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_7709905
_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_absolute_configuration ad
_chemical_formula_moiety         'C29 H40 Cl4 N2 Pt S'
_chemical_formula_sum            'C29 H40 Cl4 N2 Pt S'
_chemical_formula_weight         785.57
_chemical_name_systematic        BM177
_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             2021-02-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.94800(10)
_cell_length_b                   17.51800(10)
_cell_length_c                   17.81620(10)
_cell_measurement_reflns_used    85010
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.4890
_cell_measurement_theta_min      3.0550
_cell_volume                     3104.81(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  (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 0.977
_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    -15.00  84.00   1.00   14.15    --   10.01  38.00 150.00   99
  2  \w     39.00  99.00   1.00   14.15    --   10.01 178.00   0.00   60
  3  \w    -78.00  98.00   1.00   14.15    --   10.01   0.00 -30.00  176
  4  \w    -31.00  90.00   1.00   14.15    --   10.01  19.00  60.00  121
  5  \w    -88.00 -43.00   1.00   14.15    --  -11.19 155.00  27.42   45
  6  \w    -67.00 -26.00   1.00   14.15    --  -11.19 124.00-177.06   41
  7  \w    -42.00  21.00   1.00   14.15    --  -11.19 -77.00-180.00   63
  8  \w    -88.00 -43.00   1.00   14.15    --  -11.19 155.00-112.80   45
  9  \w    -15.00  51.00   1.00   14.15    --   10.01 -99.00-180.00   66
 10  \w    -15.00  30.00   1.00   14.15    --  -11.19 -99.00 -60.00   45
 11  \w    -87.00 -43.00   1.00   14.15    --  -11.19 154.00  94.38   44
 12  \w    -65.00 -24.00   1.00   14.15    --  -11.19 121.00-148.57   41
 13  \w    -88.00 -43.00   1.00   14.15    --  -11.19 155.00 -69.80   45
 14  \w    -88.00 -43.00   1.00   14.15    --  -11.19 155.00 -32.96   45
 15  \w    -78.00  49.00   1.00   14.15    --   10.01   0.00-120.00  127
 16  \w    -78.00  98.00   1.00   14.15    --   10.01   0.00-150.00  176
 17  \w    -78.00  98.00   1.00   14.15    --   10.01   0.00-180.00  176
 18  \w    -15.00  30.00   1.00   14.15    --  -11.19 -99.00  90.00   45
 19  \w    -15.00  30.00   1.00   14.15    --  -11.19 -99.00-120.00   45
 20  \w    -89.00 -45.00   1.00   14.15    --  -11.19 157.00  62.69   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      0.0133321000
_diffrn_orient_matrix_UB_12      -0.0331360000
_diffrn_orient_matrix_UB_13      0.0216391000
_diffrn_orient_matrix_UB_21      0.0693327000
_diffrn_orient_matrix_UB_22      0.0030963000
_diffrn_orient_matrix_UB_23      -0.0087591000
_diffrn_orient_matrix_UB_31      0.0098411000
_diffrn_orient_matrix_UB_32      0.0230658000
_diffrn_orient_matrix_UB_33      0.0322573000
_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  0.0407
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            138672
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.673
_diffrn_reflns_theta_min         2.565
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.953
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.602
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1560
_exptl_crystal_preparation       Synthesis
_exptl_crystal_recrystallization_method 'Pentane diffusion in DCM'
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.145
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 3444 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0401(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         8428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0171
_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^)+(0.0171P)^2^+1.4545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0352
_refine_ls_wR_factor_ref         0.0358
_reflns_Friedel_coverage         0.764
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.933
_reflns_number_gt                8165
_reflns_number_total             8428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00504b2.cif
_cod_data_source_block           bm177-2
_cod_database_code               7709905
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C29 H41 Cl4 N2 Pt S'
_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.a Ternary CH refined with riding coordinates:
 C13(H13), C10(H10), C22(H22), C25(H25)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C6(H6), C20(H20), C8(H8), C7(H7), C19(H19)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C28(H28A,H28B,H28C), C26(H26A,H26B,
 H26C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C15(H15A,H15B,H15C), C12(H12A,
 H12B,H12C), C29(H29A,H29B,H29C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              80277
_shelx_hkl_checksum              44747
_olex2_date_sample_data_collection 2021-02-16
_olex2_exptl_crystal_mounting_method 'Little loop'
_olex2_submission_original_sample_id BM177
_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 1.294
_oxdiff_exptl_absorpt_empirical_full_min 0.812