#------------------------------------------------------------------------------ #$Date: 2016-03-21 06:59:19 +0200 (Mon, 21 Mar 2016) $ #$Revision: 178543 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/06/49/4064960.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_4064960 loop_ _publ_author_name 'Kundu, Sabuj' 'Brennessel, William W.' 'Jones, William D.' _publ_section_title ; C--S Bond Activation of Thioesters Using Platinum(0) ; _journal_issue 19 _journal_name_full Organometallics _journal_page_first 5147 _journal_paper_doi 10.1021/om200452z _journal_volume 30 _journal_year 2011 _chemical_formula_moiety 'C16 H38 P2 Pt S2' _chemical_formula_sum 'C16 H38 P2 Pt S2' _chemical_formula_weight 551.61 _chemical_name_common jonsk22 _chemical_name_systematic ; (dippe)Pt(SMe)2 ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.427(5) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.306(3) _cell_length_b 13.148(3) _cell_length_c 15.890(4) _cell_measurement_reflns_used 3787 _cell_measurement_temperature 100.0(1) _cell_measurement_theta_max 28.16 _cell_measurement_theta_min 2.51 _cell_volume 2153.1(10) _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_collection 'APEX2 (Bruker, 2010)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _diffrn_ambient_temperature 100.0(1) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _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 0.1117 _diffrn_reflns_av_sigmaI/netI 0.0944 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 44053 _diffrn_reflns_theta_full 34.97 _diffrn_reflns_theta_max 34.97 _diffrn_reflns_theta_min 1.98 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 6.854 _exptl_absorpt_correction_T_max 0.7256 _exptl_absorpt_correction_T_min 0.4068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1096 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.351 _refine_diff_density_min -1.936 _refine_diff_density_rms 0.251 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 200 _refine_ls_number_reflns 9434 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.030 _refine_ls_R_factor_all 0.1010 _refine_ls_R_factor_gt 0.0554 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+4.5256P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.0966 _reflns_number_gt 6219 _reflns_number_total 9434 _reflns_threshold_expression >2sigma(I) _cod_data_source_file om200452z_si_002.cif _cod_data_source_block jonsk22_4a _cod_original_cell_volume 2153.1(9) _cod_database_code 4064960 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags Pt1 Pt 0.730705(18) 0.222491(15) 0.666973(12) 0.01894(5) Uani 1 1 d . P1 P 0.90298(12) 0.18167(11) 0.74701(9) 0.0206(3) Uani 1 1 d . P2 P 0.65142(12) 0.06818(10) 0.69644(8) 0.0188(3) Uani 1 1 d . S1 S 0.80095(15) 0.39372(11) 0.66298(9) 0.0304(3) Uani 1 1 d . S2 S 0.56825(13) 0.23902(11) 0.56235(8) 0.0253(3) Uani 1 1 d . C1 C 0.7916(7) 0.4396(5) 0.5555(4) 0.0387(15) Uani 1 1 d . H1A H 0.7637 0.5108 0.5554 0.058 Uiso 1 1 calc R H1B H 0.7289 0.3985 0.5237 0.058 Uiso 1 1 calc R H1C H 0.8772 0.4342 0.5294 0.058 Uiso 1 1 calc R C2 C 0.4778(6) 0.3537(5) 0.5834(4) 0.0342(14) Uani 1 1 d . H2A H 0.4099 0.3622 0.5405 0.051 Uiso 1 1 calc R H2B H 0.5365 0.4123 0.5822 0.051 Uiso 1 1 calc R H2C H 0.4379 0.3488 0.6391 0.051 Uiso 1 1 calc R C3 C 0.8722(5) 0.0617(4) 0.8022(3) 0.0250(11) Uani 1 1 d . H3A H 0.9551 0.0246 0.8096 0.030 Uiso 1 1 calc R H3B H 0.8374 0.0766 0.8587 0.030 Uiso 1 1 calc R C4 C 0.7747(5) -0.0067(4) 0.7535(3) 0.0211(10) Uani 1 1 d . H4A H 0.7309 -0.0527 0.7936 0.025 Uiso 1 1 calc R H4B H 0.8226 -0.0494 0.7128 0.025 Uiso 1 1 calc R C5 C 0.9553(5) 0.2706(5) 0.8297(3) 0.0250(11) Uani 1 1 d . H5 H 0.9887 0.3329 0.8009 0.030 Uiso 1 1 calc R C6 C 0.8411(5) 0.3038(4) 0.8836(4) 0.0304(13) Uani 1 1 d . H6A H 0.8701 0.3554 0.9240 0.046 Uiso 1 1 calc R H6B H 0.8070 0.2449 0.9141 0.046 Uiso 1 1 calc R H6C H 0.7729 0.3323 0.8474 0.046 Uiso 1 1 calc R C7 C 1.0659(6) 0.2294(6) 0.8844(4) 0.0391(15) Uani 1 1 d . H7A H 1.0937 0.2819 0.9245 0.059 Uiso 1 1 calc R H7B H 1.1391 0.2106 0.8486 0.059 Uiso 1 1 calc R H7C H 1.0360 0.1694 0.9153 0.059 Uiso 1 1 calc R C8 C 1.0504(5) 0.1559(5) 0.6850(3) 0.0267(12) Uani 1 1 d . H8 H 1.1176 0.1293 0.7250 0.032 Uiso 1 1 calc R C9 C 1.0279(6) 0.0747(5) 0.6194(4) 0.0402(16) Uani 1 1 d . H9A H 1.1076 0.0642 0.5873 0.060 Uiso 1 1 calc R H9B H 0.9580 0.0961 0.5812 0.060 Uiso 1 1 calc R H9C H 1.0034 0.0110 0.6471 0.060 Uiso 1 1 calc R C10 C 1.1055(7) 0.2503(5) 0.6451(5) 0.049(2) Uani 1 1 d . H10A H 1.1809 0.2320 0.6111 0.074 Uiso 1 1 calc R H10B H 1.1321 0.2982 0.6892 0.074 Uiso 1 1 calc R H10C H 1.0393 0.2820 0.6091 0.074 Uiso 1 1 calc R C11 C 0.5114(5) 0.0695(4) 0.7687(3) 0.0233(11) Uani 1 1 d . H11 H 0.4872 -0.0029 0.7797 0.028 Uiso 1 1 calc R C12 C 0.5498(5) 0.1172(5) 0.8537(3) 0.0280(12) Uani 1 1 d . H12A H 0.4741 0.1186 0.8906 0.042 Uiso 1 1 calc R H12B H 0.5808 0.1868 0.8446 0.042 Uiso 1 1 calc R H12C H 0.6189 0.0767 0.8799 0.042 Uiso 1 1 calc R C13 C 0.3938(5) 0.1212(5) 0.7314(4) 0.0306(13) Uani 1 1 d . H13A H 0.3208 0.1148 0.7703 0.046 Uiso 1 1 calc R H13B H 0.3712 0.0891 0.6776 0.046 Uiso 1 1 calc R H13C H 0.4129 0.1934 0.7222 0.046 Uiso 1 1 calc R C14 C 0.5976(5) -0.0156(4) 0.6104(3) 0.0239(11) Uani 1 1 d . H14 H 0.5175 0.0154 0.5853 0.029 Uiso 1 1 calc R C15 C 0.6992(5) -0.0211(5) 0.5404(3) 0.0282(12) Uani 1 1 d . H15A H 0.6656 -0.0627 0.4939 0.042 Uiso 1 1 calc R H15B H 0.7790 -0.0519 0.5626 0.042 Uiso 1 1 calc R H15C H 0.7179 0.0476 0.5199 0.042 Uiso 1 1 calc R C16 C 0.5617(7) -0.1225(5) 0.6403(4) 0.0365(15) Uani 1 1 d . H16A H 0.5351 -0.1639 0.5918 0.055 Uiso 1 1 calc R H16B H 0.4900 -0.1182 0.6803 0.055 Uiso 1 1 calc R H16C H 0.6371 -0.1539 0.6678 0.055 Uiso 1 1 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01872(8) 0.02018(9) 0.01792(8) -0.00064(9) 0.00008(6) 0.00082(9) P1 0.0169(6) 0.0243(7) 0.0207(7) -0.0025(5) -0.0006(5) -0.0014(5) P2 0.0162(6) 0.0223(6) 0.0178(6) -0.0016(5) -0.0006(5) 0.0010(5) S1 0.0385(8) 0.0231(7) 0.0295(8) 0.0016(6) -0.0039(6) -0.0054(6) S2 0.0276(6) 0.0275(7) 0.0208(6) 0.0002(5) -0.0042(5) 0.0045(5) C1 0.050(4) 0.039(4) 0.027(3) 0.008(3) 0.003(3) -0.007(3) C2 0.036(3) 0.038(4) 0.029(3) -0.004(3) -0.003(2) 0.011(3) C3 0.022(2) 0.030(3) 0.023(3) -0.003(2) 0.001(2) 0.001(2) C4 0.019(2) 0.021(2) 0.024(3) 0.000(2) 0.0002(19) 0.0037(19) C5 0.023(2) 0.031(3) 0.021(2) -0.001(2) 0.0021(19) -0.004(2) C6 0.030(3) 0.033(3) 0.028(3) -0.006(2) 0.000(2) -0.003(2) C7 0.031(3) 0.055(4) 0.031(3) -0.011(3) -0.007(2) -0.005(3) C8 0.016(2) 0.038(3) 0.027(3) -0.002(2) 0.005(2) 0.001(2) C9 0.038(3) 0.034(3) 0.049(4) -0.011(3) 0.021(3) -0.002(3) C10 0.046(4) 0.048(4) 0.054(4) -0.019(3) 0.022(3) -0.026(3) C11 0.020(2) 0.027(3) 0.023(3) 0.002(2) 0.001(2) -0.003(2) C12 0.022(3) 0.039(3) 0.022(3) -0.005(2) 0.005(2) 0.000(2) C13 0.015(2) 0.049(4) 0.028(3) -0.001(3) 0.001(2) 0.001(2) C14 0.021(2) 0.031(3) 0.020(3) -0.007(2) -0.0007(19) -0.001(2) C15 0.031(3) 0.033(3) 0.021(3) -0.009(2) 0.000(2) 0.003(2) C16 0.052(4) 0.031(3) 0.027(3) -0.005(2) -0.004(3) -0.016(3) 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' S S 0.1246 0.1234 '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 P2 Pt1 P1 87.31(5) P2 Pt1 S2 88.43(5) P1 Pt1 S2 167.49(5) P2 Pt1 S1 168.68(5) P1 Pt1 S1 90.11(5) S2 Pt1 S1 96.26(5) C3 P1 C5 104.9(3) C3 P1 C8 104.0(3) C5 P1 C8 105.1(2) C3 P1 Pt1 109.78(18) C5 P1 Pt1 118.72(19) C8 P1 Pt1 113.10(19) C14 P2 C4 104.4(2) C14 P2 C11 103.6(2) C4 P2 C11 103.8(2) C14 P2 Pt1 119.73(19) C4 P2 Pt1 109.66(17) C11 P2 Pt1 114.12(19) C1 S1 Pt1 109.1(2) C2 S2 Pt1 108.1(2) S1 C1 H1A 109.5 S1 C1 H1B 109.5 H1A C1 H1B 109.5 S1 C1 H1C 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 S2 C2 H2A 109.5 S2 C2 H2B 109.5 H2A C2 H2B 109.5 S2 C2 H2C 109.5 H2A C2 H2C 109.5 H2B C2 H2C 109.5 C4 C3 P1 112.0(4) C4 C3 H3A 109.2 P1 C3 H3A 109.2 C4 C3 H3B 109.2 P1 C3 H3B 109.2 H3A C3 H3B 107.9 C3 C4 P2 112.2(4) C3 C4 H4A 109.2 P2 C4 H4A 109.2 C3 C4 H4B 109.2 P2 C4 H4B 109.2 H4A C4 H4B 107.9 C6 C5 C7 111.0(5) C6 C5 P1 111.1(4) C7 C5 P1 113.3(4) C6 C5 H5 107.1 C7 C5 H5 107.1 P1 C5 H5 107.1 C5 C6 H6A 109.5 C5 C6 H6B 109.5 H6A C6 H6B 109.5 C5 C6 H6C 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 C5 C7 H7A 109.5 C5 C7 H7B 109.5 H7A C7 H7B 109.5 C5 C7 H7C 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 C10 C8 C9 110.4(5) C10 C8 P1 112.8(4) C9 C8 P1 112.0(4) C10 C8 H8 107.1 C9 C8 H8 107.1 P1 C8 H8 107.1 C8 C9 H9A 109.5 C8 C9 H9B 109.5 H9A C9 H9B 109.5 C8 C9 H9C 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 C8 C10 H10A 109.5 C8 C10 H10B 109.5 H10A C10 H10B 109.5 C8 C10 H10C 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 C13 C11 C12 111.2(5) C13 C11 P2 112.9(4) C12 C11 P2 110.6(4) C13 C11 H11 107.3 C12 C11 H11 107.3 P2 C11 H11 107.3 C11 C12 H12A 109.5 C11 C12 H12B 109.5 H12A C12 H12B 109.5 C11 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C11 C13 H13A 109.5 C11 C13 H13B 109.5 H13A C13 H13B 109.5 C11 C13 H13C 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 C16 C14 C15 110.4(5) C16 C14 P2 113.1(4) C15 C14 P2 111.4(4) C16 C14 H14 107.2 C15 C14 H14 107.2 P2 C14 H14 107.2 C14 C15 H15A 109.5 C14 C15 H15B 109.5 H15A C15 H15B 109.5 C14 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 C14 C16 H16A 109.5 C14 C16 H16B 109.5 H16A C16 H16B 109.5 C14 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Pt1 P2 2.2381(14) Pt1 P1 2.2414(14) Pt1 S2 2.3606(14) Pt1 S1 2.3659(15) P1 C3 1.833(6) P1 C5 1.838(6) P1 C8 1.848(5) P2 C14 1.838(5) P2 C4 1.840(5) P2 C11 1.850(5) S1 C1 1.812(6) S2 C2 1.805(6) C1 H1A 0.9800 C1 H1B 0.9800 C1 H1C 0.9800 C2 H2A 0.9800 C2 H2B 0.9800 C2 H2C 0.9800 C3 C4 1.552(7) C3 H3A 0.9900 C3 H3B 0.9900 C4 H4A 0.9900 C4 H4B 0.9900 C5 C6 1.524(7) C5 C7 1.528(8) C5 H5 1.0000 C6 H6A 0.9800 C6 H6B 0.9800 C6 H6C 0.9800 C7 H7A 0.9800 C7 H7B 0.9800 C7 H7C 0.9800 C8 C10 1.507(9) C8 C9 1.509(8) C8 H8 1.0000 C9 H9A 0.9800 C9 H9B 0.9800 C9 H9C 0.9800 C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 C11 C13 1.507(7) C11 C12 1.538(7) C11 H11 1.0000 C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800 C14 C16 1.530(8) C14 C15 1.535(7) C14 H14 1.0000 C15 H15A 0.9800 C15 H15B 0.9800 C15 H15C 0.9800 C16 H16A 0.9800 C16 H16B 0.9800 C16 H16C 0.9800 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 P2 Pt1 P1 C3 -8.84(19) S2 Pt1 P1 C3 -79.1(3) S1 Pt1 P1 C3 160.13(19) P2 Pt1 P1 C5 -129.4(2) S2 Pt1 P1 C5 160.4(3) S1 Pt1 P1 C5 39.6(2) P2 Pt1 P1 C8 106.9(2) S2 Pt1 P1 C8 36.6(3) S1 Pt1 P1 C8 -84.2(2) P1 Pt1 P2 C14 -128.1(2) S2 Pt1 P2 C14 40.1(2) S1 Pt1 P2 C14 154.9(3) P1 Pt1 P2 C4 -7.54(18) S2 Pt1 P2 C4 160.69(18) S1 Pt1 P2 C4 -84.5(3) P1 Pt1 P2 C11 108.38(19) S2 Pt1 P2 C11 -83.39(19) S1 Pt1 P2 C11 31.4(3) P2 Pt1 S1 C1 -149.8(3) P1 Pt1 S1 C1 133.4(2) S2 Pt1 S1 C1 -35.8(2) P2 Pt1 S2 C2 124.4(2) P1 Pt1 S2 C2 -165.5(3) S1 Pt1 S2 C2 -45.3(2) C5 P1 C3 C4 155.5(4) C8 P1 C3 C4 -94.4(4) Pt1 P1 C3 C4 26.9(4) P1 C3 C4 P2 -33.5(5) C14 P2 C4 C3 155.4(4) C11 P2 C4 C3 -96.4(4) Pt1 P2 C4 C3 25.9(4) C3 P1 C5 C6 -73.8(4) C8 P1 C5 C6 176.9(4) Pt1 P1 C5 C6 49.2(5) C3 P1 C5 C7 51.9(5) C8 P1 C5 C7 -57.4(5) Pt1 P1 C5 C7 174.9(3) C3 P1 C8 C10 -170.8(5) C5 P1 C8 C10 -60.9(5) Pt1 P1 C8 C10 70.1(5) C3 P1 C8 C9 63.9(5) C5 P1 C8 C9 173.8(5) Pt1 P1 C8 C9 -55.2(5) C14 P2 C11 C13 -66.9(5) C4 P2 C11 C13 -175.8(4) Pt1 P2 C11 C13 64.9(4) C14 P2 C11 C12 167.7(4) C4 P2 C11 C12 58.9(4) Pt1 P2 C11 C12 -60.4(4) C4 P2 C14 C16 49.9(5) C11 P2 C14 C16 -58.5(5) Pt1 P2 C14 C16 173.0(3) C4 P2 C14 C15 -75.1(4) C11 P2 C14 C15 176.5(4) Pt1 P2 C14 C15 48.0(5)