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_7716646
_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 Cl F6 N2 Ni'
_chemical_formula_sum            'C20 H11 Cl F6 N2 Ni'
_chemical_formula_weight         487.47
_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             2024-01-30
_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                 108.9317(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.34845(5)
_cell_length_b                   17.63964(7)
_cell_length_c                   10.81434(6)
_cell_measurement_reflns_used    27158
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      80.1450
_cell_measurement_theta_min      4.9690
_cell_volume                     1867.295(17)
_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      99.99(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    -33.00  76.00   0.50    0.10    --   41.38 -76.00 163.00  218
  2  \w     45.00 108.00   0.50    0.40    --  121.50-111.00 150.00  126
  3  \w     45.00 108.00   0.50    0.40    --  121.50-111.00   0.00  126
  4  \w     45.00 108.00   0.50    0.40    --  121.50-111.00 -60.00  126
  5  \w     45.00 108.00   0.50    0.40    --  121.50-111.00-150.00  126
  6  \w    -43.00  27.00   0.50    0.10    --   41.38 -19.00-180.00  140
  7  \w    -43.00  27.00   0.50    0.10    --   41.38 -19.00   0.00  140
  8  \w     45.00 108.00   0.50    0.40    --  121.50-111.00 120.00  126
  9  \w     45.00 108.00   0.50    0.40    --  121.50-111.00  90.00  126
 10  \w     41.00 106.00   0.50    0.40    --  121.50 -95.00  90.00  130
 11  \w     41.00 106.00   0.50    0.40    --  121.50 -95.00 120.00  130
 12  \w     41.00 106.00   0.50    0.40    --  121.50 -95.00 150.00  130
 13  \w     41.00 106.00   0.50    0.40    --  121.50 -95.00  60.00  130
 14  \w     45.00 108.00   0.50    0.40    --  121.50-111.00  30.00  126
 15  \w     41.00 106.00   0.50    0.40    --  121.50 -95.00   0.00  130
 16  \w     45.00 158.00   0.50    0.40    --  121.50 -82.00 -62.88  226
 17  \w     41.00 106.00   0.50    0.40    --  121.50 -95.00-120.00  130
 18  \w     43.00 160.00   0.50    0.40    --  121.50 -86.00  64.10  234
 19  \w     43.00 160.00   0.50    0.40    --  121.50 -86.00  64.10  234
 20  \w     41.00 106.00   0.50    0.40    --  121.50 -95.00 150.00  130
 21  \w     47.00 101.00   0.50    0.40    --  121.50 -76.00 163.00  108
 22  \w     47.00 105.00   0.50    0.40    --  121.50 -77.00 120.00  116
 23  \w     47.00 105.00   0.50    0.40    --  121.50 -77.00  90.00  116
 24  \w     46.00 158.00   0.50    0.40    --  121.50 -80.00 107.97  224
 25  \w     47.00 105.00   0.50    0.40    --  121.50 -77.00   0.00  116
 26  \w     47.00 105.00   0.50    0.40    --  121.50 -77.00-120.00  116
 27  \w     84.00 178.00   0.50    0.40    --  121.50  30.00 -30.00  188
 28  \w     87.00 178.00   0.50    0.40    --  121.50  77.00  30.00  182
 29  \w     92.00 178.00   0.50    0.40    --  121.50  61.00   0.00  172
 30  \w     87.00 178.00   0.50    0.40    --  121.50  77.00 -60.00  182
 31  \w     87.00 178.00   0.50    0.40    --  121.50  76.00 -69.00  182
 32  \w     92.00 178.00   0.50    0.40    --  121.50  61.00 -60.00  172
 33  \w     92.00 178.00   0.50    0.40    --  121.50  61.00-120.00  172
 34  \w     92.00 178.00   0.50    0.40    --  121.50  45.00 -90.00  172
 35  \w     87.00 178.00   0.50    0.40    --  121.50  77.00-150.00  182
 36  \w     14.00 117.00   0.50    0.10    --   41.38  57.00 -60.00  206
 37  \w     14.00  98.00   0.50    0.10    --   41.38  57.00  60.00  168
 38  \w      0.00  41.00   0.50    0.10    --   41.38  92.00  28.49   82
 39  \w     -3.00  23.00   0.50    0.10    --   41.38  99.00 139.45   52
 40  \w    103.00 178.00   0.50    0.40    --  121.50 111.00  90.00  150
 41  \w     63.00 146.00   0.50    0.40    --  121.50 178.00 -30.00  166
 42  \w     63.00 146.00   0.50    0.40    --  121.50 178.00 -60.00  166
 43  \w    103.00 178.00   0.50    0.40    --  121.50 111.00-180.00  150
 44  \w   -117.00  -7.00   0.50    0.10    --  -41.38 -76.00 163.00  220
 45  \w   -175.00 -66.00   0.50    0.40    -- -100.00 -76.00 163.00  218
 46  \w   -101.00 -24.00   0.50    0.40    -- -100.00  76.00 -69.00  154
 47  \w    -82.00 -23.00   0.50    0.40    -- -100.00 111.00   0.00  118
 48  \w    -75.00  34.00   0.50    0.10    --  -41.38  76.00 -69.00  218
 49  \w    -51.00 -21.00   0.50    0.40    -- -100.00  45.00  60.00   60
 50  \w    -51.00 -21.00   0.50    0.40    -- -100.00  45.00 150.00   60
;
_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      0.1250852000
_diffrn_orient_matrix_UB_12      0.0495282000
_diffrn_orient_matrix_UB_13      0.0695961000
_diffrn_orient_matrix_UB_21      -0.0354034000
_diffrn_orient_matrix_UB_22      0.0529044000
_diffrn_orient_matrix_UB_23      -0.1196851000
_diffrn_orient_matrix_UB_31      -0.0887941000
_diffrn_orient_matrix_UB_32      0.0487236000
_diffrn_orient_matrix_UB_33      0.0591788000
_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  0.0205
_diffrn_reflns_av_unetI/netI     0.0111
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            33931
_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         80.164
_diffrn_reflns_theta_min         4.998
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.457
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.253
_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    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.193
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.00144(9)
_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   1.098
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0263P)^2^+1.1473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0623
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4059
_reflns_number_total             4083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01304b2.cif
_cod_data_source_block           4g
_cod_depositor_comments
'Adding full bibliography for 7716642--7716648.cif.'
_cod_original_cell_volume        1867.293(15)
_cod_database_code               7716646
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H11 Cl F6 N2 Ni'
_chemical_oxdiff_usercomment     TAR-86_red_block
_shelx_estimated_absorpt_t_max   0.555
_shelx_estimated_absorpt_t_min   0.461
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
;
_shelx_res_checksum              37656
_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 1.575
_oxdiff_exptl_absorpt_empirical_full_min 0.837