#------------------------------------------------------------------------------ #$Date: 2012-02-03 18:16:24 +0100 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/33/2003368.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_2003368 loop_ _publ_author_name 'Francisco, R. H. P.' 'Gambardella, M. T. P.' 'Rodrigues, A. M. G. D.' 'de Souza, G. F.' 'Filgueiras, C. A. L.' _publ_section_title ; The Dimer [PtCl~2~{P(C~2~H~5~)~3~}{(C~6~H~5~)SOCH~2~}]~2~ ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 604 _journal_page_last 606 _journal_volume 51 _journal_year 1995 _chemical_formula_moiety 'C26 H44 Cl4 O2 P2 Pt2 S2' _chemical_formula_sum 'C26 H44 Cl4 O2 P2 Pt2 S2' _chemical_formula_weight 1046.7 _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _atom_type_scat_source IntTabIV _cell_angle_alpha 90. _cell_angle_beta 90. _cell_angle_gamma 90. _cell_formula_units_Z 4 _cell_length_a 12.835(3) _cell_length_b 17.596(3) _cell_length_c 16.015(3) _cell_measurement_reflns_used 21 _cell_measurement_temperature 298 _cell_measurement_theta_max 13 _cell_measurement_theta_min 9 _cell_volume 3616.9(12) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3900 _diffrn_reflns_theta_max 25 _diffrn_standards_decay_% 0.9 _diffrn_standards_interval_time 60 _diffrn_standards_number 20 _exptl_absorpt_coefficient_mu 1.6655 _exptl_absorpt_correction_T_max 1.198 _exptl_absorpt_correction_T_min 0.313 _exptl_absorpt_correction_type empirical _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 3.844 _exptl_crystal_description 'White block' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _refine_diff_density_max 1.57 _refine_diff_density_min -1.85 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 0.89 _refine_ls_hydrogen_treatment refxyz _refine_ls_number_parameters 181 _refine_ls_number_reflns 1906 _refine_ls_R_factor_obs 0.0383 _refine_ls_shift/esd_max 0.01 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'w = 1.00/[\s^2^(F) + 0.00637F^2^]' _refine_ls_wR_factor_obs 0.0428 _reflns_number_observed 1889 _reflns_number_total 2794 _reflns_observed_criterion F>=6\s(F) _[local]_cod_data_source_file mu1113.cif _[local]_cod_data_source_block mu1113a _cod_original_cell_volume 3617.0(10) _cod_database_code 2003368 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,y,1/2-z x,1/2-y,1/2+z 1/2-x,1/2+y,z -x,-y,-z 1/2-x,-y,1/2+z -x,1/2+y,1/2-z 1/2+x,1/2-y,-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_B_iso_or_equiv Pt .20831(3) .11835(2) .03934(3) 2.37(2) S .0516(2) .0878(2) .0861(2) 2.47(8) P .1852(3) .2443(2) .0636(2) 3.0(1) Cl1 .3654(3) .1468(2) -.0225(2) 4.4(1) Cl2 .2508(3) -.0104(2) .0186(2) 3.9(1) O -.0316(7) .1434(5) .0686(5) 3.6(3) C1 .054(1) .0646(6) .1944(6) 2.9(4) C2 -.035(1) .0784(7) .2388(8) 4.2(5) C3 -.036(2) .0577(8) .3240(8) 4.9(6) C4 .049(1) .0245(8) .3597(8) 4.7(5) C5 .135(1) .0105(9) .3115(9) 5.5(6) C6 .140(1) .0304(9) .2298(9) 5.0(6) C7 .100(1) .2662(6) .1508(9) 4.7(5) C8 .096(2) .3486(7) .179(1) 6.1(7) C9 .306(1) .2938(8) .089(1) 4.5(5) C10 .361(2) .266(1) .165(1) 9.(1) C11 .129(2) .2940(8) -.0239(9) 6.3(6) C12 .179(2) .282(1) -.106(1) 7.4(8) C13 .008(1) -.0024(6) .0475(6) 2.5(3) H2 -.102(1) .1044(7) .2098(8) ? H3 -.105(1) .0683(8) .3611(8) ? H4 .048(1) .0093(8) .4250(8) ? H5 .202(1) -.0172(9) .3397(9) ? H6 .210(1) .0200(9) .1935(9) ? H7A .126(1) .2323(6) .2033(9) ? H7B .022(1) .2497(6) .1333(9) ? H8A .051(2) .3608(7) .235(1) ? H8B .074(2) .3874(7) .130(1) ? H8C .178(2) .3552(7) .193(1) ? H9A .287(1) .3531(8) .099(1) ? H9B .358(1) .2880(8) .037(1) ? H10A .435(2) .294(1) .163(1) ? H10B .372(2) .205(1) .159(1) ? H10C .323(2) .278(1) .224(1) ? H11A .131(2) .3541(8) -.0102(9) ? H11B .049(2) .2759(8) -.0294(9) ? H12A .162(2) .317(1) -.160(1) ? H12B .181(2) .223(1) -.124(1) ? H12C .254(2) .299(1) -.080(1) ? H13A .067(1) -.0448(6) .0592(6) ? H13B -.0633(1) -.0183(6) .0790(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 S Pt P 93.40(10) yes S Pt Cl2 91.40(10) yes Cl1 Pt Cl2 86.90(10) yes Cl1 Pt P 88.60(10) yes S Pt Cl1 174.3(3) yes P Pt Cl2 173.90(10) yes Pt P C7 114.7(4) yes Pt P C9 113.2(5) yes Pt P C11 113.1(5) yes Pt S O 115.6(4) yes Pt S C13 112.4(4) yes Pt S C1 111.7(4) yes O S C1 110.4(5) yes O S C13 107.2(5) yes C1 S C13 97.9(5) yes C7 P C9 103.8(7) yes C7 P C11 104.7(7) yes C9 P C11 106.4(7) yes C1 C2 C3 118.0(10) no C2 C3 C4 120.0(10) no C3 C4 C5 119.0(10) no C4 C5 C6 122.0(10) no C1 C6 C5 118.0(10) no C2 C1 C6 122.0(10) no S C1 C2 116.8(9) no S C1 C6 121.0(10) no P C7 C8 117.0(10) no P C9 C10 115.0(10) no P C11 C12 117.0(10) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Pt S 2.212(3) yes Pt P 2.270(3) yes Pt Cl1 2.302(3) yes Pt Cl2 2.353(3) yes S O 1.475(9) yes S C1 1.780(10) yes S C13 1.790(10) yes P C7 1.820(10) yes P C9 1.820(10) yes P C11 1.800(10) yes C1 C2 1.37(2) no C2 C3 1.41(2) no C3 C4 1.36(2) no C4 C5 1.37(2) no C5 C6 1.36(2) no C1 C6 1.38(2) no C7 C8 1.52(2) no C9 C10 1.49(3) no C11 C12 1.48(2) no