#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/52/2005224.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_2005224 loop_ _publ_author_name 'Boag, N. M.' 'Ravetz, M. S.' _publ_section_title trans-Di-\m-chloro-bis[chloro(trimethylphosphine-P)platinum(II)] _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1942 _journal_page_last 1943 _journal_volume 52 _journal_year 1996 _chemical_formula_analytical 'C10.53 H2.63 Cl20.76 P9.06 Pt57.02' _chemical_formula_iupac '[Pt2 Cl4 (C3 H9 P1)2]' _chemical_formula_moiety 'C3 H9 Cl2 P Pt' _chemical_formula_structural 'Pt P (CH3)3 Cl2' _chemical_formula_sum 'C3 H9 Cl2 P Pt' _chemical_formula_weight 684.12 _chemical_name_systematic ; trans-Di-mu-chloro-dichlorobis(trimethylphosphine)diplatinum(II) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _audit_creation_method SHELXL _cell_angle_alpha 90 _cell_angle_beta 105.36(1) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 6.594(1) _cell_length_b 10.763(2) _cell_length_c 11.649(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 30 _cell_measurement_theta_min 15 _cell_volume 797.2(2) _computing_cell_refinement 'P3 software' _computing_data_collection 'P3 software' _computing_data_reduction 'XDISK (Siemens, 1991)' _computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 1987)' _computing_publication_material SHELXL93 _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Nicolet R3m/V diffractometer with locally modified \y box' _diffrn_measurement_method 'profile data from \q/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 0.0990 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 2668 _diffrn_reflns_theta_max 28.07 _diffrn_reflns_theta_min 2.62 _diffrn_standards_decay_% none _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 18.367 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.261 _exptl_absorpt_correction_type 'semi-empirical via \y scan (SHELXTL-Plus; Sheldrick, 1987)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.85 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description 'rhombohedral block' _exptl_crystal_F_000 616 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _refine_diff_density_max 2.14 _refine_diff_density_min -1.62 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.032 _refine_ls_goodness_of_fit_obs 1.063 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 67 _refine_ls_number_reflns 1936 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.032 _refine_ls_restrained_S_obs 1.063 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_obs 0.0426 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0618P)^2^] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_wR_factor_all 0.1131 _refine_ls_wR_factor_obs 0.1014 _reflns_number_observed 1479 _reflns_number_total 1936 _reflns_observed_criterion I>2sigma(I) _[local]_cod_data_source_file bm1079.cif _[local]_cod_data_source_block meg3a _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2005224 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_occupancy _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_type_symbol Pt1 1 .11762(6) .10541(4) .11383(3) .0335(2) Uani d . Pt Cl1 1 -0.1500(5) -.0395(4) .0794(3) .0600(9) Uani d . Cl Cl2 1 .3836(5) .2455(4) .1314(3) .0578(8) Uani d . Cl P1 1 .0863(4) .1609(3) .2905(2) .0359(6) Uani d . P C1 1 .040(2) .324(1) .301(1) .064(4) Uani d . C H1A 1 .15(1) .370(1) .279(9) .096 Uiso calc R H H1B 1 .04(2) .345(2) .381(2) .096 Uiso calc R H H1C 1 -.094(8) .345(2) .248(7) .096 Uiso calc R H C2 1 -0.119(2) .085(1) .337(1) .057(3) Uani d . C H2A 1 -.095(9) -.004(2) .341(9) .086 Uiso calc R H H2B 1 -0.252(3) .102(8) .282(5) .086 Uiso calc R H H2C 1 -0.12(1) .114(7) .415(4) .086 Uiso calc R H C3 1 .318(2) .127(2) .409(1) .067(4) Uani d . C H3A 1 .427(6) .185(7) .407(6) .101 Uiso calc R H H3B 1 .37(1) .044(4) .400(6) .101 Uiso calc R H H3C 1 .285(5) .13(1) .485(1) .101 Uiso calc R 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 Pt1 0.0417(2) 0.0356(2) 0.0246(2) -0.0020(2) 0.01109(14) -0.0001(2) Cl1 0.074(2) 0.078(2) 0.0382(14) -0.034(2) 0.0329(13) -0.019(2) Cl2 0.065(2) 0.063(2) 0.0488(15) -0.0247(15) 0.0212(13) -0.004(2) P1 0.0451(13) 0.0355(14) 0.0282(12) 0.0022(11) 0.0115(10) -0.0017(12) C1 0.087(9) 0.038(6) 0.073(9) 0.023(6) 0.032(7) -0.013(7) C2 0.063(8) 0.073(10) 0.042(6) -0.003(6) 0.026(5) -0.013(7) C3 0.062(7) 0.105(13) 0.031(6) 0.006(8) 0.006(5) -0.005(8) 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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 _geom_angle_publ_flag P1 Pt1 Cl2 . 89.81(11) yes P1 Pt1 Cl1 . 95.10(10) yes Cl2 Pt1 Cl1 . 175.06(11) ? P1 Pt1 Cl1 3 178.67(11) ? Cl2 Pt1 Cl1 3 91.28(11) yes Cl1 Pt1 Cl1 3 83.81(10) yes Pt1 Cl1 Pt1 3 96.19(10) yes C2 P1 C1 . 106.0(7) ? C2 P1 C3 . 103.2(7) ? C1 P1 C3 . 105.7(7) ? C2 P1 Pt1 . 115.2(4) ? C1 P1 Pt1 . 112.8(5) ? C3 P1 Pt1 . 113.0(5) ? 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 Pt1 P1 . 2.205(3) yes Pt1 Cl2 . 2.281(3) yes Pt1 Cl1 . 2.309(3) yes Pt1 Cl1 3 2.423(3) yes Cl1 Pt1 3 2.423(3) no P1 C2 . 1.789(13) ? P1 C1 . 1.791(12) ? P1 C3 . 1.806(12) ?