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_7716643
_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 H15 Cl F2 N2 Ni'
_chemical_formula_sum            'C20 H15 Cl F2 N2 Ni'
_chemical_formula_weight         415.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-04-13
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-04-13 deposited with the CCDC.	2024-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.3896(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.82250(6)
_cell_length_b                   7.90636(4)
_cell_length_c                   20.14341(12)
_cell_measurement_reflns_used    22372
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.5740
_cell_measurement_theta_min      2.1920
_cell_volume                     1715.983(17)
_computing_cell_refinement       'CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.117a 64-bit (release 26-03-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.117a (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(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     44.00 105.00   0.50    0.32    --  117.50 -77.00  90.00  122
  2  \w     44.00 105.00   0.50    0.32    --  117.50 -77.00 120.00  122
  3  \w     44.00 105.00   0.50    0.32    --  117.50 -77.00   0.00  122
  4  \w     44.00 105.00   0.50    0.32    --  117.50 -77.00  30.00  122
  5  \w     44.00  71.00   0.50    0.32    --  117.50 -61.00   0.00   54
  6  \w     44.00 105.00   0.50    0.32    --  117.50 -77.00 -60.00  122
  7  \w     44.00 105.00   0.50    0.32    --  117.50 -77.00-120.00  122
  8  \w     44.00 105.00   0.50    0.32    --  117.50 -77.00-180.00  122
  9  \w     44.00  69.00   0.50    0.32    --  117.50 -61.00-180.00   50
 10  \w    -34.00  43.00   0.50    0.09    --   42.78 -38.00-150.00  154
 11  \w     34.00  95.00   0.50    0.09    --   42.78-125.00-180.00  122
 12  \w     46.00 111.00   0.50    0.32    --  117.50-125.00 -30.00  130
 13  \w     49.00 104.00   0.50    0.32    --  117.50 -95.00   0.00  110
 14  \w     48.00  74.00   0.50    0.32    --  117.50 -95.00-120.00   52
 15  \w     44.00 105.00   0.50    0.32    --  117.50 -95.00-180.00  122
 16  \w     44.00 105.00   0.50    0.32    --  117.50 -95.00-150.00  122
 17  \w    115.00 151.00   0.50    0.32    --  117.50 -86.00 -98.77   72
 18  \w     44.00 149.00   0.50    0.32    --  117.50 -83.00 -42.45  210
 19  \w     44.00 149.00   0.50    0.32    --  117.50 -83.00 -42.45  210
 20  \w    121.00 147.00   0.50    0.32    --  117.50 -88.00  83.46   52
 21  \w     49.00 115.00   0.50    0.32    --  117.50 -88.00  83.46  132
 22  \w     44.00 150.00   0.50    0.32    --  117.50 -85.00 102.24  212
 23  \w     67.00 177.00   0.50    0.32    --  117.50  15.00 120.00  220
 24  \w     89.00 178.00   0.50    0.32    --  117.50  77.00 150.00  178
 25  \w     95.00 178.00   0.50    0.32    --  117.50  45.00 150.00  166
 26  \w     94.00 178.00   0.50    0.32    --  117.50  30.00 150.00  168
 27  \w    113.00 138.00   0.50    0.32    --  117.50  61.00  60.00   50
 28  \w    141.00 170.00   0.50    0.32    --  117.50  61.00  60.00   58
 29  \w     94.00 178.00   0.50    0.32    --  117.50  30.00  30.00  168
 30  \w     94.00 178.00   0.50    0.32    --  117.50  30.00  30.00  168
 31  \w      6.00 124.00   0.50    0.09    --   42.78  18.00 128.00  236
 32  \w     81.00 178.00   0.50    0.32    --  117.50  18.00 128.00  194
 33  \w     81.00 178.00   0.50    0.32    --  117.50  18.00 128.00  194
 34  \w    115.00 151.00   0.50    0.32    --  117.50  30.00 -90.00   72
 35  \w    118.00 144.00   0.50    0.32    --  117.50  45.00-180.00   52
 36  \w    130.00 156.00   0.50    0.32    --  117.50 125.00 -60.00   52
 37  \w     95.00 178.00   0.50    0.32    --  117.50 125.00   0.00  166
 38  \w     95.00 178.00   0.50    0.32    --  117.50 125.00   0.00  166
 39  \w   -123.00  -9.00   0.50    0.09    --  -42.78 -18.00 -39.00  228
 40  \w   -177.00 -62.00   0.50    0.32    --  -96.00 -18.00 -39.00  230
 41  \w    -71.00 -22.00   0.50    0.32    --  -96.00  61.00 -90.00   98
 42  \w    -27.00  38.00   0.50    0.09    --  -42.78  19.00-180.00  130
 43  \w    -51.00 -20.00   0.50    0.32    --  -96.00  45.00 -30.00   62
 44  \w    -26.00  38.00   0.50    0.09    --  -42.78  18.00 128.00  128
;
_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      -0.1394813000
_diffrn_orient_matrix_UB_12      -0.0332961000
_diffrn_orient_matrix_UB_13      -0.0174970000
_diffrn_orient_matrix_UB_21      -0.0154353000
_diffrn_orient_matrix_UB_22      -0.0328231000
_diffrn_orient_matrix_UB_23      0.0741444000
_diffrn_orient_matrix_UB_31      -0.0272689000
_diffrn_orient_matrix_UB_32      0.1892272000
_diffrn_orient_matrix_UB_33      0.0097651000
_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  0.0225
_diffrn_reflns_av_unetI/netI     0.0123
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27642
_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         80.065
_diffrn_reflns_theta_min         4.103
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.298
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.223
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.117a (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            red
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         3728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0257P)^2^+1.5319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3699
_reflns_number_total             3728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01304b2.cif
_cod_data_source_block           4b
_cod_depositor_comments
'Adding full bibliography for 7716642--7716648.cif.'
_cod_original_cell_volume        1715.982(17)
_cod_database_code               7716643
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ni Cl F2 N2 C20 H15'
_chemical_oxdiff_usercomment     TAR-96
_shelx_estimated_absorpt_t_max   0.558
_shelx_estimated_absorpt_t_min   0.391
_olex2_refinement_description
;
;
_shelx_res_checksum              15784
_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 1.176
_oxdiff_exptl_absorpt_empirical_full_min 0.901