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_7709321
_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         'C30 H45 B N2 P2 Pt S'
_chemical_formula_sum            'C30 H45 B N2 P2 Pt S'
_chemical_formula_weight         733.58
_chemical_name_systematic        tBu-PBP-Pt-SPh
_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             2021-11-11
_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                 103.5780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.87340(10)
_cell_length_b                   17.4918(2)
_cell_length_c                   14.8878(2)
_cell_measurement_reflns_used    9059
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.4500
_cell_measurement_theta_min      4.1200
_cell_volume                     3258.72(6)
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_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 -48.00   1.00    1.00    --  -35.62 -76.00   5.00   52
  2  \w    -62.00  29.00   1.00    1.00    --  -35.62  76.00 132.00   91
  3  \w    -39.00 -12.00   1.00    1.00    --  -35.62 -76.00   5.00   27
  4  \w     35.00  62.00   1.00    1.00    --   35.62 -76.00   5.00   27
  5  \w     94.00 172.00   1.00    2.06    --  107.12  76.00 132.00   78
  6  \w     43.00 121.00   1.00    2.06    --  107.12 -76.00   5.00   78
  7  \w     62.00 108.00   1.00    1.00    --   35.62-178.00 -30.00   46
  8  \w      2.00  75.00   1.00    1.00    --   35.62 -99.00-150.00   73
  9  \w     32.00  57.00   1.00    1.00    --   35.62  76.00 132.00   25
 10  \w      3.00  75.00   1.00    1.00    --   35.62 -99.00 -30.00   72
 11  \w     88.00 166.00   1.00    2.06    --  107.12  77.00  90.00   78
 12  \w     88.00 115.00   1.00    2.06    --  107.12 -30.00 -30.00   27
 13  \w     37.00  94.00   1.00    2.06    --  107.12 -30.00-180.00   57
 14  \w    150.00 176.00   1.00    2.06    --  107.12  45.00 -90.00   26
 15  \w     41.00 110.00   1.00    2.06    --  107.12-111.00   0.00   69
 16  \w     38.00  69.00   1.00    2.06    --  107.12 -95.00 150.00   31
 17  \w     75.00 101.00   1.00    2.06    --  107.12 -95.00-180.00   26
 18  \w     80.00 149.00   1.00    2.06    --  107.12 178.00  30.00   69
;
_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      -0.1036254000
_diffrn_orient_matrix_UB_12      -0.0268836000
_diffrn_orient_matrix_UB_13      0.0251150000
_diffrn_orient_matrix_UB_21      0.0606019000
_diffrn_orient_matrix_UB_22      -0.0680070000
_diffrn_orient_matrix_UB_23      0.0538524000
_diffrn_orient_matrix_UB_31      0.0273071000
_diffrn_orient_matrix_UB_32      0.0491044000
_diffrn_orient_matrix_UB_33      0.0882991000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13424
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.580
_diffrn_reflns_theta_min         3.965
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.727
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04791
_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    1.495
_exptl_crystal_description       plate
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.040
_refine_diff_density_min         -1.963
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         6216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0916P)^2^+12.3689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1682
_refine_ls_wR_factor_ref         0.1732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5512
_reflns_number_total             6216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04179g2.cif
_cod_data_source_block           20201224-xmm
_cod_database_code               7709321
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 N1 B1 S1 Pt1 '
_shelx_estimated_absorpt_t_max   0.642
_shelx_estimated_absorpt_t_min   0.443
_diffrn_oxdiff_digest_frames
;
01865b6632044759b0609f9898bbadb80f00035547b
;
_diffrn_oxdiff_digest_hkl
;
01420e94fa57f1a76237effaeeb4dfc36783e0
;
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C29(H29), C26(H26), C27(H27), C28(H28)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C24(H24A,H24B,H24C), C14(H14A,H14B,
 H14C), C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C22(H22A,H22B,H22C),
 C18(H18A,H18B,H18C)
;
_shelx_res_checksum              39801
_shelx_hkl_checksum              11867
_shelx_fab_checksum              20670
_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 14.155
_oxdiff_exptl_absorpt_empirical_full_min 0.469