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_7710041
_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 Pd2 S2'
_chemical_formula_sum            'C46 H47 N9 Pd2 S2'
_chemical_formula_weight         1002.84
_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             2022-01-10
_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                90
_cell_angle_beta                 98.347(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2035(2)
_cell_length_b                   30.9219(8)
_cell_length_c                   18.7259(5)
_cell_measurement_reflns_used    17620
_cell_measurement_temperature    297.2(2)
_cell_measurement_theta_max      77.0970
_cell_measurement_theta_min      2.6030
_cell_volume                     4699.8(2)
_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      297.2(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -34.00  25.00   0.50    6.00    --  -47.20  49.00   1.00  118
  2  \w     35.00  69.00   0.50    6.00    --   47.20  49.00   1.00   68
  3  \w     79.00 115.00   0.50    6.00    --   47.20  49.00   1.00   72
  4  \w    104.00 159.00   0.50   25.00    --  107.75  49.00   1.00  110
  5  \w    132.00 175.00   0.50   25.00    --  107.75  61.00 -60.00   86
  6  \w    117.00 161.00   0.50   25.00    --  107.75  61.00  30.00   88
  7  \w    109.00 158.00   0.50   25.00    --  107.75  77.00  60.00   98
  8  \w     95.00 164.00   0.50   25.00    --  107.75  30.00 120.00  138
  9  \w     93.00 129.00   0.50   25.00    --  107.75  61.00 -60.00   72
 10  \w     84.00 119.00   0.50    6.00    --   47.20 125.00-120.00   70
 11  \w     -9.00  47.00   0.50    6.00    --   47.20 -49.00-146.00  112
 12  \w     39.00  67.00   0.50   25.00    --  107.75 -61.00 -90.00   56
 13  \w     35.00  71.00   0.50   25.00    --  107.75 -61.00-120.00   72
 14  \w     41.00 104.00   0.50   25.00    --  107.75 -77.00-180.00  126
 15  \w     43.00  93.00   0.50   25.00    --  107.75 -77.00  60.00  100
 16  \w    -26.00  18.00   0.50    6.00    --   47.20 -19.00  60.00   88
 17  \w   -120.00 -34.00   0.50    6.00    --  -47.20 -49.00-146.00  172
 18  \w    -69.00 -34.00   0.50   25.00    -- -106.00  61.00  30.00   70
 19  \w    -63.00 -38.00   0.50   25.00    -- -106.00  61.00   0.00   50
 20  \w    -70.00 -37.00   0.50   25.00    -- -106.00  61.00 120.00   66
 21  \w    -66.00 -37.00   0.50   25.00    -- -106.00  61.00 150.00   58
 22  \w    -96.00 -35.00   0.50   25.00    -- -106.00  77.00 120.00  122
 23  \w   -118.00 -93.00   0.50   25.00    -- -106.00 -30.00 150.00   50
 24  \w   -153.00-105.00   0.50   25.00    -- -106.00 -30.00 120.00   96
 25  \w   -175.00-134.00   0.50   25.00    -- -106.00 -30.00 150.00   82
 26  \w   -163.00 -97.00   0.50   25.00    -- -106.00 -45.00 -60.00  132
 27  \w   -129.00 -93.00   0.50   25.00    -- -106.00 -49.00-146.00   72
 28  \w    -70.00 -35.00   0.50   25.00    -- -106.00  61.00-180.00   70
 29  \w    -69.00 -33.00   0.50   25.00    -- -106.00  61.00-150.00   72
 30  \w   -104.00 -38.00   0.50   25.00    -- -106.00  77.00-150.00  132
 31  \w   -104.00 -33.00   0.50   25.00    -- -106.00  77.00 -90.00  142
;
_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      -0.1853948000
_diffrn_orient_matrix_UB_12      -0.0095443000
_diffrn_orient_matrix_UB_13      -0.0044303000
_diffrn_orient_matrix_UB_21      -0.0071252000
_diffrn_orient_matrix_UB_22      0.0286697000
_diffrn_orient_matrix_UB_23      0.0668359000
_diffrn_orient_matrix_UB_31      -0.0396157000
_diffrn_orient_matrix_UB_32      0.0396330000
_diffrn_orient_matrix_UB_33      -0.0492950000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40403
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.498
_diffrn_reflns_theta_max         67.498
_diffrn_reflns_theta_min         2.780
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.325
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80945
_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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       prism
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         8447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0646P)^2^+0.9512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7556
_reflns_number_total             8447
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00252c2.cif
_cod_data_source_block           2ver0-16023_kmv-262
_cod_database_code               7710041
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C46 H47 N9 S2 Pd2'
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.528
_diffrn_oxdiff_digest_frames
;
012777c2e1cce797455894cf10060f83bf000256a70
;
_diffrn_oxdiff_digest_hkl
;
01e44185ddc672eaca4cf2a2cc851dc26c46ac
;
_reflns_odcompleteness_completeness 99.14
_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:
 C3(H3), C28(H28), C21(H21), C5(H5), C19(H19), C30(H30), C12(H12), C4(H4),
 C10(H10), C40(H40), C38(H38)
2.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C14(H14A,H14B,H14C), C32(H32A,H32B,
 H32C), C15(H15A,H15B,H15C), C34(H34A,H34B,H34C), C43(H43A,H43B,H43C), C24(H24A,
 H24B,H24C), C16(H16A,H16B,H16C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C),
 C44(H44A,H44B,H44C)
;
_shelx_res_checksum              23098
_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 1.599
_oxdiff_exptl_absorpt_empirical_full_min 0.526