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_7709318
_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         'C24 H45 B N2 P2 Pt S'
_chemical_formula_sum            'C24 H45 B N2 P2 Pt S'
_chemical_formula_weight         661.52
_chemical_name_systematic        tBu-PBP-Pt-SH
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-03-30
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.01270(10)
_cell_length_b                   14.4319(2)
_cell_length_c                   32.1440(5)
_cell_measurement_reflns_used    7256
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      71.6440
_cell_measurement_theta_min      4.5800
_cell_volume                     5572.68(13)
_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      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.962
_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    -51.00  12.00   1.00    1.58    --  -35.62  49.00  16.00   63
  2  \w   -101.00 -75.00   1.00    1.58    --  -35.62-159.00   6.00   26
  3  \w    130.00 171.00   1.00    6.30    --  107.12  73.00 171.00   41
  4  \w     40.00  77.00   1.00    6.30    --  107.12 -73.00  42.00   37
  5  \w     98.00 175.00   1.00    6.30    --  107.12  49.00  16.00   77
  6  \w    127.00 165.00   1.00    6.30    --  107.12 118.00-114.00   38
  7  \w     80.00 120.00   1.00    6.30    --  107.12 159.00  38.00   40
  8  \w    -97.00 -39.00   1.00    1.58    --  -35.62-178.00   0.00   58
  9  \w     20.00  77.00   1.00    1.58    --   35.62  57.00  60.00   57
 10  \w     58.00 106.00   1.00    1.58    --   35.62 178.00   0.00   48
 11  \w     41.00  67.00   1.00    6.30    --  107.12 -61.00-180.00   26
 12  \w     54.00 110.00   1.00    6.30    --  107.12 -95.00-180.00   56
 13  \w     76.00 116.00   1.00    6.30    --  107.12 -61.00-180.00   40
 14  \w     38.00  87.00   1.00    6.30    --  107.12 -95.00   0.00   49
;
_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      -0.1176174000
_diffrn_orient_matrix_UB_12      0.0245625000
_diffrn_orient_matrix_UB_13      -0.0156325000
_diffrn_orient_matrix_UB_21      -0.0481495000
_diffrn_orient_matrix_UB_22      -0.0830389000
_diffrn_orient_matrix_UB_23      0.0242038000
_diffrn_orient_matrix_UB_31      -0.0176528000
_diffrn_orient_matrix_UB_32      0.0623857000
_diffrn_orient_matrix_UB_33      0.0382782000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15153
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.462
_diffrn_reflns_theta_min         4.595
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.299
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61408
_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    1.577
_exptl_crystal_description       plate
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.878
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5223
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0673P)^2^+7.1339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1174
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4111
_reflns_number_total             5223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04179g2.cif
_cod_data_source_block           20210325-xmm-1
_cod_database_code               7709318
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 N1 B1 P1 Pt1 S1'
_shelx_estimated_absorpt_t_max   0.370
_shelx_estimated_absorpt_t_min   0.344
_diffrn_oxdiff_digest_frames
;
011dbe90dbd873168e9c3b8bb231977399000346b48
;
_diffrn_oxdiff_digest_hkl
;
01360e1950af32211fb036f06db103e167e36c
;
_reflns_odcompleteness_completeness 98.22
_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. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C22)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C5(H5)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C20(H20A,
 H20B,H20C), C24(H24A,H24B,H24C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C),
 C18(H18A,H18B,H18C)
;
_shelx_res_checksum              13825
_shelx_hkl_checksum              90027
_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 1.398
_oxdiff_exptl_absorpt_empirical_full_min 0.703