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_7060165
_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         'C21 H22 Cl N5 Pt S, C H Cl3'
_chemical_formula_sum            'C22 H23 Cl4 N5 Pt S'
_chemical_formula_weight         726.40
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-28
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
;
2020-10-28 deposited with the CCDC.	2020-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.722(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1744(4)
_cell_length_b                   7.7314(3)
_cell_length_c                   20.6353(5)
_cell_measurement_reflns_used    3913
_cell_measurement_temperature    273
_cell_measurement_theta_max      27.0800
_cell_measurement_theta_min      3.1230
_cell_volume                     2738.76(14)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      273
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -96.00  -62.00   1.0000    2.0500
omega____ theta____ kappa____ phi______ frames
    -      -22.5803 -178.0000   30.0000 34

  2 omega  -31.00   95.00   1.0000    2.0500
omega____ theta____ kappa____ phi______ frames
    -       23.5178    0.0000 -150.0000 126

  3 omega    8.00   77.00   1.0000    2.0500
omega____ theta____ kappa____ phi______ frames
    -       23.5178   38.0000   90.0000 69

  4 omega  -36.00   48.00   1.0000    2.0500
omega____ theta____ kappa____ phi______ frames
    -       23.5178  -77.0000  120.0000 84

  5 omega   74.00  100.00   1.0000    2.0500
omega____ theta____ kappa____ phi______ frames
    -       23.5178 -178.0000 -180.0000 26

  6 omega    4.00    7.00   1.0000    2.0500
omega____ theta____ kappa____ phi______ frames
    -       23.5178   77.0000  -60.0000 3
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0376653000
_diffrn_orient_matrix_UB_12      0.0132584000
_diffrn_orient_matrix_UB_13      -0.0122819000
_diffrn_orient_matrix_UB_21      -0.0047463000
_diffrn_orient_matrix_UB_22      -0.0743284000
_diffrn_orient_matrix_UB_23      -0.0198864000
_diffrn_orient_matrix_UB_31      -0.0162935000
_diffrn_orient_matrix_UB_32      0.0521404000
_diffrn_orient_matrix_UB_33      -0.0252253000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17663
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.814
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.610
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear greenish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.782
_refine_diff_density_min         -1.607
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0243P)^2^+0.3582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4750
_reflns_number_total             6281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj05386d3.cif
_cod_data_source_block           8a
_cod_depositor_comments
'Adding full bibliography for 7060163--7060166.cif.'
_cod_database_code               7060165
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C21 H22 Cl N5 Pt S'
_shelx_estimated_absorpt_t_max   0.604
_shelx_estimated_absorpt_t_min   0.604
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.51
_olex2_refinement_description
;
1. Others
 Fixed Sof: Cl1S(0.5) Cl2(0.5) Cl2S(0.5) Cl3S(0.5) Cl3(0.5) Cl4(0.5)
 Fixed Uiso: H20(0.055) H21A(0.084) H21B(0.084) H21C(0.084) H6(0.1) H9A(0.132)
 H9B(0.132) H9C(0.132) H8A(0.126) H8B(0.126) H8C(0.126) H4(0.101) H5(0.113)
 H15(0.16) H18A(0.181) H18B(0.181) H18C(0.181) H14(0.192) H13(0.167)
 H17A(0.186) H17B(0.186) H17C(0.186)
 Fixed X: H20(0.561014) H21A(0.609065) H21B(0.599511) H21C(0.544051)
 H6(0.189879) H9A(0.346852) H9B(0.311944) H9C(0.369465) H8A(0.252421)
 H8B(0.161395) H8C(0.211371) H4(0.094669) H5(0.086776) H15(-0.027138)
 H18A(0.153492) H18B(0.101432) H18C(0.156732) H14(-0.122978) H13(-0.098648)
 H17A(0.066972) H17B(-0.015437) H17C(0.055974)
 Fixed Y: H20(0.904459) H21A(0.993517) H21B(1.120237) H21C(1.135867)
 H6(0.103217) H9A(0.323765) H9B(0.137471) H9C(0.209737) H8A(0.731734)
 H8B(0.746843) H8C(0.806861) H4(0.493046) H5(0.22152) H15(0.14274)
 H18A(0.29654) H18B(0.130022) H18C(0.172845) H14(0.314919) H13(0.575449)
 H17A(0.752564) H17B(0.81527) H17C(0.828144)
 Fixed Z: H20(0.747807) H21A(0.602028) H21B(0.660561) H21C(0.599103)
 H6(0.677454) H9A(0.62001) H9B(0.626647) H9C(0.680513) H8A(0.799758)
 H8B(0.795208) H8C(0.736982) H4(0.771962) H5(0.731965) H15(0.545701)
 H18A(0.500859) H18B(0.501404) H18C(0.561077) H14(0.587973) H13(0.631833)
 H17A(0.671915) H17B(0.647061) H17C(0.601741)
;
_shelx_res_checksum              71679
_olex2_submission_special_instructions 'No special instructions were received'