#------------------------------------------------------------------------------ #$Date: 2014-07-12 00:06:05 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120077 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/11/50/4115015.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_4115015 loop_ _publ_author_name 'Aroop K. Roy' 'Richard B. Taylor' _publ_contact_author_address ; Mail Stop 500, Dow Corning Corporation, Midland, MI 48686-0994 ; _publ_contact_author_email ' aroop.k.roy@dowcorning.com ' _publ_contact_author_fax ' 989-496-1016 ' _publ_contact_author_name ' Aroop K. Roy' _publ_contact_author_phone ' 989-496-6959 ' _publ_section_title ; The First Alkene-Platinum-Silyl Complexes: Lifting the Hydrosilation Mechanism Shroud with Long-Lived Precatalytic Intermediates and True Pt Catalysts ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 9510 _journal_page_last 9524 _journal_volume 124 _journal_year 2002 _chemical_formula_moiety 'C10 H18 Cl4 Pt Si2 ' _chemical_formula_sum 'C10 H18 Cl4 Pt Si2' _chemical_formula_weight 531.33 _space_group_IT_number 60 _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 60 _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_space_group_name_H-M 'P b c n' _audit_creation_date 2001-12-03 _audit_creation_method 'by teXsan for Windows v1.06' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.260(2) _cell_length_b 16.961(3) _cell_length_c 11.406(2) _cell_measurement_reflns_used 0 _cell_measurement_temperature 153.2 _cell_measurement_theta_max 0.0 _cell_measurement_theta_min 0.0 _cell_volume 1598.0(6) _computing_cell_refinement 'Bruker SAINT-1000 Diffractometer Control' _computing_data_collection 'Bruker SMART-1000 Diffractometer Control' _computing_data_reduction 'Bruker SAINT-1000 Diffractometer Control' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _diffrn_ambient_temperature 153.2 _diffrn_measurement_device 'SMART-1000 CCD' _diffrn_measurement_method \w _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 _diffrn_radiation_detector CCD _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.03326 _diffrn_reflns_av_sigmaI/netI 0.023 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 14332 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_reflns_theta_max 28.26 _diffrn_reflns_theta_min 1.20 _diffrn_standards_decay_% 0.00 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 9.541 _exptl_absorpt_correction_T_max 0.24722 _exptl_absorpt_correction_T_min 0.03495 _exptl_absorpt_correction_type 'aussian face-indexed' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.208 _exptl_crystal_description 'cut block' _exptl_crystal_F_000 1008.00 _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.00 _refine_diff_density_min 0.00 _refine_ls_extinction_coef 0.000000170(10) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_goodness_of_fit_all 2.222 _refine_ls_goodness_of_fit_ref 2.400 _refine_ls_matrix_type full _refine_ls_number_constraints 6 _refine_ls_number_parameters 95 _refine_ls_number_reflns 1637 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.024 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_all 0.0500 _refine_ls_wR_factor_ref 0.025 _reflns_number_gt 1637 _reflns_number_total 2241 _reflns_threshold_expression I>3.00\s(I) _[local]_cod_data_source_file ja0127335.cif _[local]_cod_data_source_block '_s78j' _[local]_cod_cif_authors_sg_H-M 'P b c n ' _[local]_cod_chemical_formula_sum_orig 'C10 H18 Cl4 Pt Si2 ' _cod_original_cell_volume 1597.9(4) _cod_database_code 4115015 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' 1/2-x,1/2-y,1/2+z '1/2+x,1/2-y, -z' ' -x, +y,1/2-z' ' -x, -y, -z' 1/2+x,1/2+y,1/2-z '1/2-x,1/2+y, +z' ' +x, -y,1/2+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_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag Pt(1) 1.0000 0.211457(7) 0.7500 0.01349(3) 1.000 ST Uani d Cl(1) 1.31237(12) 0.35211(6) 0.68180(9) 0.0255(6) 0.500 S Uiso d Cl(2) 0.96858(12) 0.40635(6) 0.59204(9) 0.0289(7) 0.500 S Uiso d Cl(3) 1.15090(9) 0.26735(4) 0.46090(6) 0.0307(2) 1.000 . Uani d Si(1) 1.09864(9) 0.30956(4) 0.62918(6) 0.0199(2) 1.000 . Uani d C(1) 0.9859(3) 0.1073(2) 0.8859(2) 0.0200(6) 1.000 . Uani d C(2) 0.8356(3) 0.1158(2) 0.8365(2) 0.0228(6) 1.000 . Uani d C(3) 0.7686(3) 0.0681(2) 0.7365(3) 0.0258(7) 1.000 . Uani d C(4) 0.8921(4) 0.0441(2) 0.6422(3) 0.0267(7) 1.000 . Uani d C(5) 1.3124 0.3521 0.6818 0.019(2) 0.500 S Uiso d C(6) 0.9686 0.4064 0.5920 0.008(2) 0.500 S Uiso d H(1) 1.004(3) 0.130(2) 0.950(2) 0.016(7) 1.000 . Uiso d H(2) 0.773(3) 0.150(2) 0.879(2) 0.016(7) 1.000 . Uiso d H(3) 0.674(4) 0.103(2) 0.696(3) 0.043(9) 1.000 . Uiso d H(4) 0.728(3) 0.020(2) 0.767(2) 0.021(7) 1.000 . Uiso d H(5) 0.841(3) 0.031(2) 0.570(2) 0.025(7) 1.000 . Uiso d H(6) 0.941(3) -0.002(2) 0.665(2) 0.021(7) 1.000 . Uiso d H(7) 1.0135 0.4224 0.5370 0.018 0.500 S Uiso d H(8) 0.9063 0.3895 0.5743 0.018 0.500 S Uiso d H(9) 0.9418 0.4285 0.6538 0.018 0.500 S Uiso d H(10) 1.3011 0.3634 0.7537 0.018 0.500 S Uiso d H(11) 1.3686 0.3076 0.6835 0.018 0.500 S Uiso d H(12) 1.3313 0.3860 0.6332 0.018 0.500 S Uiso d 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 Pt(1) 0.01506(6) 0.00846(6) 0.01696(6) 0.0000 0.00083(5) 0.0000 Cl(3) 0.0438(4) 0.0244(3) 0.0241(3) -0.0063(3) 0.0079(3) -0.0029(3) Si(1) 0.0266(4) 0.0120(3) 0.0212(3) -0.0038(3) 0.0047(3) -0.0007(3) C(1) 0.030(1) 0.0124(10) 0.0177(11) 0.0004(11) -0.0015(11) 0.0027(9) C(2) 0.0261(13) 0.0165(12) 0.0258(13) -0.0027(11) 0.0037(11) 0.0048(10) C(3) 0.0259(13) 0.0161(12) 0.035(2) -0.0096(11) -0.0036(12) 0.0039(12) C(4) 0.034(1) 0.0142(12) 0.032(2) -0.0020(12) -0.0060(13) -0.0015(11) loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 40 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 72 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 16 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Si 0 8 0.072 0.071 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pt 0 4 -2.352 8.388 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag SI1 PT1 SI1 87.79(6) . . . ? SI1 PT1 C1 162.10(10) . . . ? SI1 PT1 C1 97.48(10) . . . ? SI1 PT1 C2 163.40(10) . . . ? SI1 PT1 C2 92.48(11) . . . ? SI1 PT1 C1 97.48(10) 4_756 4_756 4_756 ? SI1 PT1 C1 162.10(10) 4_756 4_756 4_756 ? SI1 PT1 C2 92.48(11) 4_756 4_756 4_756 ? SI1 PT1 C2 163.40(10) 4_756 4_756 4_756 ? C1 PT1 C1 82.7(2) . . . ? C1 PT1 C2 34.02(13) . . . ? C1 PT1 C2 77.6(1) . . . ? C1 PT1 C2 77.6(1) 4_756 4_756 4_756 ? C1 PT1 C2 34.02(13) 4_756 4_756 4_756 ? C2 PT1 C2 92.0(2) . . . ? SI1 CL1 H10 106.0 . . . no SI1 CL1 H11 99.3 . . . no SI1 CL1 H12 102.7 . . . no H10 CL1 H11 103.2 . . . no H10 CL1 H12 121.4 . . . no H11 CL1 H12 121.1 . . . no SI1 CL2 H7 101.6 . . . no SI1 CL2 H8 97.8 . . . no SI1 CL2 H9 109.5 . . . no H7 CL2 H8 107.1 . . . no H7 CL2 H9 130.9 . . . no H8 CL2 H9 105.3 . . . no PT1 SI1 CL1 113.11(7) . . . ? PT1 SI1 CL2 121.77(7) . . . ? PT1 SI1 CL3 111.93(6) . . . ? CL1 SI1 CL2 103.93(8) . . . ? CL1 SI1 CL3 102.51(7) . . . ? CL2 SI1 CL3 101.33(7) . . . ? PT1 C1 C2 72.2(2) . . . ? PT1 C1 C4 111.2(3) . . . ? PT1 C1 H1 102.9(28) . . . no C2 C1 C4 126.4(4) . . . ? C2 C1 H1 117.9(26) . . . no C4 C1 H1 113.3(26) 4_756 4_756 4_756 no PT1 C2 C1 73.8(2) . . . ? PT1 C2 C3 105.5(3) . . . ? PT1 C2 H2 96.4(24) . . . no C1 C2 C3 126.1(4) . . . ? C1 C2 H2 111.3(24) . . . no C3 C2 H2 122.1(24) . . . no C2 C3 C4 115.4(4) . . . ? C2 C3 H3 107.4(25) . . . no C2 C3 H4 108.4(24) . . . no C4 C3 H3 109.0(26) . . . no C4 C3 H4 105.4(25) . . . no H3 C3 H4 111.4(34) . . . no C1 C4 C3 113.9(3) 4_756 4_756 4_756 ? C1 C4 H5 106.7(24) 4_756 4_756 4_756 no C1 C4 H6 111.6(25) 4_756 4_756 4_756 no C3 C4 H5 111.7(25) . . . no C3 C4 H6 109.0(25) . . . no H5 C4 H6 103.4(33) . . . no SI1 C5 H10 106.0 . . . no SI1 C5 H11 99.3 . . . no SI1 C5 H12 102.7 . . . no H10 C5 H11 103.2 . . . no H10 C5 H12 121.4 . . . no H11 C5 H12 121.1 . . . no SI1 C6 H7 101.6 . . . no SI1 C6 H8 97.8 . . . no SI1 C6 H9 109.5 . . . no H7 C6 H8 107.1 . . . no H7 C6 H9 130.9 . . . no H8 C6 H9 105.3 . . . no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag PT1 SI1 2.3090(11) ? PT1 SI1 2.3090(11) ? PT1 C1 2.353(4) ? PT1 C1 2.353(4) ? PT1 C2 2.334(4) ? PT1 C2 2.334(4) ? CL1 SI1 1.999(2) ? CL1 H10 0.85 no CL1 H11 0.89 no CL1 H12 0.81 no CL2 SI1 2.007(2) ? CL2 H7 0.78 no CL2 H8 0.62 no CL2 H9 0.83 no CL3 SI1 2.094(2) ? C1 C2 1.371(5) ? C1 C4 1.505(6) ? C1 H1 0.84(4) no C2 C3 1.504(6) ? C2 H2 0.92(4) no C3 C4 1.537(6) ? C3 H3 1.08(5) no C3 H4 0.95(4) no C4 H5 0.95(4) no C4 H6 0.92(4) no C5 H10 0.85 no C5 H11 0.89 no C5 H12 0.81 no C6 H7 0.78 no C6 H8 0.62 no C6 H9 0.83 no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag C5 H4 2.99(4) 6_556 no C5 C5 3.4681(6) 4_856 no H1 H12 2.5058 2_755 no H4 H9 2.4586 7_645 no H4 H12 2.6840 6_446 no H6 H12 2.6950 7_745 no H11 H11 2.6491 4_856 no 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 PT1 C1 C2 C3 97.7(4) no PT1 C1 C4 C3 10.5(5) no PT1 C1 C2 C3 97.7(4) no PT1 C1 C4 C3 10.5(5) no PT1 C2 C1 C4 -103.6(4) no PT1 C2 C3 C4 45.2(4) no PT1 C2 C1 C4 -103.6(4) no PT1 C2 C3 C4 45.2(4) no CL1 SI1 PT1 SI1 82.97(7) no CL1 SI1 PT1 C1 -24.8(3) no CL1 SI1 PT1 C1 -114.21(12) no CL1 SI1 PT1 C2 174.2(4) no CL1 SI1 PT1 C2 -80.42(12) no CL2 SI1 PT1 SI1 -41.94(7) no CL2 SI1 PT1 C1 -149.7(3) no CL2 SI1 PT1 C1 120.88(12) no CL2 SI1 PT1 C2 49.3(4) no CL2 SI1 PT1 C2 154.68(13) no CL3 SI1 PT1 SI1 -161.84(8) no CL3 SI1 PT1 C1 90.4(3) no CL3 SI1 PT1 C1 0.98(12) no CL3 SI1 PT1 C2 -70.6(4) no CL3 SI1 PT1 C2 34.78(12) no SI1 PT1 C1 C2 -170.4(3) no SI1 PT1 C1 C4 -47.5(5) no SI1 PT1 C1 C2 83.3(2) no SI1 PT1 C1 C4 -153.8(3) no SI1 PT1 C2 C1 169.7(3) no SI1 PT1 C2 C3 46.0(5) no SI1 PT1 C2 C1 -99.7(2) no SI1 PT1 C2 C3 136.6(3) no C1 PT1 C1 C2 -78.6(3) no C1 PT1 C1 C4 44.3(2) no C1 PT1 C2 C3 -123.7(4) no C1 PT1 C2 C3 -28.4(3) no C1 C2 PT1 C2 64.3(2) no C1 C2 C3 C4 -35.7(6) no C1 C4 C3 C2 -39.1(5) no C2 PT1 C1 C4 122.9(4) no C2 PT1 C1 C4 10.1(3) no C2 PT1 C2 C3 -59.4(2) no C2 C1 C4 C3 93.5(5) no C3 C2 C1 C4 -5.9(7) no _journal_paper_doi 10.1021/ja0127335