A green route to platinum N-heterocyclic carbene complexes: mechanism and expanded scope
Maliszewski, Benon P.; Ritacco, Ida; Beliš, Marek; Hashim, Ishfaq Ibni; Tzouras, Nikolaos V.; Caporaso, Lucia; Cavallo, Luigi; Van Hecke, Kristof; Nahra, Fady; Cazin, Catherine S. J.; Nolan, Steven P.; Dalton Transactions  (2022) –; doi:10.1039/D2DT00504B

data_7709906
_publ_section_title
;
 A green route to platinum N-heterocyclic carbene complexes: mechanism and
 expanded scope
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00504B
_journal_year                    2022
_chemical_formula_moiety         'C95 H78 Cl2 N2 Pt S'
_chemical_formula_sum            'C95 H78 Cl2 N2 Pt S'
_chemical_formula_weight         1545.64
_chemical_name_systematic        BM303
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-01-20 deposited with the CCDC.	2022-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.583(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9622(3)
_cell_length_b                   22.0497(3)
_cell_length_c                   21.8292(4)
_cell_measurement_reflns_used    23918
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      28.2220
_cell_measurement_theta_min      2.8510
_cell_volume                     7282.5(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 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 0.865
_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    -82.00  19.00   1.00   35.00    --   -8.69 -57.00-120.00  101
  2  \w    -42.00  24.00   1.00   35.00    --   -8.69 -77.00  90.00   66
  3  \w    -37.00  64.00   1.00   35.00    --   -8.69  57.00  30.00  101
  4  \w    -15.00  17.00   1.00   35.00    --    7.60 -99.00-180.00   32
  5  \w    -11.00  49.00   1.00   35.00    --    7.60 -99.00 -60.00   60
;
_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      0.0391633000
_diffrn_orient_matrix_UB_12      -0.0082010000
_diffrn_orient_matrix_UB_13      -0.0067119000
_diffrn_orient_matrix_UB_21      0.0225812000
_diffrn_orient_matrix_UB_22      -0.0028850000
_diffrn_orient_matrix_UB_23      0.0335834000
_diffrn_orient_matrix_UB_31      -0.0124966000
_diffrn_orient_matrix_UB_32      -0.0309624000
_diffrn_orient_matrix_UB_33      -0.0013567000
_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  0.0490
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            72276
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.716
_diffrn_reflns_theta_min         2.653
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.080
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.510
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       plate
_exptl_crystal_F_000             3160
_exptl_crystal_preparation       Synthesis
_exptl_crystal_recrystallization_method 'Pentane diffusion in DCM'
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     912
_refine_ls_number_reflns         16300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0211P)^2^+7.2682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11326
_reflns_number_total             16300
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00504b2.cif
_cod_data_source_block           bm303
_cod_database_code               7709906
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C95 H79 Cl2 N2 Pt S'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_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:
 C10(H10), C23(H23), C36(H36), C55(H55), C68(H68), C81(H81)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C8(H8), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34),
 C35(H35), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45),
  C46(H46), C47(H47), C48(H48), C51(H51), C53(H53), C57(H57), C58(H58),
 C59(H59), C60(H60), C61(H61), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67),
  C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C76(H76), C77(H77),
 C78(H78), C79(H79), C80(H80), C83(H83), C84(H84), C85(H85), C86(H86), C87(H87),
  C89(H89), C90(H90), C91(H91), C92(H92), C93(H93)
2.c Idealised Me refined as rotating group:
 C94(H94A,H94B,H94C), C95(H95A,H95B,H95C)
;
_shelx_res_checksum              10191
_shelx_hkl_checksum              94370
_olex2_date_sample_data_collection 2021-09-03
_olex2_exptl_crystal_mounting_method 'Little loop'
_olex2_submission_original_sample_id BM303
_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 1.278
_oxdiff_exptl_absorpt_empirical_full_min 0.835