#------------------------------------------------------------------------------ #$Date: 2016-03-21 06:59:19 +0200 (Mon, 21 Mar 2016) $ #$Revision: 178543 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/06/49/4064959.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_4064959 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 'C17 H40 P2 Pt S' _chemical_formula_sum 'C17 H40 P2 Pt S' _chemical_formula_weight 533.58 _chemical_name_common jonsk33 _chemical_name_systematic ; (dippe)Pt(Me)(SEt) ; _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' _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 109.672(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.3969(9) _cell_length_b 15.2962(13) _cell_length_c 14.1669(12) _cell_measurement_reflns_used 3854 _cell_measurement_temperature 100.0(1) _cell_measurement_theta_max 33.44 _cell_measurement_theta_min 2.47 _cell_volume 2121.5(3) _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 0.993 _diffrn_measured_fraction_theta_max 0.993 _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 0.0816 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 65634 _diffrn_reflns_theta_full 37.78 _diffrn_reflns_theta_max 37.78 _diffrn_reflns_theta_min 2.13 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 6.858 _exptl_absorpt_correction_T_max 0.6099 _exptl_absorpt_correction_T_min 0.2899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1064 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _refine_diff_density_max 3.642 _refine_diff_density_min -2.249 _refine_diff_density_rms 0.214 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 200 _refine_ls_number_reflns 11289 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.0794 _refine_ls_R_factor_gt 0.0395 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+1.1815P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.0851 _reflns_number_gt 7556 _reflns_number_total 11289 _reflns_threshold_expression >2sigma(I) _cod_data_source_file om200452z_si_002.cif _cod_data_source_block jonsk333b _cod_database_code 4064959 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_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 0.807737(12) 0.162161(8) 0.757718(9) 0.01786(3) Uani 1 1 d . P1 P 0.61515(8) 0.23220(6) 0.74688(6) 0.01838(16) Uani 1 1 d . P2 P 0.79722(8) 0.23070(6) 0.61194(6) 0.01891(16) Uani 1 1 d . S1 S 1.01966(10) 0.10435(7) 0.76838(8) 0.0330(2) Uani 1 1 d . C1 C 1.0771(4) 0.0196(2) 0.8626(3) 0.0252(7) Uani 1 1 d . H1A H 1.1043 0.0459 0.9303 0.030 Uiso 1 1 calc R H1B H 1.0020 -0.0223 0.8559 0.030 Uiso 1 1 calc R C2 C 1.1981(4) -0.0276(3) 0.8487(3) 0.0296(8) Uani 1 1 d . H2A H 1.2297 -0.0735 0.8995 0.044 Uiso 1 1 calc R H2B H 1.2722 0.0142 0.8558 0.044 Uiso 1 1 calc R H2C H 1.1703 -0.0539 0.7818 0.044 Uiso 1 1 calc R C3 C 0.8030(4) 0.0912(3) 0.8844(3) 0.0263(7) Uani 1 1 d . H3A H 0.7218 0.1078 0.9005 0.040 Uiso 1 1 calc R H3B H 0.8852 0.1044 0.9415 0.040 Uiso 1 1 calc R H3C H 0.7999 0.0284 0.8698 0.040 Uiso 1 1 calc R C4 C 0.5447(3) 0.2833(2) 0.6228(2) 0.0208(6) Uani 1 1 d . H4A H 0.4814 0.2417 0.5762 0.025 Uiso 1 1 calc R H4B H 0.4915 0.3357 0.6279 0.025 Uiso 1 1 calc R C5 C 0.6557(3) 0.3101(2) 0.5797(3) 0.0214(6) Uani 1 1 d . H5A H 0.6918 0.3683 0.6062 0.026 Uiso 1 1 calc R H5B H 0.6152 0.3147 0.5059 0.026 Uiso 1 1 calc R C6 C 0.6326(3) 0.3232(2) 0.8355(3) 0.0246(7) Uani 1 1 d . H6 H 0.5420 0.3530 0.8184 0.029 Uiso 1 1 calc R C7 C 0.7368(4) 0.3901(3) 0.8265(3) 0.0299(8) Uani 1 1 d . H7A H 0.7536 0.4334 0.8802 0.045 Uiso 1 1 calc R H7B H 0.7013 0.4195 0.7613 0.045 Uiso 1 1 calc R H7C H 0.8225 0.3603 0.8320 0.045 Uiso 1 1 calc R C8 C 0.6726(4) 0.2898(3) 0.9436(3) 0.0314(8) Uani 1 1 d . H8A H 0.6801 0.3394 0.9890 0.047 Uiso 1 1 calc R H8B H 0.7607 0.2596 0.9617 0.047 Uiso 1 1 calc R H8C H 0.6027 0.2492 0.9493 0.047 Uiso 1 1 calc R C9 C 0.4704(3) 0.1676(2) 0.7573(2) 0.0222(6) Uani 1 1 d . H9 H 0.4982 0.1464 0.8282 0.027 Uiso 1 1 calc R C10 C 0.4464(4) 0.0868(3) 0.6912(3) 0.0282(8) Uani 1 1 d . H10A H 0.3785 0.0492 0.7050 0.042 Uiso 1 1 calc R H10B H 0.5324 0.0546 0.7053 0.042 Uiso 1 1 calc R H10C H 0.4130 0.1044 0.6206 0.042 Uiso 1 1 calc R C11 C 0.3404(3) 0.2214(3) 0.7389(3) 0.0272(7) Uani 1 1 d . H11A H 0.2692 0.1844 0.7490 0.041 Uiso 1 1 calc R H11B H 0.3093 0.2435 0.6699 0.041 Uiso 1 1 calc R H11C H 0.3594 0.2707 0.7858 0.041 Uiso 1 1 calc R C12 C 0.9469(3) 0.2945(2) 0.6095(3) 0.0218(6) Uani 1 1 d . H12 H 1.0178 0.2519 0.6055 0.026 Uiso 1 1 calc R C13 C 1.0079(4) 0.3463(3) 0.7059(3) 0.0296(8) Uani 1 1 d . H13A H 1.0940 0.3730 0.7070 0.044 Uiso 1 1 calc R H13B H 1.0250 0.3070 0.7635 0.044 Uiso 1 1 calc R H13C H 0.9439 0.3922 0.7094 0.044 Uiso 1 1 calc R C14 C 0.9158(4) 0.3552(3) 0.5186(3) 0.0304(8) Uani 1 1 d . H14A H 1.0008 0.3822 0.5175 0.046 Uiso 1 1 calc R H14B H 0.8520 0.4008 0.5230 0.046 Uiso 1 1 calc R H14C H 0.8749 0.3213 0.4570 0.046 Uiso 1 1 calc R C15 C 0.7539(4) 0.1618(3) 0.4987(3) 0.0246(7) Uani 1 1 d . H15 H 0.7379 0.2015 0.4398 0.030 Uiso 1 1 calc R C16 C 0.6212(4) 0.1125(3) 0.4847(3) 0.0302(8) Uani 1 1 d . H16A H 0.6004 0.0746 0.4256 0.045 Uiso 1 1 calc R H16B H 0.5466 0.1544 0.4752 0.045 Uiso 1 1 calc R H16C H 0.6312 0.0767 0.5441 0.045 Uiso 1 1 calc R C17 C 0.8672(4) 0.0982(3) 0.4992(4) 0.0383(10) Uani 1 1 d . H17A H 0.8385 0.0642 0.4369 0.057 Uiso 1 1 calc R H17B H 0.8856 0.0585 0.5565 0.057 Uiso 1 1 calc R H17C H 0.9502 0.1310 0.5044 0.057 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 0.01559(5) 0.02129(6) 0.01667(5) 0.00155(5) 0.00539(4) 0.00092(5) P1 0.0151(3) 0.0231(4) 0.0166(3) -0.0005(3) 0.0049(3) -0.0002(3) P2 0.0180(4) 0.0213(4) 0.0178(4) 0.0008(3) 0.0065(3) -0.0002(3) S1 0.0234(4) 0.0395(6) 0.0407(5) 0.0179(5) 0.0168(4) 0.0112(4) C1 0.0241(16) 0.0218(17) 0.0296(17) 0.0025(14) 0.0090(13) 0.0057(13) C2 0.0246(17) 0.030(2) 0.0324(19) 0.0016(16) 0.0073(14) 0.0065(14) C3 0.0274(17) 0.033(2) 0.0206(15) 0.0062(14) 0.0102(13) 0.0034(15) C4 0.0164(13) 0.0231(17) 0.0213(14) 0.0036(13) 0.0044(11) 0.0030(12) C5 0.0188(14) 0.0225(16) 0.0216(14) 0.0037(13) 0.0049(11) 0.0017(12) C6 0.0168(13) 0.029(2) 0.0264(16) -0.0080(14) 0.0047(12) -0.0004(12) C7 0.0279(18) 0.028(2) 0.0334(19) -0.0083(16) 0.0103(15) -0.0047(15) C8 0.0315(19) 0.041(2) 0.0214(16) -0.0080(16) 0.0090(14) -0.0016(17) C9 0.0194(13) 0.0286(18) 0.0189(13) 0.0001(14) 0.0069(11) -0.0037(13) C10 0.0282(18) 0.0269(19) 0.0288(18) -0.0025(15) 0.0088(14) -0.0077(15) C11 0.0177(14) 0.035(2) 0.0307(18) -0.0005(16) 0.0103(13) -0.0017(14) C12 0.0194(14) 0.0240(17) 0.0247(15) 0.0010(13) 0.0108(12) -0.0013(12) C13 0.0265(17) 0.034(2) 0.0290(17) 0.0001(16) 0.0097(14) -0.0067(15) C14 0.0312(19) 0.035(2) 0.0281(17) 0.0069(16) 0.0138(15) -0.0025(15) C15 0.0291(16) 0.0271(17) 0.0191(13) -0.0011(14) 0.0100(12) -0.0030(15) C16 0.0276(18) 0.035(2) 0.0262(17) -0.0082(16) 0.0061(14) -0.0034(15) C17 0.033(2) 0.041(3) 0.046(2) -0.016(2) 0.0200(18) -0.0051(18) 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 C3 Pt1 P1 91.63(10) C3 Pt1 P2 174.74(11) P1 Pt1 P2 87.06(3) C3 Pt1 S1 92.39(10) P1 Pt1 S1 173.57(4) P2 Pt1 S1 89.38(3) C4 P1 C6 104.33(17) C4 P1 C9 103.37(15) C6 P1 C9 104.18(16) C4 P1 Pt1 109.26(11) C6 P1 Pt1 115.85(11) C9 P1 Pt1 118.31(12) C5 P2 C15 102.74(17) C5 P2 C12 104.75(16) C15 P2 C12 104.27(16) C5 P2 Pt1 108.50(11) C15 P2 Pt1 116.54(13) C12 P2 Pt1 118.37(11) C1 S1 Pt1 112.90(12) C2 C1 S1 109.1(3) C2 C1 H1A 109.9 S1 C1 H1A 109.9 C2 C1 H1B 109.9 S1 C1 H1B 109.9 H1A C1 H1B 108.3 C1 C2 H2A 109.5 C1 C2 H2B 109.5 H2A C2 H2B 109.5 C1 C2 H2C 109.5 H2A C2 H2C 109.5 H2B C2 H2C 109.5 Pt1 C3 H3A 109.5 Pt1 C3 H3B 109.5 H3A C3 H3B 109.5 Pt1 C3 H3C 109.5 H3A C3 H3C 109.5 H3B C3 H3C 109.5 C5 C4 P1 112.6(2) C5 C4 H4A 109.1 P1 C4 H4A 109.1 C5 C4 H4B 109.1 P1 C4 H4B 109.1 H4A C4 H4B 107.8 C4 C5 P2 111.8(2) C4 C5 H5A 109.3 P2 C5 H5A 109.3 C4 C5 H5B 109.3 P2 C5 H5B 109.3 H5A C5 H5B 107.9 C7 C6 C8 110.2(3) C7 C6 P1 111.0(3) C8 C6 P1 111.2(3) C7 C6 H6 108.1 C8 C6 H6 108.1 P1 C6 H6 108.1 C6 C7 H7A 109.5 C6 C7 H7B 109.5 H7A C7 H7B 109.5 C6 C7 H7C 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 C6 C8 H8A 109.5 C6 C8 H8B 109.5 H8A C8 H8B 109.5 C6 C8 H8C 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C10 C9 C11 112.3(3) C10 C9 P1 110.8(2) C11 C9 P1 113.3(3) C10 C9 H9 106.6 C11 C9 H9 106.6 P1 C9 H9 106.6 C9 C10 H10A 109.5 C9 C10 H10B 109.5 H10A C10 H10B 109.5 C9 C10 H10C 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 C9 C11 H11A 109.5 C9 C11 H11B 109.5 H11A C11 H11B 109.5 C9 C11 H11C 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 C13 C12 C14 110.3(3) C13 C12 P2 110.9(2) C14 C12 P2 113.3(2) C13 C12 H12 107.3 C14 C12 H12 107.3 P2 C12 H12 107.3 C12 C13 H13A 109.5 C12 C13 H13B 109.5 H13A C13 H13B 109.5 C12 C13 H13C 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 C12 C14 H14A 109.5 C12 C14 H14B 109.5 H14A C14 H14B 109.5 C12 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C16 C15 C17 110.4(3) C16 C15 P2 110.0(2) C17 C15 P2 113.5(3) C16 C15 H15 107.6 C17 C15 H15 107.6 P2 C15 H15 107.6 C15 C16 H16A 109.5 C15 C16 H16B 109.5 H16A C16 H16B 109.5 C15 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C15 C17 H17A 109.5 C15 C17 H17B 109.5 H17A C17 H17B 109.5 C15 C17 H17C 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Pt1 C3 2.112(3) Pt1 P1 2.2302(9) Pt1 P2 2.2857(9) Pt1 S1 2.3315(9) P1 C4 1.836(3) P1 C6 1.842(4) P1 C9 1.847(3) P2 C5 1.842(3) P2 C15 1.844(4) P2 C12 1.848(3) S1 C1 1.811(4) C1 C2 1.520(5) C1 H1A 0.9900 C1 H1B 0.9900 C2 H2A 0.9800 C2 H2B 0.9800 C2 H2C 0.9800 C3 H3A 0.9800 C3 H3B 0.9800 C3 H3C 0.9800 C4 C5 1.532(5) C4 H4A 0.9900 C4 H4B 0.9900 C5 H5A 0.9900 C5 H5B 0.9900 C6 C7 1.527(5) C6 C8 1.533(5) C6 H6 1.0000 C7 H7A 0.9800 C7 H7B 0.9800 C7 H7C 0.9800 C8 H8A 0.9800 C8 H8B 0.9800 C8 H8C 0.9800 C9 C10 1.521(5) C9 C11 1.528(5) C9 H9 1.0000 C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 C11 H11A 0.9800 C11 H11B 0.9800 C11 H11C 0.9800 C12 C13 1.520(5) C12 C14 1.531(5) C12 H12 1.0000 C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800 C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 C15 C16 1.525(5) C15 C17 1.525(6) C15 H15 1.0000 C16 H16A 0.9800 C16 H16B 0.9800 C16 H16C 0.9800 C17 H17A 0.9800 C17 H17B 0.9800 C17 H17C 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 C3 Pt1 P1 C4 -164.01(17) P2 Pt1 P1 C4 10.89(13) S1 Pt1 P1 C4 67.4(3) C3 Pt1 P1 C6 78.56(18) P2 Pt1 P1 C6 -106.54(14) S1 Pt1 P1 C6 -50.0(3) C3 Pt1 P1 C9 -46.21(16) P2 Pt1 P1 C9 128.70(12) S1 Pt1 P1 C9 -174.8(3) C3 Pt1 P2 C5 82.2(11) P1 Pt1 P2 C5 6.55(13) S1 Pt1 P2 C5 -168.09(13) C3 Pt1 P2 C15 -33.0(12) P1 Pt1 P2 C15 -108.73(14) S1 Pt1 P2 C15 76.63(14) C3 Pt1 P2 C12 -158.7(11) P1 Pt1 P2 C12 125.61(14) S1 Pt1 P2 C12 -49.03(14) C3 Pt1 S1 C1 6.82(18) P1 Pt1 S1 C1 135.4(3) P2 Pt1 S1 C1 -168.23(15) Pt1 S1 C1 C2 167.6(2) C6 P1 C4 C5 93.9(3) C9 P1 C4 C5 -157.4(3) Pt1 P1 C4 C5 -30.6(3) P1 C4 C5 P2 36.7(3) C15 P2 C5 C4 97.3(3) C12 P2 C5 C4 -154.0(2) Pt1 P2 C5 C4 -26.7(3) C4 P1 C6 C7 -64.5(3) C9 P1 C6 C7 -172.6(3) Pt1 P1 C6 C7 55.6(3) C4 P1 C6 C8 172.4(2) C9 P1 C6 C8 64.3(3) Pt1 P1 C6 C8 -67.4(3) C4 P1 C9 C10 73.7(3) C6 P1 C9 C10 -177.5(3) Pt1 P1 C9 C10 -47.2(3) C4 P1 C9 C11 -53.6(3) C6 P1 C9 C11 55.2(3) Pt1 P1 C9 C11 -174.5(2) C5 P2 C12 C13 80.1(3) C15 P2 C12 C13 -172.3(3) Pt1 P2 C12 C13 -40.9(3) C5 P2 C12 C14 -44.5(3) C15 P2 C12 C14 63.1(3) Pt1 P2 C12 C14 -165.5(2) C5 P2 C15 C16 -64.6(3) C12 P2 C15 C16 -173.6(3) Pt1 P2 C15 C16 53.9(3) C5 P2 C15 C17 171.2(3) C12 P2 C15 C17 62.1(3) Pt1 P2 C15 C17 -70.3(3)