#------------------------------------------------------------------------------ #$Date: 2012-02-24 19:13:23 +0200 (Fri, 24 Feb 2012) $ #$Revision: 34330 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/06/49/4064961.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_4064961 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_volume 30 _journal_year 2011 _chemical_formula_moiety 'C18 H42 P2 Pt S2' _chemical_formula_sum 'C18 H42 P2 Pt S2' _chemical_formula_weight 579.67 _chemical_name_common jonsk28 _chemical_name_systematic ; (dippe)Pt(SEt)2 ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/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 104.982(1) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 15.1351(8) _cell_length_b 10.1219(5) _cell_length_c 16.4200(8) _cell_measurement_reflns_used 3989 _cell_measurement_temperature 223(2) _cell_measurement_theta_max 31.67 _cell_measurement_theta_min 2.45 _cell_volume 2430.0(2) _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 223(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _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 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 37580 _diffrn_reflns_theta_full 37.78 _diffrn_reflns_theta_max 37.78 _diffrn_reflns_theta_min 2.45 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 6.077 _exptl_absorpt_correction_T_max 0.7119 _exptl_absorpt_correction_T_min 0.3482 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1160 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.656 _refine_diff_density_min -1.134 _refine_diff_density_rms 0.133 _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 124 _refine_ls_number_reflns 6519 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0328 _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^)+(0.0313P)^2^+0.4263P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.0702 _reflns_number_gt 5179 _reflns_number_total 6519 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file om200452z_si_002.cif _[local]_cod_data_source_block jonsk28_4b _cod_database_code 4064961 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.0000 0.308153(11) 0.2500 0.02804(4) Uani 1 2 d SD . . P1 P 0.10237(4) 0.14778(6) 0.29972(4) 0.02990(11) Uani 1 1 d . A . S1 S 0.1049(7) 0.4675(19) 0.3237(18) 0.0417(16) Uani 0.50 1 d PD A 1 C1 C 0.0387(6) 0.5647(10) 0.3762(7) 0.076(3) Uani 0.50 1 d PD A 1 H1A H -0.0143 0.5997 0.3341 0.091 Uiso 0.50 1 calc PR A 1 H1B H 0.0156 0.5073 0.4142 0.091 Uiso 0.50 1 calc PR A 1 C2 C 0.0877(7) 0.6748(7) 0.4249(6) 0.0717(16) Uani 0.50 1 d PD A 1 H2A H 0.0445 0.7324 0.4420 0.108 Uiso 0.50 1 calc PR A 1 H2B H 0.1197 0.7240 0.3907 0.108 Uiso 0.50 1 calc PR A 1 H2C H 0.1314 0.6411 0.4746 0.108 Uiso 0.50 1 calc PR A 1 S1' S 0.1106(7) 0.4670(19) 0.3145(18) 0.0417(16) Uani 0.50 1 d PD A 5 C1' C 0.0528(6) 0.6085(7) 0.3418(6) 0.0593(19) Uani 0.50 1 d PD A 5 H1C H 0.0969 0.6794 0.3628 0.071 Uiso 0.50 1 calc PR A 5 H1D H 0.0075 0.6411 0.2919 0.071 Uiso 0.50 1 calc PR A 5 C2' C 0.0076(6) 0.5705(8) 0.4066(6) 0.0717(16) Uani 0.50 1 d PD A 5 H2D H 0.0124 0.6421 0.4468 0.108 Uiso 0.50 1 calc PR A 5 H2E H 0.0368 0.4922 0.4355 0.108 Uiso 0.50 1 calc PR A 5 H2F H -0.0563 0.5520 0.3806 0.108 Uiso 0.50 1 calc PR A 5 C3 C 0.04323(16) -0.0128(2) 0.28619(18) 0.0363(5) Uani 1 1 d . . . H3A H 0.0850 -0.0809 0.2757 0.044 Uiso 1 1 calc R A . H3B H 0.0271 -0.0357 0.3385 0.044 Uiso 1 1 calc R . . C4 C 0.16608(18) 0.1519(3) 0.41147(18) 0.0398(5) Uani 1 1 d . . . H4 H 0.2047 0.2323 0.4192 0.048 Uiso 1 1 calc R A . C5 C 0.1009(2) 0.1680(4) 0.4680(2) 0.0545(8) Uani 1 1 d . A . H5A H 0.1360 0.1824 0.5258 0.082 Uiso 1 1 calc R . . H5B H 0.0642 0.0887 0.4652 0.082 Uiso 1 1 calc R . . H5C H 0.0611 0.2431 0.4491 0.082 Uiso 1 1 calc R . . C6 C 0.2302(2) 0.0359(4) 0.4387(2) 0.0600(9) Uani 1 1 d . A . H6A H 0.2629 0.0462 0.4975 0.090 Uiso 1 1 calc R . . H6B H 0.2737 0.0328 0.4045 0.090 Uiso 1 1 calc R . . H6C H 0.1952 -0.0454 0.4315 0.090 Uiso 1 1 calc R . . C7 C 0.19136(17) 0.1313(3) 0.24208(18) 0.0381(5) Uani 1 1 d . . . H7 H 0.2275 0.0515 0.2639 0.046 Uiso 1 1 calc R A . C8 C 0.1500(2) 0.1104(5) 0.1487(2) 0.0646(10) Uani 1 1 d . A . H8A H 0.1985 0.0979 0.1207 0.097 Uiso 1 1 calc R . . H8B H 0.1140 0.1872 0.1253 0.097 Uiso 1 1 calc R . . H8C H 0.1111 0.0329 0.1404 0.097 Uiso 1 1 calc R . . C9 C 0.2568(3) 0.2473(4) 0.2569(3) 0.0631(10) Uani 1 1 d . A . H9A H 0.3028 0.2336 0.2260 0.095 Uiso 1 1 calc R . . H9B H 0.2863 0.2547 0.3166 0.095 Uiso 1 1 calc R . . H9C H 0.2232 0.3278 0.2374 0.095 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 0.02530(6) 0.02281(5) 0.03552(7) 0.000 0.00696(4) 0.000 P1 0.0260(3) 0.0256(2) 0.0358(3) -0.0005(2) 0.0037(2) 0.0012(2) S1 0.0349(10) 0.0294(3) 0.058(5) -0.0084(15) 0.0069(11) -0.0054(9) C1 0.065(5) 0.094(8) 0.084(7) -0.056(6) 0.047(5) -0.017(5) C2 0.080(4) 0.058(3) 0.077(4) -0.018(3) 0.020(3) 0.006(3) S1' 0.0349(10) 0.0294(3) 0.058(5) -0.0084(15) 0.0069(11) -0.0054(9) C1' 0.065(5) 0.039(3) 0.079(6) -0.010(3) 0.027(4) -0.001(3) C2' 0.080(4) 0.058(3) 0.077(4) -0.018(3) 0.020(3) 0.006(3) C3 0.0336(11) 0.0245(10) 0.0465(14) -0.0005(9) 0.0026(10) 0.0007(8) C4 0.0338(12) 0.0404(12) 0.0395(13) -0.0008(11) -0.0005(10) -0.0006(10) C5 0.0523(18) 0.071(2) 0.0373(15) 0.0010(14) 0.0060(13) -0.0041(15) C6 0.0544(18) 0.0582(19) 0.0524(18) 0.0031(15) -0.0131(15) 0.0120(15) C7 0.0302(11) 0.0357(12) 0.0493(15) -0.0034(11) 0.0118(10) 0.0052(9) C8 0.0466(17) 0.103(3) 0.0470(18) -0.0101(19) 0.0169(14) 0.0099(19) C9 0.057(2) 0.0511(19) 0.093(3) -0.0181(19) 0.041(2) -0.0152(16) 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 P1 Pt1 P1 87.48(3) 2 . P1 Pt1 S1' 174.7(8) 2 . P1 Pt1 S1' 89.2(6) . . P1 Pt1 S1' 89.2(6) 2 2 P1 Pt1 S1' 174.7(8) . 2 S1' Pt1 S1' 94.3(13) . 2 P1 Pt1 S1 89.9(6) 2 2 P1 Pt1 S1 170.9(8) . 2 S1' Pt1 S1 93.99(6) . 2 S1' Pt1 S1 4.7(11) 2 2 P1 Pt1 S1 170.9(8) 2 . P1 Pt1 S1 89.9(6) . . S1' Pt1 S1 4.7(11) . . S1' Pt1 S1 93.99(6) 2 . S1 Pt1 S1 94.0(13) 2 . C4 P1 C3 104.70(13) . . C4 P1 C7 104.48(13) . . C3 P1 C7 104.79(13) . . C4 P1 Pt1 118.71(9) . . C3 P1 Pt1 109.02(8) . . C7 P1 Pt1 113.92(9) . . C1 S1 Pt1 103.7(4) . . C2 C1 S1 114.8(6) . . C2 C1 H1A 108.6 . . S1 C1 H1A 108.6 . . C2 C1 H1B 108.6 . . S1 C1 H1B 108.6 . . H1A C1 H1B 107.5 . . 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 . . C1' S1' Pt1 108.6(5) . . C2' C1' S1' 108.9(11) . . C2' C1' H1C 109.9 . . S1' C1' H1C 109.9 . . C2' C1' H1D 109.9 . . S1' C1' H1D 109.9 . . H1C C1' H1D 108.3 . . C1' C2' H2D 109.5 . . C1' C2' H2E 109.5 . . H2D C2' H2E 109.5 . . C1' C2' H2F 109.5 . . H2D C2' H2F 109.5 . . H2E C2' H2F 109.5 . . C3 C3 P1 112.77(11) 2 . C3 C3 H3A 109.0 2 . P1 C3 H3A 109.0 . . C3 C3 H3B 109.0 2 . P1 C3 H3B 109.0 . . H3A C3 H3B 107.8 . . C6 C4 C5 111.6(3) . . C6 C4 P1 114.0(2) . . C5 C4 P1 110.8(2) . . C6 C4 H4 106.7 . . C5 C4 H4 106.7 . . P1 C4 H4 106.7 . . C4 C5 H5A 109.5 . . C4 C5 H5B 109.5 . . H5A C5 H5B 109.5 . . C4 C5 H5C 109.5 . . H5A C5 H5C 109.5 . . H5B C5 H5C 109.5 . . C4 C6 H6A 109.5 . . C4 C6 H6B 109.5 . . H6A C6 H6B 109.5 . . C4 C6 H6C 109.5 . . H6A C6 H6C 109.5 . . H6B C6 H6C 109.5 . . C8 C7 C9 110.6(3) . . C8 C7 P1 111.54(19) . . C9 C7 P1 112.5(2) . . C8 C7 H7 107.3 . . C9 C7 H7 107.3 . . P1 C7 H7 107.3 . . C7 C8 H8A 109.5 . . C7 C8 H8B 109.5 . . H8A C8 H8B 109.5 . . C7 C8 H8C 109.5 . . H8A C8 H8C 109.5 . . H8B C8 H8C 109.5 . . C7 C9 H9A 109.5 . . C7 C9 H9B 109.5 . . H9A C9 H9B 109.5 . . C7 C9 H9C 109.5 . . H9A C9 H9C 109.5 . . H9B C9 H9C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pt1 P1 2.2468(6) 2 Pt1 P1 2.2468(6) . Pt1 S1' 2.365(3) . Pt1 S1' 2.365(3) 2 Pt1 S1 2.365(3) 2 Pt1 S1 2.365(3) . P1 C4 1.839(3) . P1 C3 1.841(2) . P1 C7 1.843(3) . S1 C1 1.779(11) . C1 C2 1.457(10) . C1 H1A 0.9800 . C1 H1B 0.9800 . C2 H2A 0.9700 . C2 H2B 0.9700 . C2 H2C 0.9700 . S1' C1' 1.795(12) . C1' C2' 1.457(10) . C1' H1C 0.9800 . C1' H1D 0.9800 . C2' H2D 0.9700 . C2' H2E 0.9700 . C2' H2F 0.9700 . C3 C3 1.523(5) 2 C3 H3A 0.9800 . C3 H3B 0.9800 . C4 C6 1.516(4) . C4 C5 1.529(5) . C4 H4 0.9900 . C5 H5A 0.9700 . C5 H5B 0.9700 . C5 H5C 0.9700 . C6 H6A 0.9700 . C6 H6B 0.9700 . C6 H6C 0.9700 . C7 C8 1.513(4) . C7 C9 1.514(4) . C7 H7 0.9900 . C8 H8A 0.9700 . C8 H8B 0.9700 . C8 H8C 0.9700 . C9 H9A 0.9700 . C9 H9B 0.9700 . C9 H9C 0.9700 . 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_site_symmetry_1 _geom_torsion_site_symmetry_4 P1 Pt1 P1 C4 -127.59(11) 2 . S1' Pt1 P1 C4 48.3(6) . . S1' Pt1 P1 C4 -179(3) 2 . S1 Pt1 P1 C4 159(3) 2 . S1 Pt1 P1 C4 43.7(6) . . P1 Pt1 P1 C3 -7.94(10) 2 . S1' Pt1 P1 C3 167.9(6) . . S1' Pt1 P1 C3 -59(3) 2 . S1 Pt1 P1 C3 -81(3) 2 . S1 Pt1 P1 C3 163.3(6) . . P1 Pt1 P1 C7 108.70(10) 2 . S1' Pt1 P1 C7 -75.4(6) . . S1' Pt1 P1 C7 57(3) 2 . S1 Pt1 P1 C7 35(3) 2 . S1 Pt1 P1 C7 -80.0(6) . . P1 Pt1 S1 C1 -59(4) 2 . P1 Pt1 S1 C1 -131.7(14) . . S1' Pt1 S1 C1 146(18) . . S1' Pt1 S1 C1 52(2) 2 . S1 Pt1 S1 C1 56.6(10) 2 . Pt1 S1 C1 C2 -178.1(10) . . P1 Pt1 S1' C1' -99(3) 2 . P1 Pt1 S1' C1' -150.6(14) . . S1' Pt1 S1' C1' 33.3(9) 2 . S1 Pt1 S1' C1' 38(2) 2 . S1 Pt1 S1' C1' -52(15) . . Pt1 S1' C1' C2' 65.8(15) . . C4 P1 C3 C3 154.2(3) . 2 C7 P1 C3 C3 -96.1(3) . 2 Pt1 P1 C3 C3 26.2(3) . 2 C3 P1 C4 C6 55.8(3) . . C7 P1 C4 C6 -54.1(3) . . Pt1 P1 C4 C6 177.6(2) . . C3 P1 C4 C5 -71.1(2) . . C7 P1 C4 C5 179.0(2) . . Pt1 P1 C4 C5 50.7(2) . . C4 P1 C7 C8 173.4(3) . . C3 P1 C7 C8 63.6(3) . . Pt1 P1 C7 C8 -55.5(3) . . C4 P1 C7 C9 -61.6(3) . . C3 P1 C7 C9 -171.4(3) . . Pt1 P1 C7 C9 69.5(3) . .