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_7705654
_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         'C27 H37 N2, C2 H6 Cl3 Pt S'
_chemical_formula_sum            'C29 H43 Cl3 N2 Pt S'
_chemical_formula_weight         753.14
_chemical_name_systematic        BM49
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-07-10 deposited with the CCDC.	2020-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                79.673(3)
_cell_angle_beta                 89.901(3)
_cell_angle_gamma                81.924(4)
_cell_formula_units_Z            2
_cell_length_a                   9.0077(4)
_cell_length_b                   12.2861(5)
_cell_length_c                   14.3802(5)
_cell_measurement_reflns_used    12868
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.1200
_cell_measurement_theta_min      2.7350
_cell_volume                     1549.69(11)
_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  (Sheldrick, 2015)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.896
_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    -18.00  83.00   1.00   15.75    --   10.17  57.00-150.00  101
  2  \w    -63.00  38.00   1.00   15.75    --   10.17 -57.00  60.00  101
  3  \w    -18.00  83.00   1.00   15.75    --   10.17  57.00   0.00  101
  4  \w    -44.00  21.00   1.00   15.75    --  -11.11  77.00 -60.00   65
  5  \w    -15.00  51.00   1.00   15.75    --   10.17 -99.00-150.00   66
  6  \w    -42.00   9.00   1.00   15.75    --   10.17 -77.00 -90.00   51
  7  \w    -18.00  83.00   1.00   15.75    --   10.17  57.00  90.00  101
  8  \w    -15.00  51.00   1.00   15.75    --   10.17 -99.00 150.00   66
  9  \w    -44.00  21.00   1.00   15.75    --  -11.11  77.00 -30.00   65
 10  \w    -44.00  21.00   1.00   15.75    --  -11.11  77.00-150.00   65
;
_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      -0.0311346000
_diffrn_orient_matrix_UB_12      0.0555362000
_diffrn_orient_matrix_UB_13      0.0030575000
_diffrn_orient_matrix_UB_21      0.0690220000
_diffrn_orient_matrix_UB_22      0.0185810000
_diffrn_orient_matrix_UB_23      -0.0142017000
_diffrn_orient_matrix_UB_31      -0.0244055000
_diffrn_orient_matrix_UB_32      0.0092412000
_diffrn_orient_matrix_UB_33      -0.0480021000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34411
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.653
_diffrn_reflns_theta_min         2.647
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.874
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.228
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       needle
_exptl_crystal_F_000             752
_exptl_crystal_preparation       Synthesis
_exptl_crystal_recrystallization_method 'Acetone diffusion in pentane'
_exptl_crystal_size_max          0.517
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.055
_refine_diff_density_max         2.341
_refine_diff_density_min         -2.276
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         7843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0284P)^2^+2.7308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6309
_reflns_number_total             7843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03480k2.cif
_cod_data_source_block           bm49-2
_cod_depositor_comments
'Adding full bibliography for 7705653--7705658.cif.'
_cod_database_code               7705654
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C29 H43 Cl3 N2 Pt S'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 Ternary CH refined with riding coordinates:
 C13(H13), C22(H22), C25(H25), C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C18(H18), C1(H1), C2(H2), C19(H19), C20(H20), C8(H8), C7(H7), C6(H6)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C27(H27A,H27B,H27C), C23(H23A,H23B,H23C), C28(H28A,H28B,
 H28C), C24(H24A,H24B,H24C), C29(H29A,H29B,H29C), C14(H14A,H14B,H14C), C11(H11A,
 H11B,H11C), C26(H26A,H26B,H26C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              23219
_olex2_date_sample_data_collection 2020-06-24
_olex2_exptl_crystal_mounting_method 'Little loop'
_olex2_submission_original_sample_id BM49
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.901
_oxdiff_exptl_absorpt_empirical_full_min 0.348