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_7705656
_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_absolute_configuration ad
_chemical_formula_moiety         'C23 H30 Cl2 N2 Pt S, C H Cl3'
_chemical_formula_sum            'C24 H31 Cl5 N2 Pt S'
_chemical_formula_weight         751.90
_chemical_name_systematic        BM18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-08
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0629(2)
_cell_length_b                   15.8461(2)
_cell_length_c                   17.4890(2)
_cell_measurement_reflns_used    13967
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.5240
_cell_measurement_theta_min      3.0650
_cell_volume                     2788.76(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.932
_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    -64.00  35.00   1.00   25.00    --   10.17 -38.00 -90.00   99
  2  \w    -18.00  83.00   1.00   25.00    --   10.17  57.00  90.00  101
  3  \w     27.00  90.00   1.00   25.00    --   10.17-163.00 145.00   63
  4  \w    -83.00 -39.00   1.00   25.00    --  -11.11 -57.00-150.00   44
;
_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      0.0649032000
_diffrn_orient_matrix_UB_12      0.0045806000
_diffrn_orient_matrix_UB_13      -0.0152570000
_diffrn_orient_matrix_UB_21      -0.0253244000
_diffrn_orient_matrix_UB_22      -0.0067527000
_diffrn_orient_matrix_UB_23      -0.0373385000
_diffrn_orient_matrix_UB_31      -0.0106474000
_diffrn_orient_matrix_UB_32      0.0440285000
_diffrn_orient_matrix_UB_33      -0.0041394000
_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  0.0347
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24777
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.569
_diffrn_reflns_theta_min         2.571
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.602
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.753
_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    1.791
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_preparation       Synthesis
_exptl_crystal_recrystallization_method 'Hexane diffusion in chloroform'
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.741
_refine_diff_density_min         -1.255
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
;
 Flack x determined using 2415 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.017(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         6815
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0217P)^2^+7.0582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0604
_refine_ls_wR_factor_ref         0.0627
_reflns_Friedel_coverage         0.683
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.801
_reflns_number_gt                6348
_reflns_number_total             6815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03480k2.cif
_cod_data_source_block           bm18
_cod_depositor_comments
'Adding full bibliography for 7705653--7705658.cif.'
_cod_database_code               7705656
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C23 H30 Cl2 N2 Pt S'
_shelx_estimated_absorpt_t_max   0.599
_shelx_estimated_absorpt_t_min   0.489
_reflns_odcompleteness_completeness 99.78
_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. Restrained distances
 C24A-Cl3A = C24A-Cl4A = C24A-Cl5A
 1.746 with sigma of 0.01
 C24B-Cl3B = C24B-Cl4B = C24B-Cl5B
 1.746 with sigma of 0.01
 Cl3A-Cl4A = Cl3A-Cl5A = Cl4A-Cl5A
 2.9 with sigma of 0.02
 Cl3B-Cl4B = Cl3B-Cl5B = Cl4B-Cl5B
 2.9 with sigma of 0.02
3. Rigid bond restraints
 Cl3A, Cl3B, Cl4A, Cl4B, Cl5A, Cl5B
 with sigma for 1-2 distances of 0.007 and sigma for 1-3 distances of 0.007
4. Uiso/Uaniso restraints and constraints
Cl3A \\sim Cl3B \\sim Cl4A \\sim Cl4B \\sim Cl5A \\sim Cl5B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C24A) = Uanis(C24B)
Uanis(Cl3A) = Uanis(Cl3B)
Uanis(Cl4A) = Uanis(Cl4B)
Uanis(Cl5A) = Uanis(Cl5B)
5. Others
 Sof(Cl4B)=Sof(Cl3B)=Sof(Cl5B)=Sof(C24B)=Sof(H24B)=1-FVAR(1)
 Sof(C24A)=Sof(H24A)=Sof(Cl4A)=Sof(Cl5A)=Sof(Cl3A)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C24A(H24A), C24B(H24B)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C2(H2), C17(H17), C15(H15), C8(H8)
6.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C10(H10A,H10B,H10C), C22(H22A,H22B,H22C), C12(H12A,H12B,
 H12C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C11(H11A,H11B,H11C), C23(H23A,
 H23B,H23C)
;
_shelx_res_checksum              78721
_olex2_date_sample_data_collection 2020-05-28
_olex2_exptl_crystal_mounting_method 'Little loop'
_olex2_submission_original_sample_id BM18
_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 1.518
_oxdiff_exptl_absorpt_empirical_full_min 0.600