PdII- and PtII-mediated coupling of aryl isocyanides with N-heterocyclic thiones
Popov, Roman A.; Mikherdov, Alexander S.; Novikov, Alexander S.; Myznikov, Leonid V.; Boyarskiy, Vadim P.; New Journal of Chemistry 45 (2021) 1785–1789; doi:10.1039/D0NJ05386D

data_7060166
_publ_section_title
;
 PdII- and PtII-mediated coupling of aryl isocyanides with N-heterocyclic
 thiones
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1785
_journal_page_last               1789
_journal_paper_doi               10.1039/D0NJ05386D
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C22 H23 Cl N4 Pt S'
_chemical_formula_sum            'C22 H23 Cl N4 Pt S'
_chemical_formula_weight         606.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-04-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-15 deposited with the CCDC.	2020-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.247(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2546(18)
_cell_length_b                   15.9382(14)
_cell_length_c                   7.3011(6)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      31.1110
_cell_measurement_theta_min      3.4150
_cell_volume                     2231.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3829
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.912
_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     -9.00  28.00   1.00    7.96    --   16.86  38.00-120.00   37
  2  \w     49.00  76.00   1.00    7.96    --   16.86  38.00-120.00   27
  3  \w      2.00  43.00   1.00    7.96    --   16.86 -57.00-180.00   41
  4  \w     58.00 105.00   1.00    7.96    --   16.86-178.00  90.00   47
  5  \w     57.00 106.00   1.00    7.96    --   16.86 178.00 -30.00   49
  6  \w    -57.00  27.00   1.00    7.96    --   16.86 -57.00  90.00   84
  7  \w    -69.00   7.00   1.00    7.96    --  -14.99 -19.00 120.00   76
  8  \w    -14.00  19.00   1.00    7.96    --  -14.99 -99.00 -60.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0068297000
_diffrn_orient_matrix_UB_12      0.0426343000
_diffrn_orient_matrix_UB_13      0.0199486000
_diffrn_orient_matrix_UB_21      -0.0353166000
_diffrn_orient_matrix_UB_22      -0.0055105000
_diffrn_orient_matrix_UB_23      -0.0341756000
_diffrn_orient_matrix_UB_31      -0.0083867000
_diffrn_orient_matrix_UB_32      -0.0116822000
_diffrn_orient_matrix_UB_33      0.0893116000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            24705
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.421
_diffrn_reflns_theta_min         3.080
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.518
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.804
_exptl_crystal_description       prism
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.785
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         6738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0128P)^2^+0.2986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5702
_reflns_number_total             6738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj05386d3.cif
_cod_data_source_block           7a
_cod_depositor_comments
'Adding full bibliography for 7060163--7060166.cif.'
_cod_database_code               7060166
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C22 Cl N4 Pt S'
_shelx_estimated_absorpt_t_max   0.562
_shelx_estimated_absorpt_t_min   0.562
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.51
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H9A(0.042) H9B(0.042) H9C(0.042) H22A(0.027) H22B(0.027)
 H22C(0.027) H4(0.027) H6(0.027) H8A(0.04) H8B(0.04) H8C(0.04) H18A(0.043)
 H18B(0.043) H18C(0.043) H21(0.023) H5(0.032) H15(0.028) H20(0.022) H13(0.028)
 H14(0.029) H17A(0.04) H17B(0.04) H17C(0.04)
 Fixed X: H9A(0.345616) H9B(0.302173) H9C(0.332148) H22A(0.6145)
 H22B(0.605481) H22C(0.572784) H4(0.083148) H6(0.179636) H8A(0.216274)
 H8B(0.145912) H8C(0.216917) H18A(0.246683) H18B(0.207059) H18C(0.235426)
 H21(0.41628) H5(0.077745) H15(0.085845) H20(0.531248) H13(-0.02048) H14(-
 0.017473) H17A(0.098919) H17B(0.036476) H17C(0.1134)
 Fixed Y: H9A(0.458934) H9B(0.460674) H9C(0.375581) H22A(0.400671)
 H22B(0.321782) H22C(0.407937) H4(0.368881) H6(0.461511) H8A(0.264216)
 H8B(0.306555) H8C(0.352156) H18A(0.697669) H18B(0.691481) H18C(0.610018)
 H21(0.238665) H5(0.435553) H15(0.714437) H20(0.225447) H13(0.631326)
 H14(0.700827) H17A(0.504378) H17B(0.560696) H17C(0.590912)
 Fixed Z: H9A(0.109467) H9B(-0.08287) H9C(-0.00215) H22A(0.744548)
 H22B(0.868409) H22C(0.918472) H4(0.338232) H6(-0.081236) H8A(0.558746)
 H8B(0.600226) H8C(0.655063) H18A(0.13357) H18B(-0.063318) H18C(0.038021)
 H21(0.45903) H5(0.055313) H15(-0.057657) H20(0.630089) H13(0.353254)
 H14(0.0755) H17A(0.568268) H17B(0.617226) H17C(0.666485)
;
_shelx_res_checksum              2067
_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 2.205
_oxdiff_exptl_absorpt_empirical_full_min 0.711