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_7716644
_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 H13 Cl F4 N2 Ni'
_chemical_formula_sum            'C20 H13 Cl F4 N2 Ni'
_chemical_formula_weight         451.48
_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   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-03-06
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-03-06 deposited with the CCDC.	2024-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.8036(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.95480(7)
_cell_length_b                   17.60556(13)
_cell_length_c                   13.33453(10)
_cell_measurement_reflns_used    22210
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.7440
_cell_measurement_theta_min      2.5100
_cell_volume                     1787.74(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.104a 64-bit (release 22-12-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(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 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     21.00 119.00   0.50    0.50    --   42.78  45.00-137.00  196
  2  \w     21.00 119.00   0.50    0.50    --   42.78  45.00-137.00  196
  3  \w    -80.00 -22.00   0.50    1.80    --  -96.00  99.00 -39.00  116
  4  \w    -51.00 -20.00   0.50    1.80    --  -96.00  45.00-137.00   62
  5  \w     44.00 106.00   0.50    1.80    --  117.50 -99.00-145.00  124
  6  \w     95.00 178.00   0.50    1.80    --  117.50  45.00-137.00  166
  7  \w    101.00 178.00   0.50    1.80    --  117.50  86.00  66.00  154
  8  \w    -76.00  31.00   0.50    0.50    --  -42.78  86.00  66.00  214
  9  \w    -37.00  27.00   0.50    0.50    --   42.78 -19.00 -60.00  128
 10  \w    -51.00 -20.00   0.50    1.80    --  -96.00  45.00  60.00   62
 11  \w     46.00 111.00   0.50    1.80    --  117.50-125.00 -60.00  130
 12  \w     44.00  71.00   0.50    1.80    --  117.50 -61.00  30.00   54
 13  \w     95.00 178.00   0.50    1.80    --  117.50 125.00  90.00  166
 14  \w     89.00 178.00   0.50    1.80    --  117.50  77.00 -60.00  178
 15  \w      0.00  37.00   0.50    0.50    --   42.81 -85.00 -52.00   74
 16  \w      2.00  28.00   0.50    0.50    --  -42.81  19.00  30.00   52
 17  \w    -86.00 -48.00   0.50    0.50    --  -42.81 -77.00 -90.00   76
 18  \w   -114.00 -87.00   0.50    0.50    --  -42.81 -77.00 -90.00   54
 19  \w    -29.00  27.00   0.50    0.50    --   42.81 -19.00  60.00  112
 20  \w     65.00  91.00   0.50    0.50    --   42.81-125.00-150.00   52
 21  \w     36.00  62.00   0.50    0.50    --   42.81-125.00-150.00   52
 22  \w     40.00  89.00   0.50    0.50    --   42.81-125.00 150.00   98
 23  \w    -49.00 -21.00   0.50    1.80    --  -96.00  45.00  30.00   56
 24  \w    -51.00 -22.00   0.50    1.80    --  -96.00  45.00 -90.00   58
 25  \w     45.00  70.00   0.50    1.80    --  117.50 -61.00-150.00   50
 26  \w     76.00 111.00   0.50    1.80    --  117.50-125.00-150.00   70
 27  \w     46.00  77.00   0.50    1.80    --  117.50 -77.00 120.00   62
 28  \w     51.00  78.00   0.50    1.80    --  117.50 -77.00 150.00   54
 29  \w     96.00 139.00   0.50    1.80    --  117.50  30.00  60.00   86
 30  \w     49.00  74.00   0.50    1.80    --  117.50-125.00-150.00   50
 31  \w    109.00 135.00   0.50    1.80    --  117.50  30.00  30.00   52
 32  \w    107.00 155.00   0.50    1.80    --  117.50  77.00  90.00   96
 33  \w    107.00 168.00   0.50    1.80    --  117.50  77.00 -30.00  122
 34  \w     77.00 111.00   0.50    1.80    --  117.50-125.00  60.00   68
 35  \w     73.00 111.00   0.50    1.80    --  117.50-125.00  30.00   76
 36  \w     60.00  90.00   0.50    1.80    --  117.50 -82.00  40.45   60
 37  \w     84.00 110.00   0.50    1.80    --  117.50-125.00 -30.00   52
 38  \w     93.00 118.00   0.50    1.80    --  117.50 -87.00-105.83   50
 39  \w    132.00 168.00   0.50    1.80    --  117.50 125.00  30.00   72
 40  \w     77.00 111.00   0.50    1.80    --  117.50-125.00-120.00   68
 41  \w     50.00 101.00   0.50    1.80    --  117.50 -77.00  60.00  102
 42  \w     69.00  95.00   0.50    1.80    --  117.50 -85.00 -52.00   52
 43  \w     45.00  71.00   0.50    1.80    --  117.50 -61.00 -30.00   52
 44  \w    108.00 133.00   0.50    1.80    --  117.50  30.00 150.00   50
 45  \w   -167.00-141.00   0.50    1.80    --  -96.00 -85.00 -52.00   52
 46  \w     44.00  69.00   0.50    1.80    --  117.50 -61.00  90.00   50
 47  \w     47.00  94.00   0.50    1.80    --  117.50 -95.00 150.00   94
 48  \w     53.00  79.00   0.50    1.80    --  117.50 -77.00 -90.00   52
 49  \w    118.00 149.00   0.50    1.80    --  117.50  61.00  90.00   62
 50  \w    136.00 178.00   0.50    1.80    --  117.50  45.00 150.00   84
 51  \w     56.00  95.00   0.50    1.80    --  117.50 -95.00   0.00   78
 52  \w     83.00 109.00   0.50    1.80    --  117.50 -78.00 -52.45   52
 53  \w    116.00 155.00   0.50    1.80    --  117.50 125.00 -60.00   78
 54  \w    131.00 157.00   0.50    1.80    --  117.50  77.00   0.00   52
 55  \w     68.00  97.00   0.50    1.80    --  117.50 -77.00  90.00   58
 56  \w     61.00 105.00   0.50    1.80    --  117.50 -85.00   3.73   88
 57  \w     44.00  69.00   0.50    1.80    --  117.50 -61.00   0.00   50
 58  \w   -116.00 -20.00   0.50    0.50    --  -42.81 -57.00 -30.00  192
 59  \w   -116.00 -20.00   0.50    0.50    --  -42.81 -57.00  60.00  192
 60  \w    -37.00  27.00   0.50    0.50    --   42.81 -19.00-180.00  128
 61  \w     14.00 117.00   0.50    0.50    --   42.81  77.00 -90.00  206
 62  \w     14.00 117.00   0.50    0.50    --   42.81  77.00  90.00  206
 63  \w     14.00  78.00   0.50    0.50    --   42.81  77.00-180.00  128
 64  \w      9.00  43.00   0.50    0.50    --   42.81  89.00  14.22   68
;
_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      -0.0377883000
_diffrn_orient_matrix_UB_12      -0.0770443000
_diffrn_orient_matrix_UB_13      -0.0569079000
_diffrn_orient_matrix_UB_21      -0.1646554000
_diffrn_orient_matrix_UB_22      -0.0096375000
_diffrn_orient_matrix_UB_23      0.0374890000
_diffrn_orient_matrix_UB_31      -0.1113276000
_diffrn_orient_matrix_UB_32      0.0403415000
_diffrn_orient_matrix_UB_33      -0.0996154000
_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  0.0183
_diffrn_reflns_av_unetI/netI     0.0096
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28249
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.980
_diffrn_reflns_theta_min         4.278
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.389
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.104a (Rigaku Oxford Diffraction, 2023)
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 intense red'
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0241
_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^)+(0.0315P)^2^+1.0770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0657
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3779
_reflns_number_total             3890
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01304b2.cif
_cod_data_source_block           4e
_cod_depositor_comments
'Adding full bibliography for 7716642--7716648.cif.'
_cod_database_code               7716644
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H13N2F4ClNi
_chemical_oxdiff_usercomment     TAR-87_tarabrin
_shelx_estimated_absorpt_t_max   0.773
_shelx_estimated_absorpt_t_min   0.687
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
;
_shelx_res_checksum              95494
_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 1.156
_oxdiff_exptl_absorpt_empirical_full_min 0.943