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_7710040
_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         'C45 H48 Cl2 N6 Pt2'
_chemical_formula_sum            'C45 H48 Cl2 N6 Pt2'
_chemical_formula_weight         1133.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-10
_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                92.1540(10)
_cell_angle_beta                 90.2040(10)
_cell_angle_gamma                92.1370(10)
_cell_formula_units_Z            2
_cell_length_a                   7.50970(10)
_cell_length_b                   8.75810(10)
_cell_length_c                   33.6683(2)
_cell_measurement_reflns_used    31506
_cell_measurement_temperature    296.8(8)
_cell_measurement_theta_max      76.5750
_cell_measurement_theta_min      2.6110
_cell_volume                     2211.26(4)
_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      air
_diffrn_ambient_temperature      296.8(8)
_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  20.00   0.50    0.40    --  -47.20  35.00 -15.00   88
  2  \w    -41.00  23.00   0.50    0.40    --  -47.20  37.00 120.00  128
  3  \w    -58.00 -33.00   0.50    1.20    -- -106.00 129.00 -42.41   50
  4  \w    -61.00 -35.00   0.50    1.20    -- -106.00 110.00 -88.28   52
  5  \w    -58.00 -33.00   0.50    1.20    -- -106.00 125.00-120.00   50
  6  \w    -69.00 -43.00   0.50    1.20    -- -106.00  77.00-120.00   52
  7  \w    -91.00 -53.00   0.50    1.20    -- -106.00 125.00-150.00   76
  8  \w   -108.00 -69.00   0.50    1.20    -- -106.00 110.00 -88.28   78
  9  \w    -70.00 -33.00   0.50    1.20    -- -106.00  61.00   0.00   74
 10  \w    -67.00  25.00   0.50    0.40    --  -47.20  77.00 -30.00  184
 11  \w     37.00 116.00   0.50    0.40    --   47.20  35.00 -15.00  158
 12  \w    109.00 146.00   0.50    1.20    --  107.75  35.00 -15.00   74
 13  \w     95.00 167.00   0.50    1.20    --  107.75  15.00  60.00  144
 14  \w    143.00 169.00   0.50    1.20    --  107.75  15.00 120.00   52
 15  \w    101.00 139.00   0.50    1.20    --  107.75  15.00 120.00   76
 16  \w     73.00 105.00   0.50    1.20    --  107.75 -94.00 150.00   64
 17  \w     71.00 111.00   0.50    1.20    --  107.75-125.00  30.00   80
 18  \w     42.00 103.00   0.50    1.20    --  107.75 -94.00 -60.00  122
 19  \w     48.00  81.00   0.50    1.20    --  107.75 -77.00-150.00   66
 20  \w     45.00  74.00   0.50    1.20    --  107.75 -94.00-180.00   58
 21  \w     35.00  71.00   0.50    1.20    --  107.75 -61.00-150.00   72
 22  \w     41.00  90.00   0.50    1.20    --  107.75-125.00 -60.00   98
 23  \w     36.00  61.00   0.50    1.20    --  107.75 -61.00  30.00   50
 24  \w     36.00  81.00   0.50    1.20    --  107.75 -77.00  60.00   90
 25  \w     46.00 102.00   0.50    1.20    --  107.75 -94.00  30.00  112
 26  \w     38.00  68.00   0.50    1.20    --  107.75-125.00 150.00   60
 27  \w     40.00  67.00   0.50    1.20    --  107.75 -61.00   0.00   54
 28  \w     39.00  66.00   0.50    1.20    --  107.75 -61.00 -30.00   54
 29  \w     50.00  76.00   0.50    0.40    --   47.20-125.00-150.00   52
 30  \w    -17.00   8.00   0.50    0.40    --   47.20 -35.00-172.00   50
 31  \w    -18.00  58.00   0.50    0.40    --   47.20 -57.00-180.00  152
 32  \w    101.00 176.00   0.50    1.20    --  107.75  30.00-180.00  150
 33  \w     95.00 160.00   0.50    1.20    --  107.75  45.00-150.00  130
 34  \w     89.00 114.00   0.50    0.40    --   47.20 125.00-180.00   50
 35  \w     85.00 178.00   0.50    1.20    --  107.75  77.00 -90.00  186
 36  \w    -69.00 -40.00   0.50    1.20    -- -106.00  61.00 150.00   58
 37  \w    -91.00 -41.00   0.50    1.20    -- -106.00  77.00  90.00  100
 38  \w   -108.00 -33.00   0.50    1.20    -- -106.00 110.00 126.46  150
 39  \w   -112.00 -46.00   0.50    1.20    -- -106.00 125.00 150.00  132
 40  \w   -107.00 -34.00   0.50    1.20    -- -106.00 106.00  80.53  146
 41  \w   -107.00 -70.00   0.50    1.20    -- -106.00 107.00   3.12   74
 42  \w   -107.00 -82.00   0.50    1.20    -- -106.00 111.00  36.76   50
 43  \w   -117.00 -89.00   0.50    1.20    -- -106.00 135.00  84.26   56
 44  \w   -124.00 -82.00   0.50    1.20    -- -106.00 142.00  47.74   84
 45  \w   -120.00 -36.00   0.50    1.20    -- -106.00 136.00 -90.93  168
 46  \w   -105.00 -79.00   0.50    1.20    -- -106.00 125.00-120.00   52
 47  \w   -108.00 -64.00   0.50    1.20    -- -106.00 111.00-176.93   88
 48  \w   -119.00 -45.00   0.50    0.40    --  -47.20 -35.00-172.00  148
 49  \w   -123.00 -97.00   0.50    1.20    -- -106.00 141.00 179.62   52
 50  \w   -129.00-104.00   0.50    1.20    -- -106.00 -45.00  60.00   50
 51  \w   -160.00 -98.00   0.50    1.20    -- -106.00 -30.00 -90.00  124
 52  \w   -172.00-120.00   0.50    1.20    -- -106.00 -35.00-172.00  104
 53  \w    -27.00  -1.00   0.50    0.40    --  -47.20  35.00 -15.00   52
 54  \w    -52.00 -27.00   0.50    0.40    --   10.00 150.00  28.72   50
 55  \w    -13.00  21.00   0.50    0.40    --   18.00 100.00  86.79   68
 56  \w     -4.00  21.00   0.50    0.40    --   22.00  85.00-107.90   50
 57  \w     -2.00  23.00   0.50    0.40    --   30.00  96.00-148.24   50
 58  \w     12.00  37.00   0.50    0.40    --   42.00  92.00 168.92   50
 59  \w     16.00  42.00   0.50    0.40    --   42.00  89.00 -46.89   52
 60  \w     23.00  49.00   0.50    0.40    --   46.00  79.00  55.59   52
 61  \w    -50.00 -24.00   0.50    0.40    --  -47.20 -77.00  30.00   52
 62  \w     35.00  62.00   0.50    0.40    --   47.20  37.00-180.00   54
 63  \w     27.00  80.00   0.50    0.40    --   50.00  78.00 -98.53  106
 64  \w     30.00  55.00   0.50    0.40    --   54.00  80.00  95.50   50
 65  \w     30.00  66.00   0.50    0.40    --   54.00  80.00-152.06   72
 66  \w     31.00  56.00   0.50    0.40    --   54.00  77.00-169.54   50
 67  \w     31.00  57.00   0.50    0.40    --   54.00  79.00 130.90   52
 68  \w     96.00 124.00   0.50    0.40    --   54.00  79.00  21.63   56
 69  \w     30.00  56.00   0.50    0.40    --   54.00  79.00  21.63   52
 70  \w     34.00  60.00   0.50    0.40    --   58.00  79.00 -23.51   52
 71  \w     35.00  64.00   0.50    0.40    --   58.00  78.00 -74.13   58
 72  \w     35.00  64.00   0.50    0.40    --   58.00  77.00-144.56   58
 73  \w     36.00  62.00   0.50    0.40    --   58.00  76.00  71.32   52
 74  \w     40.00  66.00   0.50    0.40    --   62.00  76.00-110.94   52
 75  \w     38.00  63.00   0.50    0.40    --   62.00  80.00 139.31   50
 76  \w     39.00  65.00   0.50    0.40    --   62.00  78.00  84.81   52
 77  \w     43.00  81.00   0.50    0.40    --   66.00  78.00 -98.42   76
 78  \w     42.00  68.00   0.50    0.40    --   66.00  79.00 -64.71   52
 79  \w     43.00  69.00   0.50    0.40    --   66.00  78.00 110.80   52
 80  \w     42.00  68.00   0.50    0.40    --   66.00  79.00  20.13   52
 81  \w    -76.00 -51.00   0.50    0.40    --  -70.00 -68.00 161.72   50
 82  \w     47.00  72.00   0.50    0.40    --   70.00  78.00 -37.75   50
 83  \w     48.00  81.00   0.50    0.40    --   70.00  76.00 -16.55   66
 84  \w     48.00  74.00   0.50    0.40    --   70.00  77.00 158.33   52
 85  \w    -79.00 -53.00   0.50    0.40    --  -74.00 -74.00 167.63   52
 86  \w    -79.00 -53.00   0.50    0.40    --  -74.00 -73.00  27.01   52
 87  \w    -78.00 -64.50   0.50    0.40    --  -74.00 -73.00-168.76   27
;
_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      -0.1626618000
_diffrn_orient_matrix_UB_12      0.1021580000
_diffrn_orient_matrix_UB_13      0.0009088000
_diffrn_orient_matrix_UB_21      -0.1109072000
_diffrn_orient_matrix_UB_22      -0.1271972000
_diffrn_orient_matrix_UB_23      0.0198760000
_diffrn_orient_matrix_UB_31      0.0581683000
_diffrn_orient_matrix_UB_32      0.0664342000
_diffrn_orient_matrix_UB_33      0.0412412000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            44150
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        62.498
_diffrn_reflns_theta_max         62.498
_diffrn_reflns_theta_min         2.627
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.060
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84520
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       prism
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.695
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         7053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+10.6451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6680
_reflns_number_total             7053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00252c2.cif
_cod_data_source_block           16023_kmv288_1
_cod_database_code               7710040
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C25 H27 Cl1 N4 Pt1'
_shelx_estimated_absorpt_t_max   0.780
_shelx_estimated_absorpt_t_min   0.421
_diffrn_oxdiff_digest_frames
;
013b7150c44ff553883fde7551b7f0d25f000329bcc
;
_diffrn_oxdiff_digest_hkl
;
0161ede3c2e07ac1bed2f9434edbe96b95ca5e
;
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.99821(17)
 0.00179(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C29(H29), C5(H5), C6(H6), C20(H20), C31(H31), C3(H3), C4(H4),
 C39(H39), C13(H13), C41(H41), C11(H11)
3.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C24(H24A,H24B,H24C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C15(H15A,H15B,H15C), C25(H25A,H25B,H25C), C35(H35A,H35B,H35C), C43(H43A,
 H43B,H43C), C45(H45A,H45B,H45C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C),
 C44(H44A,H44B,H44C)
;
_shelx_res_checksum              84552
_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 1.722
_oxdiff_exptl_absorpt_empirical_full_min 0.519