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_7709320
_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         'C28 H44 O2 P2 Pt S'
_chemical_formula_sum            'C28 H44 O2 P2 Pt S'
_chemical_formula_weight         701.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-05-15
_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                90
_cell_angle_beta                 106.5180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.79010(10)
_cell_length_b                   12.6583(2)
_cell_length_c                   20.8480(2)
_cell_measurement_reflns_used    10500
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      71.4420
_cell_measurement_theta_min      4.4250
_cell_volume                     3236.01(7)
_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  'ShelXL (Sheldrick, 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 0.976
_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   -100.00 -12.00   1.00    1.00    --  -35.62 144.00 170.00   88
  2  \w    -90.00  -3.00   1.00    1.00    --  -35.62 126.00   2.00   87
  3  \w     39.00 131.00   1.00    1.48    --  107.12-144.00 117.00   92
  4  \w     41.00 115.00   1.00    1.48    --  107.12-126.00 -74.00   74
  5  \w     96.00 140.00   1.00    1.48    --  107.12 126.00   2.00   44
  6  \w    105.00 131.00   1.00    1.48    --  107.12 144.00 170.00   26
  7  \w   -102.00 -37.00   1.00    1.00    --  -35.62 -57.00  60.00   65
  8  \w      0.00  27.00   1.00    1.00    --  -35.62  57.00-180.00   27
  9  \w   -105.00 -17.00   1.00    1.00    --  -35.62 -38.00 -90.00   88
 10  \w     65.00 107.00   1.00    1.00    --   35.62 178.00-120.00   42
 11  \w     46.00 110.00   1.00    1.48    --  107.12 -95.00 -60.00   64
 12  \w     39.00 108.00   1.00    1.48    --  107.12 -45.00 -60.00   69
 13  \w    151.00 176.00   1.00    1.48    --  107.12 111.00 120.00   25
 14  \w    120.00 146.00   1.00    1.48    --  107.12 -15.00-120.00   26
 15  \w     37.00  89.00   1.00    1.48    --  107.12 -15.00-120.00   52
 16  \w     39.00  74.00   1.00    1.48    --  107.12 -95.00 -90.00   35
 17  \w     92.00 174.00   1.00    1.48    --  107.12  61.00  60.00   82
 18  \w     68.00 102.00   1.00    1.48    --  107.12 -61.00-120.00   34
 19  \w     89.00 130.00   1.00    1.48    --  107.12  77.00  90.00   41
;
_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      -0.0734768000
_diffrn_orient_matrix_UB_12      -0.0982198000
_diffrn_orient_matrix_UB_13      -0.0190292000
_diffrn_orient_matrix_UB_21      -0.1017189000
_diffrn_orient_matrix_UB_22      0.0714768000
_diffrn_orient_matrix_UB_23      -0.0179429000
_diffrn_orient_matrix_UB_31      0.0063476000
_diffrn_orient_matrix_UB_32      0.0080363000
_diffrn_orient_matrix_UB_33      -0.0724995000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15296
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.531
_diffrn_reflns_theta_min         4.424
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.800
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61901
_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    1.440
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.926
_refine_diff_density_min         -1.785
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         6160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+6.2227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5684
_reflns_number_total             6160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04179g2.cif
_cod_data_source_block           cjr-20210513
_cod_database_code               7709320
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 O1 P1 Pt1 S1'
_shelx_estimated_absorpt_t_max   0.157
_shelx_estimated_absorpt_t_min   0.047
_diffrn_oxdiff_digest_frames
;
017606195215e344d8944e1a41b5c57a5200036bc76
;
_diffrn_oxdiff_digest_hkl
;
016881100b256948cdc3e43972355814ff6c49
;
_reflns_odcompleteness_completeness 99.98
_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.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C5(H5), C8(H8), C10(H10), C9(H9), C11(H11), C4(H4), C3(H3)
2.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C24(H24A,H24B,H24C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C26(H26A,H26B,H26C), C20(H20A,H20B,H20C), C16(H16A,H16B,H16C), C28(H28A,
 H28B,H28C), C22(H22A,H22B,H22C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C),
 C23(H23A,H23B,H23C)
;
_shelx_res_checksum              51417
_shelx_hkl_checksum              20798
_shelx_fab_checksum              62449
_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 1.405
_oxdiff_exptl_absorpt_empirical_full_min 0.788