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_7705658
_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 H42 Cl2 N2 Pt S'
_chemical_formula_sum            'C29 H42 Cl2 N2 Pt S'
_chemical_formula_weight         716.69
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-24
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.25390(10)
_cell_length_b                   17.7182(2)
_cell_length_c                   10.16940(10)
_cell_measurement_reflns_used    38032
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.2620
_cell_measurement_theta_min      2.6050
_cell_volume                     2928.68(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    '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 0.975
_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    -36.00  24.00   1.00    6.00    --  -11.03 -85.00 153.00   60
  2  \w    -83.00  18.00   1.00    6.00    --  -11.03 -61.00 -95.00  101
  3  \w    -65.00 -20.00   1.00    6.00    --  -11.03 121.00 129.36   45
  4  \w    -20.00  30.00   1.00    6.00    --  -11.03 -99.00 -30.00   50
  5  \w    -85.00  13.00   1.00    6.00    --  -11.03 -38.00-120.00   98
  6  \w    -91.00  30.00   1.00    6.00    --  -11.03 -19.00 -30.00  121
  7  \w    -79.00 -34.00   1.00    6.00    --  -11.03 144.00  35.56   45
  8  \w     35.00  99.00   1.00    6.00    --   10.17 178.00-120.00   64
  9  \w    -86.00 -38.00   1.00    6.00    --  -11.03 153.00 156.49   48
 10  \w    -20.00  30.00   1.00    6.00    --  -11.03 -99.00  60.00   50
 11  \w    -83.00 -36.00   1.00    6.00    --  -11.03 149.00 -96.49   47
 12  \w    -36.00  63.00   1.00    6.00    --  -11.03  38.00  60.00   99
 13  \w    -39.00  62.00   1.00    6.00    --  -11.03  57.00 -30.00  101
 14  \w    -66.00 -41.00   1.00    6.00    --   10.17 -77.00 150.00   25
 15  \w    -64.00  35.00   1.00    6.00    --   10.17 -38.00 -90.00   99
 16  \w    -88.00 -40.00   1.00    6.00    --  -11.03 156.00-150.24   48
 17  \w    -86.00 -38.00   1.00    6.00    --  -11.03 153.00 -47.05   48
 18  \w    -20.00  30.00   1.00    6.00    --  -11.03 -99.00 120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0280286000
_diffrn_orient_matrix_UB_12      -0.0078974000
_diffrn_orient_matrix_UB_13      0.0516391000
_diffrn_orient_matrix_UB_21      -0.0136133000
_diffrn_orient_matrix_UB_22      0.0326542000
_diffrn_orient_matrix_UB_23      0.0339973000
_diffrn_orient_matrix_UB_31      -0.0305442000
_diffrn_orient_matrix_UB_32      -0.0217958000
_diffrn_orient_matrix_UB_33      0.0322514000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            94758
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.701
_diffrn_reflns_theta_min         2.506
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.065
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.996
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.096
_refine_diff_density_max         2.663
_refine_diff_density_min         -2.577
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4184
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0088P)^2^+43.0855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3654
_reflns_number_total             4184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03480k2.cif
_cod_data_source_block           fn022
_cod_depositor_comments
'Adding full bibliography for 7705653--7705658.cif.'
_cod_database_code               7705658
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C29 H42 Cl2 N2 Pt S'
_reflns_odcompleteness_completeness 99.79
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.005 and
sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5) C16(0.5) H16A(0.5)
 H16B(0.5) H16C(0.5)
4.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7)
4.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              77387
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_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 1.210
_oxdiff_exptl_absorpt_empirical_full_min 0.839