Platinum thiolate complexes supported by PBP and POCOP pincer ligands as efficient catalysts for the hydrosilylation of carbonyl compounds
Xue, Man-Man; Chang, Jiarui; Zhang, Jie; Chen, Xuenian; Dalton Transactions  (2022) –; doi:10.1039/D1DT04179G

data_7709319
_publ_section_title
;
 Platinum thiolate complexes supported by PBP and POCOP pincer ligands as
 efficient catalysts for the hydrosilylation of carbonyl compounds
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04179G
_journal_year                    2022
_chemical_formula_moiety         'C22 H40 O2 P2 Pt S'
_chemical_formula_sum            'C22 H40 O2 P2 Pt S'
_chemical_formula_weight         625.63
_chemical_name_systematic        tBu-POCOP-Pt-SH
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-04-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-27 deposited with the CCDC.	2022-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                100.588(3)
_cell_angle_beta                 95.692(3)
_cell_angle_gamma                104.316(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3204(3)
_cell_length_b                   12.0711(4)
_cell_length_c                   13.4168(4)
_cell_measurement_reflns_used    7188
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      71.4020
_cell_measurement_theta_min      3.8510
_cell_volume                     1268.58(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -30.00  23.00   1.00    1.00    --  -35.62  26.00 134.00   53
  2  \w   -103.00 -13.00   1.00    1.00    --  -35.62 -26.00 -28.00   90
  3  \w    -12.00  13.00   1.00    1.00    --   35.62 -26.00 -28.00   25
  4  \w     35.00  60.00   1.00    1.00    --   35.62  26.00 134.00   25
  5  \w     37.00  99.00   1.00    1.00    --  107.12 -26.00 -28.00   62
  6  \w     84.00 131.00   1.00    1.00    --  107.12  26.00 134.00   47
  7  \w   -100.00 -74.00   1.00    1.00    --  -35.62-178.00 150.00   26
  8  \w   -103.00 -35.00   1.00    1.00    --  -35.62-178.00-150.00   68
  9  \w    -44.00  32.00   1.00    1.00    --  -35.62  57.00 150.00   76
 10  \w     27.00  60.00   1.00    1.00    --   35.62 -99.00  90.00   33
 11  \w    -23.00  52.00   1.00    1.00    --   35.62 -57.00-150.00   75
 12  \w     28.00  72.00   1.00    1.00    --   35.62 -99.00-180.00   44
 13  \w     23.00  71.00   1.00    1.00    --   35.62 -99.00   0.00   48
 14  \w     40.00 105.00   1.00    1.00    --  107.12 -61.00  60.00   65
 15  \w    131.00 172.00   1.00    1.00    --  107.12  61.00   0.00   41
 16  \w     38.00  74.00   1.00    1.00    --  107.12 -95.00   0.00   36
 17  \w     43.00  69.00   1.00    1.00    --  107.12 -95.00  60.00   26
 18  \w     75.00 107.00   1.00    1.00    --  107.12 -95.00  60.00   32
 19  \w     94.00 176.00   1.00    1.00    --  107.12  45.00 -30.00   82
 20  \w    113.00 175.00   1.00    1.00    --  107.12  45.00  60.00   62
 21  \w     90.00 126.00   1.00    1.00    --  107.12  61.00   0.00   36
 22  \w    136.00 162.00   1.00    1.00    --  107.12  77.00 120.00   26
 23  \w     94.00 122.00   1.00    1.00    --  107.12  77.00 120.00   28
 24  \w     76.00 110.00   1.00    1.00    --  107.12 -95.00-150.00   34
 25  \w     40.00  69.00   1.00    1.00    --  107.12 -95.00-150.00   29
 26  \w     58.00 130.00   1.00    1.00    --  107.12 -77.00 -90.00   72
 27  \w     83.00 109.00   1.00    1.00    --  107.12 -95.00   0.00   26
 28  \w     42.00  90.00   1.00    1.00    --  107.12-111.00-180.00   48
 29  \w     51.00 125.00   1.00    1.00    --  107.12 -45.00-180.00   74
 30  \w    107.00 132.00   1.00    1.00    --  107.12 111.00   0.00   25
 31  \w     42.00 112.00   1.00    1.00    --  107.12-111.00-150.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0953071000
_diffrn_orient_matrix_UB_12      -0.0938208000
_diffrn_orient_matrix_UB_13      -0.0234974000
_diffrn_orient_matrix_UB_21      0.1411376000
_diffrn_orient_matrix_UB_22      0.0897084000
_diffrn_orient_matrix_UB_23      -0.0317678000
_diffrn_orient_matrix_UB_31      0.0915078000
_diffrn_orient_matrix_UB_32      0.0367118000
_diffrn_orient_matrix_UB_33      0.1113812000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8829
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.416
_diffrn_reflns_theta_min         3.390
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.414
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.00021(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4809
_refine_ls_number_restraints     374
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0272P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0491
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4555
_reflns_number_total             4809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04179g2.cif
_cod_data_source_block           cjr-20210409
_cod_database_code               7709319
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 O1 P1 Pt1 S1'
_shelx_estimated_absorpt_t_max   0.342
_shelx_estimated_absorpt_t_min   0.257
_diffrn_oxdiff_digest_frames
;
01b52dc287d832fa22d666e90f1c53818d00038480d
;
_diffrn_oxdiff_digest_hkl
;
0111054950305ad129a223153ee6c4fbc61294
;
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S1-H1
 1.35 with sigma of 0.02
 Pt1-H1
 3.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C2 \\sim C6 \\sim C5 \\sim C1 \\sim C3 \\sim C4 \\sim C7 \\sim C15 \\sim C19
\\sim C11 \\sim C22 \\sim C14 \\sim C20 \\sim C17 \\sim C18 \\sim C21 \\sim C16
\\sim C8 \\sim C9 \\sim C13 \\sim C12 \\sim C10: within 3.8A with sigma of 0.01
and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C4(H4)
4.b Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c), C14(H14a,H14b,H14c), C20(H20a,H20b,H20c), C17(H17a,H17b,
 H17c), C18(H18a,H18b,H18c), C21(H21a,H21b,H21c), C16(H16a,H16b,H16c), C8(H8a,
 H8b,H8c), C9(H9a,H9b,H9c), C13(H13a,H13b,H13c), C12(H12a,H12b,H12c), C10(H10a,
 H10b,H10c)
;
_shelx_res_checksum              73089
_shelx_hkl_checksum              75048
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.517
_oxdiff_exptl_absorpt_empirical_full_min 0.776