Synthesis and characterization of Pd/NHCF complexes with fluorinated aryl groups
Prima, Darya O.; Pankov, Roman O.; Kostyukovich, Alexander Yu.; Minyaev, Mikhail E.; Burykina, Julia V.; Ananikov, Valentine P.; Dalton Transactions  (2022) –; doi:10.1039/D2DT00892K

data_7710505
_publ_section_title
;
 Synthesis and characterization of Pd/NHCF complexes with fluorinated aryl
 groups
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00892K
_journal_year                    2022
_chemical_formula_moiety         'C20 H15 Cl2 F2 N3 Pd'
_chemical_formula_sum            'C20 H15 Cl2 F2 N3 Pd'
_chemical_formula_weight         512.65
_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             2021-09-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-12-27 deposited with the CCDC.	2022-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.913(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.4450(2)
_cell_length_b                   13.5214(3)
_cell_length_c                   31.7529(7)
_cell_measurement_reflns_used    23231
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      35.3390
_cell_measurement_theta_min      2.1380
_cell_volume                     4045.70(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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 0.999
_diffrn_measured_fraction_theta_max 0.923
_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    -43.00 -13.00   0.30    3.50    --  -26.44 -38.00 136.00  100
  2  \w    -52.00  21.20   0.30    3.50    --   26.75 -38.00 136.00  244
  3  \w     -5.00 104.20   0.30    3.50    --   26.75  38.00 -68.00  364
  4  \w   -102.00 -69.00   0.30    3.50    --  -26.44-178.00-120.00  110
  5  \w   -104.00 -68.00   0.30    3.50    --  -26.44-178.00-150.00  120
  6  \w     42.00  97.20   0.30    3.50    --   26.75 178.00 120.00  184
;
_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      -0.0660073000
_diffrn_orient_matrix_UB_12      0.0205682000
_diffrn_orient_matrix_UB_13      0.0047264000
_diffrn_orient_matrix_UB_21      0.0295921000
_diffrn_orient_matrix_UB_22      0.0142877000
_diffrn_orient_matrix_UB_23      0.0202258000
_diffrn_orient_matrix_UB_31      0.0205129000
_diffrn_orient_matrix_UB_32      0.0461263000
_diffrn_orient_matrix_UB_33      -0.0084053000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            41826
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.000
_diffrn_reflns_theta_min         2.161
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.106a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         16449
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+0.9405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13781
_reflns_number_total             16449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00892k2.cif
_cod_data_source_block           4a_2
_cod_database_code               7710505
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pd Cl2 F2 N3 C20 H20'
_chemical_oxdiff_usercomment     Pro_4a_O-F
_shelx_estimated_absorpt_t_max   0.839
_shelx_estimated_absorpt_t_min   0.760
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.07
_olex2_refinement_description
;
;
_shelx_res_checksum              98501
_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 1.388
_oxdiff_exptl_absorpt_empirical_full_min 0.811