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_7705657
_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         'C71 H62 Cl2 N2 Pt S, 2(C H Cl3)'
_chemical_formula_sum            'C73 H64 Cl8 N2 Pt S'
_chemical_formula_weight         1480.01
_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             2020-07-06
_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                   18.2534(2)
_cell_length_b                   19.4975(2)
_cell_length_c                   37.0427(3)
_cell_measurement_reflns_used    15446
_cell_measurement_temperature    100.80(10)
_cell_measurement_theta_max      73.7370
_cell_measurement_theta_min      3.3740
_cell_volume                     13183.3(2)
_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 (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      100.80(10)
_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 0.980
_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    -83.00  38.00   1.00    5.00    --  -41.68  19.00 -60.00  121
  2  \w     27.00  98.00   1.00    5.00    --   41.68-125.00  60.00   71
  3  \w     33.00 112.00   1.00   27.00    --  106.01-125.00  60.00   79
  4  \w     80.00 178.00   1.00   27.00    --  106.01  45.00-150.00   98
  5  \w     33.00 112.00   1.00   27.00    --  106.01-125.00  30.00   79
  6  \w    103.00 178.00   1.00   27.00    --  106.01  77.00-150.00   75
  7  \w    113.00 178.00   1.00   27.00    --  106.01  77.00 -60.00   65
  8  \w     83.00 163.00   1.00   27.00    --  106.01  30.00 -60.00   80
;
_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      0.0148409000
_diffrn_orient_matrix_UB_12      -0.0015674000
_diffrn_orient_matrix_UB_13      -0.0409328000
_diffrn_orient_matrix_UB_21      -0.0204337000
_diffrn_orient_matrix_UB_22      0.0765161000
_diffrn_orient_matrix_UB_23      -0.0026247000
_diffrn_orient_matrix_UB_31      0.0805255000
_diffrn_orient_matrix_UB_32      0.0196675000
_diffrn_orient_matrix_UB_33      0.0068742000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            53525
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.000
_diffrn_reflns_theta_min         3.400
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.600
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    1.491
_exptl_crystal_description       needle
_exptl_crystal_F_000             5968
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.053
_refine_diff_density_max         1.525
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         13110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+26.3294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10707
_reflns_number_total             13110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03480k2.cif
_cod_data_source_block           nt213
_cod_depositor_comments
'Adding full bibliography for 7705653--7705658.cif.'
_cod_database_code               7705657
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C69 H58 Cl2 N2 Pt S'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C12(H12), C26(H26), C45(H45), C59(H59), C72(H72), C73(H73)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C8(H8), C10(H10), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C28(H28), C29(H29),
  C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37),
 C38(H38), C41(H41), C43(H43), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51),
  C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C61(H61), C62(H62),
 C63(H63), C64(H64), C65(H65), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C25(H25A,H25B,H25C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              2975
_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 1.343
_oxdiff_exptl_absorpt_empirical_full_min 0.852