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_7716642
_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 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             2024-01-24
_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                 100.8923(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.99026(4)
_cell_length_b                   19.21028(11)
_cell_length_c                   11.91822(6)
_cell_measurement_reflns_used    18527
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      80.1490
_cell_measurement_theta_min      3.7960
_cell_volume                     1796.431(17)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.92a 64-bit (release 05-10-2023))'
_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 0.999
_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     -1.00  68.00   0.50    0.05    --   15.16 -99.00-180.00  138
  2  \w     -1.00  68.00   0.50    0.05    --   15.16 -99.00-120.00  138
  3  \w    -21.00  61.00   0.50    0.05    --   15.16 -84.00 -25.00  164
  4  \w     34.00 112.00   0.50    0.20    --   71.20-125.00   0.00  156
  5  \w     43.00 108.00   0.50    0.25    --  127.25-111.00-180.00  130
  6  \w     37.00 105.00   0.50    0.25    --  127.25 -92.00-120.00  136
  7  \w     37.00 105.00   0.50    0.25    --  127.25 -92.00 -90.00  136
  8  \w     37.00 105.00   0.50    0.25    --  127.25 -92.00 -30.00  136
  9  \w     37.00 105.00   0.50    0.25    --  127.25 -92.00 -30.00  136
 10  \w     43.00 108.00   0.50    0.25    --  127.25-111.00  90.00  130
 11  \w     52.00  78.00   0.50    0.25    --  127.25 -92.00  30.00   52
 12  \w     38.00 174.00   0.50    0.25    --  127.25 -84.00 -25.00  272
 13  \w     38.00 174.00   0.50    0.25    --  127.25 -84.00 -25.00  272
 14  \w    -18.00 117.00   0.50    0.20    --   71.20 -84.00 -25.00  270
 15  \w     85.00 111.00   0.50    0.25    --  127.25 -80.00 102.37   52
 16  \w     41.00 105.00   0.50    0.25    --  127.25 -77.00 150.00  128
 17  \w     41.00 105.00   0.50    0.25    --  127.25 -77.00  90.00  128
 18  \w     49.00  76.00   0.50    0.25    --  127.25 -64.00  30.00   54
 19  \w     41.00 105.00   0.50    0.25    --  127.25 -77.00   0.00  128
 20  \w     -7.00  71.00   0.50    0.20    --   71.20 -61.00 150.00  156
 21  \w     49.00  76.00   0.50    0.25    --  127.25 -64.00   0.00   54
 22  \w     49.00  76.00   0.50    0.25    --  127.25 -64.00 -30.00   54
 23  \w     49.00  76.00   0.50    0.25    --  127.25 -64.00-120.00   54
 24  \w     49.00  75.00   0.50    0.25    --  127.25 -64.00-180.00   52
 25  \w    -17.00  35.00   0.50    0.20    --   71.20 -30.00 150.00  104
 26  \w     44.00 178.00   0.50    0.25    --  127.25  28.00  -3.64  268
 27  \w     90.00 178.00   0.50    0.25    --  127.25  64.00  90.00  176
 28  \w     84.00 178.00   0.50    0.25    --  127.25  77.00  60.00  188
 29  \w    104.00 130.00   0.50    0.25    --  127.25  50.00 150.00   52
 30  \w     90.00 178.00   0.50    0.25    --  127.25  64.00  30.00  176
 31  \w     90.00 178.00   0.50    0.25    --  127.25  64.00  30.00  176
 32  \w     90.00 177.00   0.50    0.25    --  127.25  64.00   0.00  174
 33  \w     77.00 178.00   0.50    0.25    --  127.25  38.00  30.00  202
 34  \w     44.00 178.00   0.50    0.25    --  127.25  28.00  -3.64  268
 35  \w     90.00 178.00   0.50    0.25    --  127.25  64.00-180.00  176
 36  \w     63.00 146.00   0.50    0.25    --  127.25 178.00 -30.00  166
 37  \w     63.00 146.00   0.50    0.25    --  127.25 178.00  90.00  166
 38  \w    103.00 178.00   0.50    0.25    --  127.25 111.00  60.00  150
 39  \w    102.00 153.00   0.50    0.20    --   71.20  84.00  94.00  102
 40  \w    101.00 178.00   0.50    0.25    --  127.25  84.00  94.00  154
 41  \w    128.00 169.00   0.50    0.25    --  127.25 111.00 -60.00   82
 42  \w     64.00 143.00   0.50    0.25    --  127.25 178.00-180.00  158
 43  \w    -25.00  11.00   0.50    0.20    --  -71.20  15.00-150.00   72
 44  \w   -110.00 -39.00   0.50    0.05    --  -15.16 178.00-180.00  142
 45  \w    -61.00  43.00   0.50    0.05    --  -15.16  84.00  94.00  208
 46  \w   -152.00 -23.00   0.50    0.25    -- -105.75  84.00  94.00  258
 47  \w    -82.00 -27.00   0.50    0.25    -- -105.75 111.00 150.00  110
 48  \w    -35.00  11.00   0.50    0.20    --  -71.20  30.00  60.00   92
 49  \w    -20.00  30.00   0.50    0.05    --  -15.16 -84.00 -25.00  100
 50  \w   -160.00 -79.00   0.50    0.20    --  -71.20 -84.00 -25.00  162
 51  \w   -177.00 -79.00   0.50    0.25    -- -105.75 -84.00 -25.00  196
;
_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      -0.1349592000
_diffrn_orient_matrix_UB_12      0.0582161000
_diffrn_orient_matrix_UB_13      -0.0141500000
_diffrn_orient_matrix_UB_21      0.0992038000
_diffrn_orient_matrix_UB_22      0.0401556000
_diffrn_orient_matrix_UB_23      -0.0782809000
_diffrn_orient_matrix_UB_31      -0.1024467000
_diffrn_orient_matrix_UB_32      -0.0378206000
_diffrn_orient_matrix_UB_33      -0.1048699000
_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  0.0221
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24230
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.377
_diffrn_reflns_theta_min         4.424
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.372
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.105
_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            red
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.559
_exptl_crystal_size_mid          0.440
_exptl_crystal_size_min          0.206
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.00311(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         3931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0253P)^2^+1.3841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3907
_reflns_number_total             3931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01304b2.cif
_cod_data_source_block           4c
_cod_depositor_comments
'Adding full bibliography for 7716642--7716648.cif.'
_cod_original_cell_volume        1796.430(17)
_cod_database_code               7716642
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H13 Cl F4 N2 Ni'
_chemical_oxdiff_usercomment     TAR-84p
_shelx_estimated_absorpt_t_max   0.543
_shelx_estimated_absorpt_t_min   0.254
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
;
_shelx_res_checksum              78877
_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 1.154
_oxdiff_exptl_absorpt_empirical_full_min 0.865