Synthesis and comparative study of (NHC<sub>F</sub>)PdCl<sub>2</sub>Py and (NHC<sub>F</sub>)Ni(Cp)Cl complexes: investigation of the electronic properties of NHC ligands and complex characteristics.
Pankov, Roman O.; Tarabrin, Ignatii R.; Son, Alexandra G.; Minyaev, Mikhail E.; Prima, Darya O.; Ananikov, Valentine P.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12503–12518; doi:10.1039/d4dt01304b

data_7716647
_publ_section_title
;
 Synthesis and comparative study of (NHC<sub>F</sub>)PdCl<sub>2</sub>Py
 and (NHC<sub>F</sub>)Ni(Cp)Cl complexes: investigation of the electronic
 properties of NHC ligands and complex characteristics.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12503
_journal_page_last               12518
_journal_paper_doi               10.1039/d4dt01304b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C20 H11 F4 N3 O2 Pd'
_chemical_formula_sum            'C20 H11 F4 N3 O2 Pd'
_chemical_formula_weight         507.72
_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   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-06-13
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2024-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                88.7087(14)
_cell_angle_beta                 84.9983(14)
_cell_angle_gamma                82.4843(17)
_cell_formula_units_Z            2
_cell_length_a                   3.68882(7)
_cell_length_b                   11.4296(2)
_cell_length_c                   20.0470(3)
_cell_measurement_reflns_used    7596
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      79.2340
_cell_measurement_theta_min      2.1860
_cell_volume                     834.71(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.124a 64-bit (release 23-05-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL  (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.953
_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    -51.00  -6.00   0.50    3.00    --  -46.47  64.00  73.00   90
  2  \w    -78.00 -44.00   0.50    3.00    --  -46.47 -64.00 -63.00   68
  3  \w     68.00 102.00   0.50    3.00    --   46.47  64.00  73.00   68
  4  \w     20.00  45.00   0.50    3.00    --   46.47 -64.00 -63.00   50
  5  \w   -144.00-118.00   0.50   12.00    --  -91.75 -64.00 -63.00   52
  6  \w    -72.00 -47.00   0.50   12.00    --  -91.75  64.00  73.00   50
  7  \w     98.00 140.00   0.50   12.00    --  113.25  64.00  73.00   84
  8  \w     41.00  66.00   0.50   12.00    --  113.25 -64.00 -63.00   50
  9  \w     -7.00  28.00   0.50    3.00    --  -46.47  19.00-150.00   70
 10  \w    -54.00 -15.00   0.50    3.00    --  -46.47 125.00-180.00   78
 11  \w    -26.00  28.00   0.50    3.00    --  -46.47  19.00 -60.00  108
 12  \w    -25.00  28.00   0.50    3.00    --  -46.47  19.00-180.00  106
 13  \w    -72.00 -32.00   0.50    3.00    --  -46.47 -38.00-180.00   80
 14  \w     34.00 120.00   0.50    3.00    --   46.47  38.00-150.00  172
 15  \w     39.00  87.00   0.50    3.00    --   46.47-125.00 150.00   96
 16  \w   -137.00 -73.00   0.50   12.00    --  -91.75 -65.00 165.82  128
 17  \w    -93.00 -68.00   0.50   12.00    --  -91.75 -77.00-150.00   50
 18  \w     44.00  70.00   0.50   12.00    --  113.25 -61.00-150.00   52
 19  \w    140.00 177.00   0.50   12.00    --  113.25  61.00 120.00   74
 20  \w     76.00 102.00   0.50   12.00    --  113.25 -81.00 109.81   52
 21  \w     94.00 123.00   0.50   12.00    --  113.25  77.00 150.00   58
 22  \w    139.00 172.00   0.50   12.00    --  113.25  77.00 150.00   66
 23  \w     43.00  69.00   0.50   12.00    --  113.25 -77.00 120.00   52
 24  \w     99.00 151.00   0.50   12.00    --  113.25  30.00  30.00  104
 25  \w    103.00 129.00   0.50   12.00    --  113.25 -88.00 114.58   52
 26  \w     90.00 115.00   0.50   12.00    --  113.25  77.00-150.00   50
 27  \w     85.00 126.00   0.50   12.00    --  113.25 -88.00-136.75   82
 28  \w     66.00  92.00   0.50   12.00    --  113.25 -88.00 114.58   52
 29  \w    132.00 165.00   0.50   12.00    --  113.25  77.00-150.00   66
 30  \w    152.00 177.00   0.50   12.00    --  113.25  30.00-150.00   50
 31  \w    105.00 139.00   0.50   12.00    --  113.25 -81.00 109.81   68
 32  \w     71.00 102.00   0.50   12.00    --  113.25 -77.00 120.00   62
 33  \w     42.00  98.00   0.50   12.00    --  113.25 -95.00  30.00  112
 34  \w    122.00 148.00   0.50   12.00    --  113.25  45.00-150.00   52
 35  \w     96.00 178.00   0.50   12.00    --  113.25  15.00   0.00  164
 36  \w    103.00 129.00   0.50   12.00    --  113.25 125.00 150.00   52
 37  \w    101.00 127.00   0.50   12.00    --  113.25  30.00  90.00   52
 38  \w    129.00 155.00   0.50   12.00    --  113.25 125.00 120.00   52
 39  \w     41.00  69.00   0.50   12.00    --  113.25 -61.00 150.00   56
 40  \w    150.00 176.00   0.50   12.00    --  113.25  77.00  30.00   52
 41  \w     90.00 145.00   0.50   12.00    --  113.25  77.00-180.00  110
 42  \w     43.00  98.00   0.50   12.00    --  113.25 -77.00  30.00  110
 43  \w    111.00 137.00   0.50   12.00    --  113.25  61.00-180.00   52
 44  \w     75.00 100.00   0.50   12.00    --  113.25 -77.00 -90.00   50
 45  \w    149.00 177.00   0.50   12.00    --  113.25  77.00-180.00   56
 46  \w     43.00  69.00   0.50   12.00    --  113.25-125.00   0.00   52
 47  \w    153.00 178.00   0.50   12.00    --  113.25 125.00 -60.00   50
 48  \w     55.00  87.00   0.50   12.00    --  113.25 -77.00-150.00   64
 49  \w     45.00  83.00   0.50   12.00    --  113.25-125.00 150.00   76
 50  \w    134.00 177.00   0.50   12.00    --  113.25  45.00  60.00   86
 51  \w    108.00 133.00   0.50   12.00    --  113.25  30.00-180.00   50
 52  \w    110.00 135.00   0.50   12.00    --  113.25  30.00-150.00   50
 53  \w     95.00 134.00   0.50   12.00    --  113.25 125.00 -60.00   78
 54  \w     42.00  69.00   0.50   12.00    --  113.25 -61.00 -60.00   54
 55  \w    130.00 163.00   0.50   12.00    --  113.25  15.00 -30.00   66
 56  \w     45.00 113.00   0.50   12.00    --  113.25 -88.00 -14.30  136
 57  \w     42.00  76.00   0.50   12.00    --  113.25 -77.00 -60.00   68
 58  \w     62.00 105.00   0.50   12.00    --  113.25 -77.00  60.00   86
 59  \w     96.00 138.00   0.50   12.00    --  113.25  61.00-150.00   84
 60  \w     41.00  69.00   0.50   12.00    --  113.25 -61.00 -30.00   56
 61  \w    153.00 178.00   0.50   12.00    --  113.25  15.00-180.00   50
 62  \w    123.00 178.00   0.50   12.00    --  113.25  45.00 -90.00  110
 63  \w     99.00 132.00   0.50   12.00    --  113.25  45.00 -60.00   66
 64  \w    149.00 175.00   0.50   12.00    --  113.25  45.00 -60.00   52
 65  \w    102.00 127.00   0.50   12.00    --  113.25  45.00 120.00   50
 66  \w    134.00 160.00   0.50   12.00    --  113.25  45.00 120.00   52
 67  \w    101.00 142.00   0.50   12.00    --  113.25  30.00 -90.00   82
 68  \w    151.00 178.00   0.50   12.00    --  113.25  30.00 150.00   54
 69  \w    121.00 147.00   0.50   12.00    --  113.25  61.00  30.00   52
 70  \w     91.00 122.00   0.50   12.00    --  113.25  77.00-120.00   62
 71  \w     97.00 137.00   0.50   12.00    --  113.25  15.00-180.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.3093445000
_diffrn_orient_matrix_UB_12      -0.0006216000
_diffrn_orient_matrix_UB_13      0.0567851000
_diffrn_orient_matrix_UB_21      -0.0260999000
_diffrn_orient_matrix_UB_22      0.1352095000
_diffrn_orient_matrix_UB_23      0.0048789000
_diffrn_orient_matrix_UB_31      -0.2869961000
_diffrn_orient_matrix_UB_32      0.0142829000
_diffrn_orient_matrix_UB_33      -0.0519920000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12853
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.654
_diffrn_reflns_theta_min         2.212
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.614
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.551
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.125a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_diffrn    2.020
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.022
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         3473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0312
_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^)+3.8844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3248
_reflns_number_total             3473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01304b2.cif
_cod_data_source_block           DPR553
_cod_depositor_comments
'Adding full bibliography for 7716642--7716648.cif.'
_cod_database_code               7716647
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H11F4N3O2Pd
_chemical_oxdiff_usercomment     PDO-553-Pd
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.513
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
;
_shelx_res_checksum              49367
_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 1.262
_oxdiff_exptl_absorpt_empirical_full_min 0.921