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_7709904
_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         'C37 H58 Cl2 N2 Pt S'
_chemical_formula_sum            'C37 H58 Cl2 N2 Pt S'
_chemical_formula_weight         828.89
_chemical_name_systematic        BM393
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-01-20 deposited with the CCDC.	2022-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.3300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   24.1264(4)
_cell_length_b                   26.3470(3)
_cell_length_c                   24.1852(4)
_cell_measurement_reflns_used    35350
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4910
_cell_measurement_theta_min      2.8130
_cell_volume                     15373.3(4)
_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(2)
_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 0.884
_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    -25.00  21.00   1.00   40.00    --    7.83  77.00 -90.00   46
  2  \w    -66.00  32.00   1.00   40.00    --    7.83 -38.00   0.00   98
  3  \w    -82.00  19.00   1.00   40.00    --   -8.69 -57.00 -60.00  101
  4  \w    -42.00  18.00   1.00   40.00    --    7.83 -77.00 -90.00   60
  5  \w    -41.00  21.00   1.00   40.00    --   -8.69  77.00 120.00   62
;
_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      0.0234644000
_diffrn_orient_matrix_UB_12      0.0134744000
_diffrn_orient_matrix_UB_13      0.0099623000
_diffrn_orient_matrix_UB_21      -0.0176006000
_diffrn_orient_matrix_UB_22      0.0161079000
_diffrn_orient_matrix_UB_23      0.0155250000
_diffrn_orient_matrix_UB_31      0.0019359000
_diffrn_orient_matrix_UB_32      -0.0168435000
_diffrn_orient_matrix_UB_33      0.0228065000
_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  0.0494
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            79382
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.770
_diffrn_reflns_theta_min         2.467
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.870
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.662
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       irregular
_exptl_crystal_F_000             6752
_exptl_crystal_preparation       Synthesis
_exptl_crystal_recrystallization_method 'iPrOH diffusion in water'
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.101
_refine_diff_density_max         1.280
_refine_diff_density_min         -1.729
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         17698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0203P)^2^+70.1126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16245
_reflns_number_total             17698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00504b2.cif
_cod_data_source_block           bm393-2
_cod_database_code               7709904
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C37 H58 Cl2 N2 Pt S'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8171(4)
 0.1829(4)
2. 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
3.a Ternary CH refined with riding coordinates:
 C10(H10), C15(H15), C26(H26), C31(H31), C47(H47), C52(H52), C63(H63), C68(H68)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C16(H16A,H16B), C18(H18A,H18B), C27(H27A,
 H27B), C29(H29A,H29B), C32(H32A,H32B), C34(H34A,H34B), C48(H48A,H48B),
 C50(H50A,H50B), C53(H53A,H53B), C55(H55A,H55B), C64(H64A,H64B), C66(H66A,H66B),
  C69(H69A,H69B), C71(H71A,H71B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C22(H22), C23(H23), C24(H24),
 C39(H39), C40(H40), C43(H43), C44(H44), C45(H45), C59(H59), C60(H60), C61(H61)
3.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C49(H49A,H49B,H49C),
 C51(H51A,H51B,H51C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C65(H65A,H65B,
 H65C), C67(H67A,H67B,H67C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C73(H73A,
 H73B,H73C), C74(H74A,H74B,H74C)
;
_shelx_res_checksum              84291
_shelx_hkl_checksum              53313
_olex2_date_sample_data_collection 2022-01-17
_olex2_exptl_crystal_mounting_method 'Litho loop'
_olex2_submission_original_sample_id BM393
_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 1.289
_oxdiff_exptl_absorpt_empirical_full_min 0.794