A general protocol for the synthesis of Pt-NHC (NHC = N-heterocyclic carbene) hydrosilylation catalysts.
Maliszewski, Benon P.; Tzouras, Nikolaos V.; Guillet, Sébastien G; Saab, Marina; Beliš, Marek; Van Hecke, Kristof; Nahra, Fady; Nolan, Steven P.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 14673–14679; doi:10.1039/d0dt03480k

data_7705653
_publ_section_title
;
 A general protocol for the synthesis of Pt-NHC (NHC = N-heterocyclic
 carbene) hydrosilylation catalysts.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14673
_journal_page_last               14679
_journal_paper_doi               10.1039/d0dt03480k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C29 H44 Cl2 N2 Pt S'
_chemical_formula_sum            'C29 H44 Cl2 N2 Pt S'
_chemical_formula_weight         718.70
_chemical_name_systematic        BM15-3
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-25
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-07-10 deposited with the CCDC.	2020-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.3260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   17.9235(2)
_cell_length_b                   30.6798(4)
_cell_length_c                   16.1692(2)
_cell_measurement_reflns_used    19141
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.6860
_cell_measurement_theta_min      4.9170
_cell_volume                     8891.13(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.980
_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   -122.00  -1.00   1.00    4.00    --  -41.68 -19.00-150.00  121
  2  \w      6.00  83.00   1.00    4.00    --   41.68 -99.00 -90.00   77
  3  \w     34.00 135.00   1.00   12.50    --  106.01 -61.00 -90.00  101
  4  \w     33.00 112.00   1.00   12.50    --  106.01-125.00-180.00   79
  5  \w     53.00 178.00   1.00   12.50    --  106.01  15.00 120.00  125
  6  \w     23.00 107.00   1.00   12.50    --  106.01 -94.00  90.00   84
  7  \w   -116.00 -17.00   1.00    4.00    --  -41.68 -38.00 120.00   99
  8  \w     14.00 115.00   1.00    4.00    --   41.68  57.00  30.00  101
  9  \w     77.00 178.00   1.00   12.50    --  106.01  61.00 -30.00  101
 10  \w     33.00 112.00   1.00   12.50    --  106.01-125.00 -60.00   79
 11  \w     77.00 178.00   1.00   12.50    --  106.01  61.00 150.00  101
 12  \w     53.00 178.00   1.00   12.50    --  106.01  15.00 -90.00  125
 13  \w   -115.00 -14.00   1.00    4.00    --  -41.68 -57.00  60.00  101
 14  \w     27.00  98.00   1.00    4.00    --   41.68-125.00 120.00   71
 15  \w     77.00 178.00   1.00   12.50    --  106.01  61.00   0.00  101
 16  \w     77.00 136.00   1.00   12.50    --  106.01  61.00 -60.00   59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0531110000
_diffrn_orient_matrix_UB_12      0.0333135000
_diffrn_orient_matrix_UB_13      0.0398740000
_diffrn_orient_matrix_UB_21      0.0635155000
_diffrn_orient_matrix_UB_22      0.0338409000
_diffrn_orient_matrix_UB_23      0.0025232000
_diffrn_orient_matrix_UB_31      -0.0231144000
_diffrn_orient_matrix_UB_32      0.0163514000
_diffrn_orient_matrix_UB_33      -0.0864681000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            83614
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.884
_diffrn_reflns_theta_min         2.855
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.314
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       block
_exptl_crystal_F_000             4320
_exptl_crystal_preparation       Synthesis
_exptl_crystal_recrystallization_method 'Hexane diffusion in acetone'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.053
_refine_diff_density_max         3.925
_refine_diff_density_min         -2.469
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     976
_refine_ls_number_reflns         17663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0687
_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^)+(0.0441P)^2^+155.1160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1544
_refine_ls_wR_factor_ref         0.1629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14480
_reflns_number_total             17663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03480k2.cif
_cod_data_source_block           bm15-3
_cod_depositor_comments
'Adding full bibliography for 7705653--7705658.cif.'
_cod_database_code               7705653
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C29 H44 N2 Pt Cl2 S'
_shelx_estimated_absorpt_t_max   0.585
_shelx_estimated_absorpt_t_min   0.397
_reflns_odcompleteness_completeness 99.80
_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 Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25), C39(H39), C42(H42), C51(H51),
 C54(H54), C68(H68), C71(H71), C80(H80), C83(H83)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C31(H31A,H31B), C32(H32A,H32B), C60(H60A,H60B),
 C61(H61A,H61B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C35(H35), C36(H36),
 C37(H37), C47(H47), C48(H48), C49(H49), C64(H64), C65(H65), C66(H66), C76(H76),
  C77(H77), C78(H78)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C40(H40A,H40B,H40C),
 C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,
 H57B,H57C), C58(H58A,H58B,H58C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C),
 C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C81(H81A,H81B,H81C), C82(H82A,H82B,
 H82C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C87(H87A,
 H87B,H87C)
;
_shelx_res_checksum              60219
_olex2_exptl_crystal_mounting_method 'Little loop'
_olex2_submission_original_sample_id BM15-3
_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 2.457
_oxdiff_exptl_absorpt_empirical_full_min 0.295