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_7716645
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-10-10
_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                 92.6788(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.87858(6)
_cell_length_b                   10.65567(5)
_cell_length_c                   15.41970(8)
_cell_measurement_reflns_used    19140
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.9420
_cell_measurement_theta_min      2.8580
_cell_volume                     1785.476(16)
_computing_cell_refinement       'CrysAlisPro 1.171.43.91a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.102a 64-bit (release 15-09-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.91a (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 0.998
_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    -45.00  39.00   0.50    0.21    --  -41.38  40.00  22.00  168
  2  \w    -71.00 -24.00   0.50    0.21    -- -100.00  61.00 -30.00   94
  3  \w    -51.00 -21.00   0.50    0.21    -- -100.00  45.00-120.00   60
  4  \w    -45.00 -19.00   0.50    0.21    -- -100.00  40.00  22.00   52
  5  \w    -71.00 -24.00   0.50    0.21    -- -100.00  61.00-120.00   94
  6  \w    -51.00 -21.00   0.50    0.21    -- -100.00  45.00-150.00   60
  7  \w     34.00  99.00   0.50    0.21    --   41.38-125.00-180.00  130
  8  \w     45.00 108.00   0.50    0.21    --  121.50-111.00-180.00  126
  9  \w     45.00 108.00   0.50    0.21    --  121.50-111.00-150.00  126
 10  \w     45.00 108.00   0.50    0.21    --  121.50-111.00 -90.00  126
 11  \w     45.00 108.00   0.50    0.21    --  121.50-111.00 -30.00  126
 12  \w     79.00 104.00   0.50    0.21    --  121.50 -95.00 -90.00   50
 13  \w     41.00 106.00   0.50    0.21    --  121.50 -95.00 -30.00  130
 14  \w     43.00 160.00   0.50    0.21    --  121.50 -86.00 120.91  234
 15  \w     45.00 108.00   0.50    0.21    --  121.50-111.00  90.00  126
 16  \w     41.00 106.00   0.50    0.21    --  121.50 -94.00  67.58  130
 17  \w     45.00 108.00   0.50    0.21    --  121.50-111.00  30.00  126
 18  \w     34.00  99.00   0.50    0.21    --   41.38-125.00  60.00  130
 19  \w    -39.00  45.00   0.50    0.21    --   41.38 -40.00-131.00  168
 20  \w     47.00 105.00   0.50    0.21    --  121.50 -77.00-180.00  116
 21  \w     47.00 105.00   0.50    0.21    --  121.50 -77.00 -90.00  116
 22  \w     47.00 105.00   0.50    0.21    --  121.50 -77.00   0.00  116
 23  \w     47.00 105.00   0.50    0.21    --  121.50 -77.00  60.00  116
 24  \w     47.00 105.00   0.50    0.21    --  121.50 -77.00 120.00  116
 25  \w     47.00 105.00   0.50    0.21    --  121.50 -77.00 150.00  116
 26  \w      1.00  42.00   0.50    0.21    --   41.38  91.00 127.66   82
 27  \w    103.00 178.00   0.50    0.21    --  121.50 111.00 150.00  150
 28  \w     71.00  97.00   0.50    0.21    --  121.50 178.00 150.00   52
 29  \w    103.00 178.00   0.50    0.21    --  121.50 111.00  60.00  150
 30  \w    116.00 142.00   0.50    0.21    --  121.50 111.00 -30.00   52
 31  \w    105.00 130.00   0.50    0.21    --  121.50 178.00-150.00   50
 32  \w    103.00 178.00   0.50    0.21    --  121.50 111.00-120.00  150
 33  \w     42.00 178.00   0.50    0.21    --  121.50  15.00-150.00  272
 34  \w     93.00 147.00   0.50    0.21    --  121.50  45.00-180.00  108
 35  \w     92.00 178.00   0.50    0.21    --  121.50  61.00-120.00  172
 36  \w     91.00 178.00   0.50    0.21    --  121.50  40.00  22.00  174
 37  \w     87.00 178.00   0.50    0.21    --  121.50  77.00  30.00  182
 38  \w     87.00 178.00   0.50    0.21    --  121.50  77.00  60.00  182
 39  \w     87.00 178.00   0.50    0.21    --  121.50  77.00 120.00  182
 40  \w    112.00 155.00   0.50    0.21    --  121.50  30.00   0.00   86
 41  \w     11.00 122.00   0.50    0.21    --   41.38  40.00  22.00  222
 42  \w   -122.00 -11.00   0.50    0.21    --  -41.38 -40.00-131.00  222
 43  \w   -177.00 -69.00   0.50    0.21    -- -100.00 -40.00-131.00  216
;
_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      0.1080245000
_diffrn_orient_matrix_UB_12      -0.0423228000
_diffrn_orient_matrix_UB_13      -0.0541449000
_diffrn_orient_matrix_UB_21      -0.0632181000
_diffrn_orient_matrix_UB_22      0.0591664000
_diffrn_orient_matrix_UB_23      -0.0815929000
_diffrn_orient_matrix_UB_31      0.0665744000
_diffrn_orient_matrix_UB_32      0.1249584000
_diffrn_orient_matrix_UB_33      0.0203171000
_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  0.0216
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24172
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.226
_diffrn_reflns_theta_min         4.068
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.393
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.328
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.91a (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    1.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.00057(8)
_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   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         3896
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0259P)^2^+1.4482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3876
_reflns_number_total             3896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01304b2.cif
_cod_data_source_block           4d
_cod_depositor_comments
'Adding full bibliography for 7716642--7716648.cif.'
_cod_database_code               7716645
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H13N2F4ClNi
_chemical_oxdiff_usercomment     TAR-70
_shelx_estimated_absorpt_t_max   0.509
_shelx_estimated_absorpt_t_min   0.252
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C6-F6 \\sim C8-F8A \\sim C12-F12 \\sim C14-F14A
 with sigma of 0.02
 C7-F8A \\sim C9-F8A
 with sigma of 0.02
3. Restrained planarity
 C4, C5, C6, F6, C7, F7, C8, F8A, C9
 with sigma of 0.1
 C10, C11, C12, F12, C13, F13, C14, F14A, C15
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(F6) = Uanis(F8A)
Uanis(F12) = Uanis(F14A)
5. Others
 Sof(H6A)=Sof(F8A)=1-FVAR(1)
 Sof(F6)=Sof(H8)=FVAR(1)
 Sof(H12A)=Sof(F14A)=1-FVAR(2)
 Sof(F12)=Sof(H14)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C6(H6A), C8(H8), C12(H12A), C14(H14)
;
_shelx_res_checksum              82227
_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 1.160
_oxdiff_exptl_absorpt_empirical_full_min 0.849