#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/07/2010757.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_2010757 loop_ _publ_author_name 'Perez-Lourido, P.' 'Garcia-Vazquez, J. A.' 'Romero, J.' 'Fernandez, P.' 'Sousa-Pedrares, A.' 'Sousa, A.' _publ_section_title ; Bis[2-(diphenylphosphinoyl)benzene] disulfide ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first e101 _journal_page_last e102 _journal_volume 56 _journal_year 2000 _chemical_formula_moiety 'C36 H28 O2 P2 S2' _chemical_formula_sum 'C36 H28 O2 P2 S2' _chemical_formula_weight 618.64 _chemical_name_systematic ; Bis[2-(diphenylphosphinyl)benzene] disulfide ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 104.50(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.249(3) _cell_length_b 10.801(2) _cell_length_c 21.193(5) _cell_measurement_reflns_used 25 _cell_measurement_temperature 203(2) _cell_measurement_theta_max 16.06 _cell_measurement_theta_min 12.54 _cell_volume 2936.2(11) _computing_cell_refinement 'Nonius CAD-4 software' _computing_data_collection 'Nonius CAD-4 software' _computing_data_reduction 'Nonius CAD-4 software' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 203(2) _diffrn_measured_fraction_theta_full .999 _diffrn_measured_fraction_theta_max .999 _diffrn_measurement_device_type 'Nonius CAD-4 MACH-3' _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 .71073 _diffrn_reflns_av_R_equivalents .024 _diffrn_reflns_av_sigmaI/netI .0536 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 2697 _diffrn_reflns_theta_full 24.97 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_min 1.99 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 150 _diffrn_standards_number 6 _exptl_absorpt_coefficient_mu .324 _exptl_absorpt_correction_T_max .938 _exptl_absorpt_correction_T_min .923 _exptl_absorpt_correction_type none _exptl_crystal_colour 'Light brown' _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Plate _exptl_crystal_F_000 1288 _exptl_crystal_size_max .25 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .20 _refine_diff_density_max .294 _refine_diff_density_min -.243 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 246 _refine_ls_number_reflns 2575 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all .073 _refine_ls_R_factor_gt .042 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0376P)^2^+1.9871P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .091 _reflns_number_gt 1848 _reflns_number_total 2575 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file qb0174.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 2936.3(11) _cod_database_code 2010757 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 P1 .20423(5) .09582(7) .62966(3) .02145(19) Uani d . 1 . . P S1 .05358(6) .16905(7) .72343(4) .0308(2) Uani d . 1 . . S O1 .18759(14) .22402(17) .60483(9) .0272(5) Uani d . 1 . . O C1 .0824(2) .0170(3) .62503(13) .0217(6) Uani d . 1 . . C C2 .0158(2) .0485(3) .66455(13) .0233(6) Uani d . 1 . . C C3 -.0805(2) -.0092(3) .65439(14) .0281(7) Uani d . 1 . . C C4 -.1118(2) -.0952(3) .60562(15) .0311(7) Uani d . 1 . . C C5 -.0485(2) -.1240(3) .56540(15) .0306(7) Uani d . 1 . . C C6 .0481(2) -.0697(3) .57568(14) .0264(7) Uani d . 1 . . C C7 .2751(2) .0048(3) .58403(13) .0226(6) Uani d . 1 . . C C8 .3053(3) -.1173(3) .59921(16) .0386(8) Uani d . 1 . . C C9 .3626(3) -.1794(4) .56282(18) .0473(9) Uani d . 1 . . C C10 .3890(3) -.1210(4) .51195(18) .0453(9) Uani d . 1 . . C C11 .3601(2) -.0010(3) .49675(16) .0376(8) Uani d . 1 . . C C12 .3035(2) .0618(3) .53276(14) .0271(7) Uani d . 1 . . C C13 .2822(2) .0876(3) .71241(13) .0224(6) Uani d . 1 . . C C14 .2890(2) -.0178(3) .75031(15) .0295(7) Uani d . 1 . . C C15 .3567(3) -.0215(3) .81182(15) .0337(8) Uani d . 1 . . C C16 .4173(2) .0798(3) .83487(16) .0369(8) Uani d . 1 . . C C17 .4101(2) .1852(3) .79789(16) .0371(8) Uani d . 1 . . C C18 .3428(2) .1892(3) .73651(14) .0272(7) Uani d . 1 . . C H3 -.125(2) .013(3) .6827(14) .038(9) Uiso d . 1 . . H H4 -.174(2) -.133(2) .5992(12) .016(7) Uiso d . 1 . . H H5 -.070(2) -.179(3) .5351(15) .039(9) Uiso d . 1 . . H H6 .091(2) -.089(3) .5485(14) .030(8) Uiso d . 1 . . H H8 .286(2) -.155(3) .6338(15) .040(9) Uiso d . 1 . . H H9 .381(2) -.265(3) .5737(15) .043(9) Uiso d . 1 . . H H10 .427(2) -.170(3) .4886(15) .043(9) Uiso d . 1 . . H H11 .379(2) .040(3) .4617(14) .032(8) Uiso d . 1 . . H H12 .286(2) .152(3) .5236(13) .025(8) Uiso d . 1 . . H H14 .248(2) -.087(3) .7335(13) .030(8) Uiso d . 1 . . H H15 .362(2) -.092(3) .8342(15) .038(9) Uiso d . 1 . . H H16 .467(2) .074(3) .8766(15) .039(9) Uiso d . 1 . . H H17 .450(2) .255(3) .8130(13) .030(8) Uiso d . 1 . . H H18 .336(2) .263(3) .7095(14) .035(8) Uiso d . 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 P1 .0202(4) .0219(4) .0230(4) -.0029(3) .0068(3) -.0001(3) S1 .0304(4) .0303(4) .0372(5) -.0072(3) .0185(3) -.0066(3) O1 .0265(10) .0226(11) .0333(11) -.0033(9) .0090(9) .0013(9) C1 .0184(13) .0235(15) .0213(15) -.0012(12) .0012(11) .0072(12) C2 .0233(15) .0218(15) .0242(15) -.0003(12) .0047(12) .0045(12) C3 .0216(15) .0334(18) .0301(17) -.0017(14) .0080(13) .0075(14) C4 .0198(15) .0375(18) .0316(17) -.0105(15) -.0019(13) .0092(15) C5 .0335(17) .0272(17) .0262(17) -.0077(14) -.0016(14) .0018(14) C6 .0259(15) .0315(18) .0217(15) -.0016(13) .0056(13) .0015(13) C7 .0202(14) .0251(16) .0219(15) -.0018(12) .0040(12) -.0029(12) C8 .052(2) .034(2) .0339(19) .0085(16) .0180(16) .0042(15) C9 .057(2) .035(2) .051(2) .0164(18) .0161(19) .0020(18) C10 .044(2) .052(2) .045(2) .0121(18) .0204(17) -.0075(18) C11 .0386(19) .048(2) .0312(18) -.0029(16) .0183(15) -.0009(16) C12 .0242(15) .0311(18) .0256(16) -.0025(13) .0054(12) -.0014(13) C13 .0210(14) .0245(15) .0237(14) -.0028(13) .0092(11) -.0045(13) C14 .0325(17) .0247(16) .0322(18) -.0038(14) .0097(14) .0002(14) C15 .0426(19) .0316(19) .0276(18) .0067(16) .0103(15) .0069(15) C16 .0302(17) .053(2) .0250(17) .0034(17) .0024(14) -.0025(17) C17 .0333(18) .044(2) .0329(19) -.0147(17) .0067(15) -.0090(16) C18 .0308(16) .0267(17) .0250(16) -.0051(13) .0088(13) -.0028(13) 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 P1 O1 . 1.478(2) ? P1 C7 . 1.800(3) ? P1 C13 . 1.801(3) ? P1 C1 . 1.806(3) ? S1 C2 . 1.786(3) ? S1 S1 2_556 2.0212(15) ? C1 C6 . 1.392(4) ? C1 C2 . 1.402(4) ? C2 C3 . 1.387(4) ? C3 C4 . 1.374(4) ? C4 C5 . 1.374(4) ? C5 C6 . 1.375(4) ? C7 C12 . 1.381(4) ? C7 C8 . 1.392(4) ? C8 C9 . 1.383(5) ? C9 C10 . 1.368(5) ? C10 C11 . 1.367(5) ? C11 C12 . 1.375(4) ? C13 C18 . 1.380(4) ? C13 C14 . 1.383(4) ? C14 C15 . 1.386(4) ? C15 C16 . 1.373(5) ? C16 C17 . 1.372(5) ? C17 C18 . 1.381(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' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 '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_site_symmetry_3 _geom_angle O1 P1 C7 . 111.84(12) O1 P1 C13 . 113.01(12) C7 P1 C13 . 104.33(12) O1 P1 C1 . 111.76(12) C7 P1 C1 . 107.00(13) C13 P1 C1 . 108.46(12) C2 S1 S1 2_556 106.02(9) C6 C1 C2 . 118.5(2) C6 C1 P1 . 118.5(2) C2 C1 P1 . 122.7(2) C3 C2 C1 . 119.3(3) C3 C2 S1 . 121.5(2) C1 C2 S1 . 119.1(2) C4 C3 C2 . 120.9(3) C5 C4 C3 . 120.2(3) C4 C5 C6 . 119.6(3) C5 C6 C1 . 121.4(3) C12 C7 C8 . 119.0(3) C12 C7 P1 . 117.4(2) C8 C7 P1 . 123.5(2) C9 C8 C7 . 119.8(3) C10 C9 C8 . 120.0(3) C11 C10 C9 . 120.8(3) C10 C11 C12 . 119.8(3) C11 C12 C7 . 120.7(3) C18 C13 C14 . 119.5(3) C18 C13 P1 . 117.4(2) C14 C13 P1 . 123.0(2) C13 C14 C15 . 120.2(3) C16 C15 C14 . 119.7(3) C17 C16 C15 . 120.4(3) C16 C17 C18 . 120.0(3) C13 C18 C17 . 120.2(3)