#------------------------------------------------------------------------------ #$Date: 2009-11-14 14:09:05 +0100 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003303.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003303 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 611 _journal_page_last 613 _publ_section_title ; The trans Influence of the Silyl Ligand. Structure of trans-PtCl(PMe~2~Ph)~2~(SiPh~3~) ; _chemical_formula_sum 'C34 H37 Cl P2 Pt Si' _chemical_formula_weight 766.26 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' '1/2-x, -y,1/2+z' ' -x, -y, -z' '1/2-x,1/2+y, +z' ' +x,1/2-y,1/2+z' '1/2+x, +y,1/2-z' _symmetry_space_group_name_H-M 'P b c a' _cell_length_a 10.716(1) _cell_length_b 17.431(4) _cell_length_c 35.029(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6543(1) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_meas ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _cell_measurement_reflns_used 39 _cell_measurement_theta_min 19.2 _cell_measurement_theta_max 51.1 _exptl_absorpt_coefficient_mu 4.569 _cell_measurement_temperature 295 _exptl_crystal_description 'prism' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.260 _exptl_crystal_size_min 0.250 _exptl_crystal_colour 'yellow' _chemical_compound_source ;The title compound was prepared by the interaction of cis-[PtCl~2~(PMe~2~Ph)~2~] with triphenylsilane in boiling benzene--triethylamine solution (Chatt, Earborn, Ibekwe & Kapoor, 1967). Single crystals were formed on cooling to room temperature. ; _diffrn_measurement_device 'CAD-4' _diffrn_measurement_method '\w/2\q' _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.266 _exptl_absorpt_correction_T_max 0.374 _diffrn_reflns_number 7109 _reflns_number_total 7109 _reflns_number_observed 3526 _reflns_observed_criterion I>3\s(I) _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 26.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 43 _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% -2.10 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.0299 _refine_ls_wR_factor_obs 0.0336 _refine_ls_wR_factor_all ? _refine_ls_goodness_of_fit_obs 1.302 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 3526 _refine_ls_number_parameters 379 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme 'w = 1/[\s^2^(F)]' _refine_ls_shift/esd_max 0.0094 _refine_diff_density_max 1.26590 _refine_diff_density_min -0.73613 _refine_ls_extinction_method none _refine_ls_extinction_coef 0 loop_ _atom_type_symbol _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag Pt 'International Tables' -2.352 8.388 Cl 'International Tables' 0.132 0.159 Si 'International Tables' 0.072 0.071 P 'International Tables' 0.090 0.095 C 'International Tables' 0.002 0.002 H 'International Tables' 0.000 0.000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Pt 0.34567(2) 0.05467(1) 0.64573(7) 2.78(1) Cl 0.5290(2) 0.0063(1) 0.68073(5) 5.2(1) P(1) 0.4743(2) 0.0734(1) 0.59466(5) 4.2(1) P(2) 0.2452(2) 0.0533(1) 0.70446(5) 3.43(8) Si 0.1623(2) 0.0703(1) 0.61136(5) 2.76(8) C(10) 0.4383(7) 0.1422(4) 0.5584(2) 4.0(4) C(11) 0.467(1) 0.1316(5) 0.5201(2) 5.9(5) C(12) 0.446(1) 0.1882(6) 0.4936(3) 8.5(7) C(13) 0.393(2) 0.2551(7) 0.5049(4) 12(1) C(14) 0.360(2) 0.2666(6) 0.5419(4) 12(1) C(15) 0.383(1) 0.2109(5) 0.5688(2) 7.2(6) C(16) 0.6229(8) 0.1187(9) 0.6110(3) 10.5(8) C(17) 0.516(1) -0.0138(8) 0.5701(3) 8.5(8) C(20) 0.3055(6) 0.1332(5) 0.7327(2) 3.7(3) C(21) 0.3874(8) 0.1850(5) 0.7176(2) 4.9(4) C(22) 0.426(1) 0.2477(6) 0.7384(3) 6.7(6) C(23) 0.386(1) 0.2612(6) 0.7735(3) 6.9(6) C(24) 0.307(1) 0.2073(7) 0.7902(3) 7.2(6) C(25) 0.2673(8) 0.1433(6) 0.7699(2) 5.6(5) C(26) 0.0785(7) 0.0666(6) 0.7099(2) 4.9(5) C(27) 0.273(1) -0.0325(6) 0.7327(3) 5.5(5) C(30) 0.0803(7) 0.1657(4) 0.6186(2) 3.5(3) C(31) 0.1322(7) 0.2227(4) 0.6412(2) 4.4(4) C(32) 0.073(1) 0.2922(5) 0.6462(3) 6.1(5) C(33) -0.036(1) 0.3072(6) 0.6289(3) 7.1(6) C(34) -0.092(1) 0.2525(7) 0.6063(3) 6.4(5) C(35) -0.0318(8) 0.1820(5) 0.6009(2) 5.1(4) C(40) 0.0555(6) -0.0110(4) 0.6266(2) 3.2(3) C(41) 0.1066(8) -0.0837(5) 0.6335(2) 4.4(4) C(42) 0.032(1) -0.1445(5) 0.6459(3) 6.8(5) C(43) -0.093(1) -0.1341(6) 0.6515(3) 6.4(6) C(44) -0.1446(8) -0.0644(6) 0.6446(3) 6.2(5) C(45) -0.0719(7) -0.0044(5) 0.6325(2) 4.4(4) C(50) 0.1689(6) 0.0566(5) 0.5576(2) 4.1(3) C(51) 0.1429(8) 0.1120(6) 0.5315(2) 6.4(5) C(52) 0.141(1) 0.100(1) 0.4927(3) 10(1) C(53) 0.166(1) 0.031(1) 0.4790(3) 10(1) C(54) 0.192(1) -0.028(1) 0.5025(4) 11(1) C(55) 0.194(1) -0.0136(6) 0.5423(2) 7.1(6) H(1) 0.050(7) 0.112(4) 0.693(2) 5.5 H(2) 0.062(7) 0.072(4) 0.733(2) 5.5 H(3) 0.034(7) 0.026(4) 0.704(2) 5.5 H(4) 0.357(7) -0.038(5) 0.736(2) 6.3 H(5) 0.230(8) -0.074(4) 0.719(2) 6.3 H(6) 0.245(8) -0.023(5) 0.757(2) 6.3 H(7) 0.5022 0.0842 0.5121 7.1 H(8) 0.4683 0.1804 0.4676 10.2 H(9) 0.3795 0.2946 0.4867 15.0 H(10) 0.3215 0.3133 0.5493 14.8 H(11) 0.3604 0.2195 0.5947 8.6 H(12) 0.4182 0.1777 0.6924 5.9 H(13) 0.4833 0.2825 0.7272 8.1 H(14) 0.4102 0.3062 0.7869 8.3 H(15) 0.2793 0.2144 0.8158 8.7 H(16) 0.2143 0.1066 0.7817 6.8 H(17) 0.2099 0.2137 0.6535 5.3 H(18) 0.1102 0.3300 0.6621 7.3 H(19) -0.0745 0.3557 0.6322 8.6 H(20) -0.1697 0.2625 0.5945 7.7 H(21) -0.0691 0.1446 0.5848 6.1 H(22) 0.1933 -0.0918 0.6297 5.2 H(23) 0.0683 -0.1934 0.6505 8.1 H(24) -0.1433 -0.1754 0.6601 7.7 H(25) -0.2316 -0.0572 0.6482 7.5 H(26) -0.1106 0.0438 0.6279 5.2 H(27) 0.1253 0.1622 0.5405 7.7 H(28) 0.1205 0.1404 0.4758 12.3 H(29) 0.1662 0.0228 0.4522 12.3 H(30) 0.2082 -0.0775 0.4927 13.1 H(31) 0.2130 -0.0548 0.5590 8.5 H(34) 0.425(9) -0.036(5) 0.550(3) 9.1 H(35) 0.54(1) -0.045(6) 0.586(3) 9.1 H(36) 0.58(1) -0.005(6) 0.557(3) 9.1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Pt 0.0275(1) 0.0004(2) 0.0012(1) 0.0489(2) -0.0037(1) 0.0291(1) Cl 0.042(1) 0.019(1) -0.010(1) 0.107(2) -0.003(1) 0.051(1) P(1) 0.034(1) 0.001(1) 0.0068(9) 0.084(2) 0.002(1) 0.039(1) P(2) 0.037(1) -0.000(1) 0.0039(8) 0.062(1) 0.000(1) 0.0314(8) Si 0.032(1) -0.001(1) -0.0020(9) 0.039(1) -0.0009(8) 0.034(1) C(10) 0.055(5) -0.010(4) 0.017(4) 0.052(5) 0.003(4) 0.046(4) C(11) 0.091(7) 0.004(6) 0.020(5) 0.076(6) 0.005(5) 0.059(5) C(12) 0.16(1) 0.025(8) 0.050(8) 0.082(8) 0.023(7) 0.086(7) C(13) 0.28(2) 0.04(1) 0.11(1) 0.074(8) 0.041(7) 0.12(1) C(14) 0.30(2) 0.03(1) 0.12(1) 0.050(6) 0.017(7) 0.12(1) C(15) 0.15(1) -0.017(6) 0.050(6) 0.054(6) -0.003(5) 0.064(6) C(16) 0.048(6) -0.060(8) -0.011(5) 0.27(2) 0.03(1) 0.086(8) C(17) 0.15(1) 0.07(1) 0.057(8) 0.11(1) 0.019(6) 0.066(7) C(20) 0.038(4) 0.005(4) -0.007(3) 0.066(5) -0.009(4) 0.036(4) C(21) 0.067(5) -0.012(5) 0.006(4) 0.076(6) -0.014(4) 0.043(4) C(22) 0.101(8) -0.026(6) -0.007(6) 0.090(7) -0.015(5) 0.064(6) C(23) 0.110(9) 0.008(6) -0.027(6) 0.082(7) -0.027(6) 0.070(7) C(24) 0.092(8) 0.019(7) -0.006(5) 0.13(1) -0.044(6) 0.057(6) C(25) 0.056(5) -0.000(5) 0.008(4) 0.112(8) -0.022(5) 0.045(5) C(26) 0.037(4) -0.007(5) 0.005(4) 0.111(9) -0.005(5) 0.037(4) C(27) 0.081(7) 0.001(6) 0.007(6) 0.076(7) 0.007(5) 0.052(5) C(30) 0.047(4) 0.007(4) 0.007(4) 0.043(4) 0.006(4) 0.044(4) C(31) 0.067(5) -0.007(4) 0.014(4) 0.046(4) -0.002(4) 0.055(5) C(32) 0.094(7) -0.009(5) 0.034(7) 0.034(5) -0.011(5) 0.102(7) C(33) 0.11(1) 0.038(7) 0.051(8) 0.055(6) 0.025(6) 0.104(9) C(34) 0.072(6) 0.029(6) 0.022(6) 0.087(7) 0.043(6) 0.085(7) C(35) 0.063(5) 0.015(5) 0.002(5) 0.067(6) 0.012(5) 0.062(5) C(40) 0.039(4) -0.007(4) -0.002(3) 0.041(4) -0.001(4) 0.042(4) C(41) 0.057(5) 0.009(4) 0.003(4) 0.051(5) 0.012(4) 0.058(5) C(42) 0.100(8) -0.006(5) 0.014(7) 0.041(5) 0.010(6) 0.116(8) C(43) 0.086(7) -0.035(6) 0.014(6) 0.068(7) 0.012(6) 0.089(7) C(44) 0.044(5) -0.023(5) -0.003(5) 0.094(7) 0.009(7) 0.098(7) C(45) 0.033(4) -0.009(4) -0.006(4) 0.068(6) 0.004(4) 0.065(5) C(50) 0.033(4) -0.013(5) 0.001(3) 0.083(5) -0.007(4) 0.039(4) C(51) 0.073(6) 0.016(6) 0.008(5) 0.128(8) 0.018(5) 0.042(5) C(52) 0.083(8) 0.04(1) 0.009(7) 0.26(2) 0.03(1) 0.051(7) C(53) 0.076(9) -0.05(1) 0.013(6) 0.27(2) -0.02(1) 0.047(7) C(54) 0.15(1) -0.11(1) 0.058(9) 0.18(1) -0.07(1) 0.092(9) C(55) 0.106(8) -0.042(7) 0.041(5) 0.107(8) -0.029(6) 0.058(6)