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_7705655
_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         'C17 H30 Cl2 N2 Pt S, C H Cl3'
_chemical_formula_sum            'C18 H31 Cl5 N2 Pt S'
_chemical_formula_weight         679.84
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_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            8
_cell_length_a                   12.76940(10)
_cell_length_b                   19.3085(2)
_cell_length_c                   20.1949(2)
_cell_measurement_reflns_used    10877
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.7620
_cell_measurement_theta_min      4.3540
_cell_volume                     4979.21(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.979
_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    -74.00  34.00   1.00    1.00    --  -41.68  77.00   0.00  108
  2  \w   -122.00  -1.00   1.00    1.00    --  -41.68 -19.00  30.00  121
  3  \w      6.00  83.00   1.00    1.00    --   41.68 -99.00 -30.00   77
  4  \w    103.00 178.00   1.00    2.00    --  106.01  77.00 -30.00   75
  5  \w     23.00 107.00   1.00    2.00    --  106.01 -94.00  60.00   84
  6  \w     30.00 139.00   1.00    2.00    --  106.01 -77.00 120.00  109
  7  \w     53.00 178.00   1.00    2.00    --  106.01  15.00  60.00  125
  8  \w   -115.00 -25.00   1.00    1.00    --  -41.68 -57.00-180.00   90
  9  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00 -90.00  101
;
_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      -0.0153353000
_diffrn_orient_matrix_UB_12      0.0025814000
_diffrn_orient_matrix_UB_13      0.0756522000
_diffrn_orient_matrix_UB_21      -0.0868958000
_diffrn_orient_matrix_UB_22      -0.0550932000
_diffrn_orient_matrix_UB_23      -0.0053175000
_diffrn_orient_matrix_UB_31      0.0822503000
_diffrn_orient_matrix_UB_32      -0.0576302000
_diffrn_orient_matrix_UB_33      0.0084854000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24360
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.919
_diffrn_reflns_theta_min         4.379
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.317
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            'light colourless'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_description       needle
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.813
_refine_diff_density_min         -1.101
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0241
_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^)+(0.0280P)^2^+0.9474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4279
_reflns_number_total             4934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03480k2.cif
_cod_data_source_block           nt212
_cod_depositor_comments
'Adding full bibliography for 7705653--7705658.cif.'
_cod_database_code               7705655
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C17 H30 Cl2 N2 Pt S'
_reflns_odcompleteness_completeness 99.66
_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:
 C6(H6), C12(H12), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16B,H16A), C17(H17A,H17B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              34385
_olex2_date_sample_data_collection 2019-12-11
_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 1.885
_oxdiff_exptl_absorpt_empirical_full_min 0.697