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_7716648
_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, 0.501(H2 O)'
_chemical_formula_sum            'C20 H16 Cl F2 N2 Ni O0.5'
_chemical_formula_weight         424.51
_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             2024-06-13
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2024-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.5562(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.53819(6)
_cell_length_b                   18.09252(12)
_cell_length_c                   12.13920(8)
_cell_measurement_reflns_used    17122
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      80.0190
_cell_measurement_theta_min      3.7890
_cell_volume                     1806.54(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.125a 64-bit (release 04-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.125a (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 0.999
_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    -32.00  76.00   0.50    0.05    --    0.00  72.00-127.00  216
  2  \w    -32.00  76.00   0.50    0.05    --    0.00  72.00-127.00  216
  3  \w      9.00 117.00   0.50    0.15    --   41.38  72.00-127.00  216
  4  \w     45.00 101.00   0.50    0.25    --  121.50-111.00-120.00  112
  5  \w     45.00 108.00   0.50    0.25    --  121.50-111.00 -60.00  126
  6  \w     46.00  72.00   0.50    0.25    --  121.50-111.00   0.00   52
  7  \w     41.00 106.00   0.50    0.25    --  121.50 -95.00 -30.00  130
  8  \w     41.00 106.00   0.50    0.25    --  121.50 -95.00   0.00  130
  9  \w     46.00  72.00   0.50    0.25    --  121.50 -82.00 -19.62   52
 10  \w     45.00 108.00   0.50    0.25    --  121.50-111.00  90.00  126
 11  \w     41.00 106.00   0.50    0.25    --  121.50 -95.00 150.00  130
 12  \w     46.00 157.00   0.50    0.25    --  121.50 -79.00  42.04  222
 13  \w     46.00 157.00   0.50    0.25    --  121.50 -79.00  42.04  222
 14  \w     47.00  74.00   0.50    0.25    --  121.50 -77.00  90.00   54
 15  \w     47.00 105.00   0.50    0.25    --  121.50 -77.00 150.00  116
 16  \w    123.00 156.00   0.50    0.25    --  121.50 -79.00  62.54   66
 17  \w     92.00 118.00   0.50    0.25    --  121.50 -79.00  62.54   52
 18  \w     76.00 102.00   0.50    0.25    --  121.50 -77.00   0.00   52
 19  \w     47.00  91.00   0.50    0.25    --  121.50 -72.00 103.00   88
 20  \w     59.00  90.00   0.50    0.25    --  121.50 -77.00 -60.00   62
 21  \w    -33.00  74.00   0.50    0.15    --   41.38 -72.00 103.00  214
 22  \w    -75.00  33.00   0.50    0.05    --    0.00 -72.00 103.00  216
 23  \w     47.00 105.00   0.50    0.25    --  121.50 -77.00 -90.00  116
 24  \w     60.00  86.00   0.50    0.25    --  121.50 -77.00-150.00   52
 25  \w     42.00 178.00   0.50    0.25    --  121.50  15.00-150.00  272
 26  \w     89.00 178.00   0.50    0.25    --  121.50  72.00-127.00  178
 27  \w     92.00 178.00   0.50    0.25    --  121.50  61.00 -60.00  172
 28  \w    100.00 127.00   0.50    0.25    --  121.50  45.00   0.00   54
 29  \w     92.00 178.00   0.50    0.25    --  121.50  45.00 -30.00  172
 30  \w     92.00 178.00   0.50    0.25    --  121.50  45.00 -30.00  172
 31  \w     92.00 171.00   0.50    0.25    --  121.50  45.00  90.00  158
 32  \w     84.00 178.00   0.50    0.25    --  121.50  30.00 150.00  188
 33  \w     84.00 178.00   0.50    0.25    --  121.50  30.00 150.00  188
 34  \w     58.00  84.00   0.50    0.25    --  121.50  17.00-104.25   52
 35  \w     92.00 178.00   0.50    0.25    --  121.50  45.00-150.00  172
 36  \w    138.00 178.00   0.50    0.25    --  121.50  45.00-150.00   80
 37  \w     96.00 144.00   0.50    0.25    --  121.50  45.00-180.00   96
 38  \w    142.00 171.00   0.50    0.25    --  121.50  15.00-150.00   58
 39  \w     65.00 178.00   0.50    0.25    --  121.50  22.00 -75.63  226
 40  \w    137.00 163.00   0.50    0.25    --  121.50  15.00 120.00   52
 41  \w     42.00  97.00   0.50    0.25    --  121.50  15.00 120.00  110
 42  \w     -1.00  29.00   0.50    0.15    --   41.38  96.00  -5.07   60
 43  \w    -86.00 -39.00   0.50    0.05    --    0.00 178.00 -60.00   94
 44  \w    -51.00 -21.00   0.50    0.25    -- -100.00  45.00  90.00   60
 45  \w    -27.00  41.00   0.50    0.15    --  -41.38  19.00  60.00  136
 46  \w    121.00 146.00   0.50    0.25    --  121.50 178.00 -60.00   50
 47  \w    -27.00  41.00   0.50    0.15    --  -41.38  19.00  30.00  136
 48  \w    -82.00 -23.00   0.50    0.25    -- -100.00 111.00   0.00  118
 49  \w    -91.00 -24.00   0.50    0.25    -- -100.00  72.00-127.00  134
 50  \w   -175.00 -67.00   0.50    0.25    -- -100.00 -72.00 103.00  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      -0.0694334000
_diffrn_orient_matrix_UB_12      -0.0670528000
_diffrn_orient_matrix_UB_13      0.0494501000
_diffrn_orient_matrix_UB_21      -0.1681193000
_diffrn_orient_matrix_UB_22      0.0142497000
_diffrn_orient_matrix_UB_23      -0.0834046000
_diffrn_orient_matrix_UB_31      0.0446083000
_diffrn_orient_matrix_UB_32      -0.0505163000
_diffrn_orient_matrix_UB_33      -0.0891641000
_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  0.0309
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26603
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.311
_diffrn_reflns_theta_min         4.502
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.167
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.287
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.125a (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            'clear red'
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.00067(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   1.053
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         3948
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+1.1244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3841
_reflns_number_total             3948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01304b2.cif
_cod_data_source_block           DPR557
_cod_depositor_comments
'Adding full bibliography for 7716642--7716648.cif.'
_cod_original_formula_sum        'C20 H16 Cl F2 N2 Ni O0.50'
_cod_database_code               7716648
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H16.00 Cl F2 N2 Ni O0.50'
_chemical_oxdiff_usercomment     DPR557
_shelx_estimated_absorpt_t_max   0.764
_shelx_estimated_absorpt_t_min   0.270
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1-H1A = O1-H1B
 0.84 with sigma of 0.02
 Ni1-Cl1 \\sim Ni1-Cl1A \\sim Ni1-Cl1B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cl1) = Uanis(Cl1A) = Uanis(Cl1B)
4. Others
 1*[Sof(Cl1)+Sof(O1)+Sof(H1A)+Sof(H1B)]+1*[Sof(Cl1A)]+1*[Sof(Cl1B)]=1 with esd
 of 0.00001
 Sof(Cl1)=Sof(O1)=Sof(H1A)=Sof(H1B)=FVAR(1)
;
_shelx_res_checksum              86030
_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 1.175
_oxdiff_exptl_absorpt_empirical_full_min 0.913