Experimental and computational tuning of metalla-N-heterocyclic carbenes at palladium(ii) and platinum(ii) centers
Kashina, Maria V.; Luzyanin, Konstantin V.; Katlenok, Eugene A.; Novikov, Alexander S.; Kinzhalov, Mikhail A.; Dalton Transactions  (2022) –; doi:10.1039/D2DT00252C

data_7710042
_publ_section_title
;
 Experimental and computational tuning of metalla-N-heterocyclic carbenes
 at palladium(ii) and platinum(ii) centers
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00252C
_journal_year                    2022
_chemical_formula_moiety         'C46 H47 N9 Pt2 S2'
_chemical_formula_sum            'C46 H47 N9 Pt2 S2'
_chemical_formula_weight         1180.22
_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             2022-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-24 deposited with the CCDC.	2022-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.8860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.08540(10)
_cell_length_b                   30.3986(3)
_cell_length_c                   18.7295(2)
_cell_measurement_reflns_used    54662
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      77.0520
_cell_measurement_theta_min      2.7740
_cell_volume                     4559.89(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -24.00  25.00   0.50    0.09    --   47.20 -19.00   0.00   98
  2  \w    -22.00  25.00   0.50    0.09    --   47.20 -19.00 -60.00   94
  3  \w     95.00 178.00   0.50    0.35    --  107.75  30.00-120.00  166
  4  \w    103.00 128.00   0.50    0.35    --  107.75 120.00 -49.00   50
  5  \w    115.00 155.00   0.50    0.35    --  107.75  61.00  30.00   80
  6  \w    101.00 178.00   0.50    0.35    --  107.75  15.00 -30.00  154
  7  \w     84.00 111.00   0.50    0.09    --   47.20 125.00 150.00   54
  8  \w     63.00  88.00   0.50    0.09    --   47.20 154.00 108.00   50
  9  \w     90.00 136.00   0.50    0.35    --  107.75 154.00 108.00   92
 10  \w     56.00  84.00   0.50    0.35    --  107.75 154.00 108.00   56
 11  \w     76.00 114.00   0.50    0.09    --   47.20 125.00-120.00   76
 12  \w     74.00 120.00   0.50    0.09    --   47.20 125.00-150.00   92
 13  \w     35.00  71.00   0.50    0.35    --  107.75 -61.00-120.00   72
 14  \w     43.00  71.00   0.50    0.35    --  107.75 -61.00 -90.00   56
 15  \w     61.00  87.00   0.50    0.35    --  107.75 -94.00-150.00   52
 16  \w     71.00 105.00   0.50    0.35    --  107.75 -77.00-180.00   68
 17  \w     58.00  94.00   0.50    0.35    --  107.75 -94.00-120.00   72
 18  \w     42.00 110.00   0.50    0.35    --  107.75-120.00-133.00  136
 19  \w     38.00  71.00   0.50    0.35    --  107.75 -61.00 -60.00   66
 20  \w     35.00  60.00   0.50    0.35    --  107.75 -61.00   0.00   50
 21  \w     39.00  70.00   0.50    0.35    --  107.75 -61.00  90.00   62
 22  \w     39.00  67.00   0.50    0.35    --  107.75 -61.00 120.00   56
 23  \w     36.00  94.00   0.50    0.35    --  107.75-125.00 120.00  116
 24  \w     75.00 112.00   0.50    0.35    --  107.75-125.00  60.00   74
 25  \w     59.00  84.00   0.50    0.35    --  107.75-154.00  68.00   50
 26  \w     22.00  92.00   0.50    0.09    --   47.20-120.00-133.00  140
 27  \w    -58.00 -33.00   0.50    0.35    -- -106.00  61.00  90.00   50
 28  \w    -85.00 -33.00   0.50    0.35    -- -106.00  77.00 150.00  104
 29  \w    -94.00 -69.00   0.50    0.09    --  -47.20 154.00 108.00   50
 30  \w    -78.00 -51.00   0.50    0.09    --  -47.20 120.00 -49.00   54
 31  \w   -104.00 -73.00   0.50    0.35    -- -106.00 120.00 -49.00   62
 32  \w    -71.00 -46.00   0.50    0.35    -- -106.00  61.00 -30.00   50
 33  \w    -95.00 -69.00   0.50    0.35    -- -106.00 154.00 108.00   52
 34  \w   -124.00 -99.00   0.50    0.35    -- -106.00 143.00-100.44   50
 35  \w   -112.00 -43.00   0.50    0.35    -- -106.00 125.00-150.00  138
 36  \w   -108.00 -76.00   0.50    0.35    -- -106.00 109.00 -91.24   64
 37  \w   -177.00-122.00   0.50    0.35    -- -106.00 -30.00  60.00  110
 38  \w   -109.00 -73.00   0.50    0.09    --  -47.20-125.00 -90.00   72
 39  \w   -111.00 -86.00   0.50    0.09    --  -47.20-154.00  68.00   50
 40  \w   -151.00-126.00   0.50    0.35    -- -106.00-120.00-133.00   50
 41  \w   -132.00-101.00   0.50    0.35    -- -106.00 154.00 108.00   62
 42  \w    -21.00  26.00   0.50    0.09    --   47.20 -19.00-120.00   94
 43  \w     86.00 118.00   0.50    0.09    --   47.20 125.00 -90.00   64
 44  \w     21.00  62.00   0.50    0.09    --   47.20 -57.00 -90.00   82
 45  \w     54.00 120.00   0.50    0.09    --   47.20  37.00  60.00  132
 46  \w    -71.00 -46.00   0.50    0.35    -- -106.00  61.00 -60.00   50
 47  \w   -177.00-134.00   0.50    0.35    -- -106.00 -45.00 120.00   86
 48  \w    -59.00 -33.00   0.50    0.35    -- -106.00  61.00 -30.00   52
 49  \w    -61.00 -36.00   0.50    0.35    -- -106.00 125.00  90.00   50
 50  \w    -66.00 -40.00   0.50    0.35    -- -106.00 109.00 169.33   52
 51  \w   -118.00 -90.00   0.50    0.35    -- -106.00 -61.00 150.00   56
 52  \w   -108.00 -76.00   0.50    0.35    -- -106.00 110.00  50.58   64
 53  \w    -95.00 -65.00   0.50    0.35    -- -106.00 125.00  60.00   60
 54  \w   -108.00 -72.00   0.50    0.35    -- -106.00 112.00  56.71   72
 55  \w   -168.00-122.00   0.50    0.35    -- -106.00 -61.00  90.00   92
 56  \w   -112.00 -85.00   0.50    0.35    -- -106.00 125.00  90.00   54
 57  \w   -123.00 -86.00   0.50    0.35    -- -106.00 141.00  79.86   74
 58  \w    -85.00 -59.00   0.50    0.35    -- -106.00 141.00  79.86   52
 59  \w   -108.00 -83.00   0.50    0.35    -- -106.00 110.00 -33.26   50
 60  \w   -176.00-144.00   0.50    0.35    -- -106.00 -61.00 150.00   64
 61  \w    -86.00 -61.00   0.50    0.35    -- -106.00 154.00 108.00   50
 62  \w   -108.00 -83.00   0.50    0.35    -- -106.00 109.00 154.77   50
 63  \w   -107.00 -81.00   0.50    0.35    -- -106.00 109.00 169.33   52
 64  \w     78.00 103.00   0.50    0.35    --  107.75 -77.00 -30.00   50
 65  \w     43.00  69.00   0.50    0.35    --  107.75-125.00  30.00   52
 66  \w     41.00  73.00   0.50    0.35    --  107.75 -77.00 -30.00   64
 67  \w    102.00 168.00   0.50    0.35    --  107.75  61.00-150.00  132
 68  \w     41.00  78.00   0.50    0.35    --  107.75 -94.00 120.00   74
 69  \w    145.00 174.00   0.50    0.35    --  107.75  77.00   0.00   58
 70  \w     83.00 109.00   0.50    0.35    --  107.75-125.00  30.00   52
 71  \w     35.00  60.00   0.50    0.35    --  107.75 -61.00 -90.00   50
 72  \w     76.00 105.00   0.50    0.35    --  107.75 -77.00 -90.00   58
 73  \w     45.00  70.00   0.50    0.35    --  107.75 -77.00 -90.00   50
 74  \w     80.00 105.00   0.50    0.35    --  107.75 -77.00 120.00   50
 75  \w     95.00 125.00   0.50    0.35    --  107.75  77.00   0.00   60
 76  \w     44.00  69.00   0.50    0.35    --  107.75 -61.00  60.00   50
 77  \w     35.00  60.00   0.50    0.35    --  107.75 -61.00-150.00   50
 78  \w    147.00 177.00   0.50    0.35    --  107.75  15.00   0.00   60
 79  \w     85.00 112.00   0.50    0.35    --  107.75-125.00  90.00   54
 80  \w    138.00 166.00   0.50    0.35    --  107.75  15.00  30.00   56
 81  \w     95.00 127.00   0.50    0.35    --  107.75  15.00   0.00   64
 82  \w     71.00  97.00   0.50    0.35    --  107.75 -77.00-120.00   52
 83  \w     38.00  64.00   0.50    0.35    --  107.75 -77.00-120.00   52
 84  \w     48.00  74.00   0.50    0.35    --  107.75 -94.00  60.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1029602000
_diffrn_orient_matrix_UB_12      0.0015848000
_diffrn_orient_matrix_UB_13      0.0633481000
_diffrn_orient_matrix_UB_21      0.0218582000
_diffrn_orient_matrix_UB_22      0.0503182000
_diffrn_orient_matrix_UB_23      0.0042011000
_diffrn_orient_matrix_UB_31      -0.1609663000
_diffrn_orient_matrix_UB_32      0.0057726000
_diffrn_orient_matrix_UB_33      -0.0535576000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            81279
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.499
_diffrn_reflns_theta_max         67.499
_diffrn_reflns_theta_min         2.790
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.497
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       prism
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         8233
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0212
_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^)+(0.0198P)^2^+7.8265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0498
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8064
_reflns_number_total             8233
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00252c2.cif
_cod_data_source_block           2ver0-15674_kmv-261
_cod_database_code               7710042
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C46 H48 N9 S2 Pt2 '
_shelx_estimated_absorpt_t_max   0.368
_shelx_estimated_absorpt_t_min   0.368
_diffrn_oxdiff_digest_frames
;
01c6ea38619fd2cf191c221520eace1e5600069b49f
;
_diffrn_oxdiff_digest_hkl
;
01d2477a6c4a2dc148ba76872b00b16afec143
;
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 Aromatic/amide H refined with riding coordinates:
 C21(H21), C3(H3), C19(H19), C4(H4), C12(H12), C28(H28), C5(H5), C30(H30),
 C10(H10), C38(H38), C40(H40)
2.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C25(H25A,H25B,H25C), C23(H23A,H23B,H23C), C16(H16A,H16B,
 H16C), C34(H34A,H34B,H34C), C14(H14A,H14B,H14C), C33(H33A,H33B,H33C), C15(H15A,
 H15B,H15C), C24(H24A,H24B,H24C), C44(H44A,H44B,H44C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C)
;
_shelx_res_checksum              60712
_shelx_fab_checksum              66453
_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 2.030
_oxdiff_exptl_absorpt_empirical_full_min 0.614