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_7710506
_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 H13 Cl2 F4 N3 Pd, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C20.5 H14 Cl3 F4 N3 Pd'
_chemical_formula_weight         591.10
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-09-29
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.7586(3)
_cell_length_b                   7.15170(10)
_cell_length_c                   26.0618(4)
_cell_measurement_reflns_used    38683
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      35.8010
_cell_measurement_theta_min      2.3740
_cell_volume                     4241.89(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.117a (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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(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 0.921
_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    -91.00  -7.00   0.35    4.21    --  -17.72 -14.00  -3.00  240
  2  \w     44.00  90.55   0.35    4.21    --   17.87 173.00  64.00  133
  3  \w    -89.00  -3.60   0.35    4.21    --  -17.72 -57.00 -90.00  244
  4  \w    -56.00   5.25   0.35    4.21    --   17.87 -19.00 -60.00  175
  5  \w    -56.00   3.15   0.35    4.21    --   17.87 -14.00  -3.00  169
  6  \w    -56.00   3.15   0.35    4.21    --   17.87 -19.00 150.00  169
;
_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      0.0269764000
_diffrn_orient_matrix_UB_12      -0.0024486000
_diffrn_orient_matrix_UB_13      -0.0136135000
_diffrn_orient_matrix_UB_21      -0.0154570000
_diffrn_orient_matrix_UB_22      -0.0179297000
_diffrn_orient_matrix_UB_23      -0.0231145000
_diffrn_orient_matrix_UB_31      -0.0021588000
_diffrn_orient_matrix_UB_32      0.0975131000
_diffrn_orient_matrix_UB_33      -0.0045979000
_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  0.0286
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            63848
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.498
_diffrn_reflns_theta_min         2.376
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.302
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.117a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         8926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+3.0892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7935
_reflns_number_total             8926
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00892k2.cif
_cod_data_source_block           4c
_cod_original_formula_sum        'C20.50 H14 Cl3 F4 N3 Pd'
_cod_database_code               7710506
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20.50 H14 Cl3 F4 N3 Pd'
_chemical_oxdiff_usercomment     Pro-193
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.829
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.07
_olex2_refinement_description
;
;
_shelx_res_checksum              42223
_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 2.845
_oxdiff_exptl_absorpt_empirical_full_min 0.543