(16) y Br1 Sb1 C7 C12 94.0(18) ? Br1 Sb1 C13 C14 -113.2(16) y Br1 Sb1 C13 C18 65.1(14) ? Br2 Sb1 C1 C2 143.4(13) ? Br2 Sb1 C1 C6 -37.9(15) ? Br2 Sb1 C7 C8 93.9(16) ? Br2 Sb1 C7 C12 -82.9(18) ? Br2 Sb1 C13 C14 62.7(16) ? Br2 Sb1 C13 C18 -119.0(14) ? Br3 Sb2 C19 C20 -133.9(15) y Br3 Sb2 C19 C24 42.1(16) ? Br3 Sb2 C25 C26 135.8(15) y Br3 Sb2 C25 C30 -43.8(16) ? Br3 Sb2 C31 C32 -130.5(16) y Br3 Sb2 C31 C36 49.9(17) ? Br4 Sb2 C19 C20 45.4(15) ? Br4 Sb2 C19 C24 -138.5(16) ? Br4 Sb2 C25 C26 -43.1(15) ? Br4 Sb2 C25 C30 137.3(16) ? Br4 Sb2 C31 C32 49.1(16) ? Br4 Sb2 C31 C36 -130.5(17) ? loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 264804