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_7710508
_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      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.2541(2)
_cell_length_b                   14.2448(2)
_cell_length_c                   24.6718(3)
_cell_measurement_reflns_used    41862
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      35.3080
_cell_measurement_theta_min      2.4290
_cell_volume                     3955.20(10)
_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)'
_computing_structure_solution    'XT  (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 1.000
_diffrn_measured_fraction_theta_max 0.973
_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     41.00 108.90   0.35    1.70    --   26.74 178.00 150.00  194
  2  \w      0.00 101.15   0.35    1.70    --   26.74  57.00 -30.00  289
  3  \w    -59.00   4.00   0.35    1.70    --   26.74 -19.00 -90.00  180
  4  \w    -52.00  32.00   0.35    1.70    --   26.74 -48.00-157.00  240
  5  \w   -101.00   7.15   0.35    1.70    --  -26.43 -77.00  30.00  309
  6  \w   -111.00 -63.75   0.35    1.70    --  -26.43-178.00 120.00  135
  7  \w   -111.00 -85.80   0.35    1.70    --  -26.43-178.00-150.00   72
  8  \w   -101.00   7.15   0.35    1.70    --  -26.43 -77.00-180.00  309
  9  \w   -105.00 -51.80   0.35    1.70    --  -26.43 157.00  14.00  152
;
_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      0.0076829000
_diffrn_orient_matrix_UB_12      -0.0033813000
_diffrn_orient_matrix_UB_13      0.0284628000
_diffrn_orient_matrix_UB_21      0.0507073000
_diffrn_orient_matrix_UB_22      0.0293925000
_diffrn_orient_matrix_UB_23      -0.0017229000
_diffrn_orient_matrix_UB_31      -0.0365971000
_diffrn_orient_matrix_UB_32      0.0400752000
_diffrn_orient_matrix_UB_33      0.0036518000
_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  0.0503
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            76516
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.992
_diffrn_reflns_theta_min         2.450
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.237
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61440
_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    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         8463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0245
_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^)+(0.0293P)^2^+1.7222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7332
_reflns_number_total             8463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00892k2.cif
_cod_data_source_block           4a_1
_cod_database_code               7710508
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     Pro_4b_O-F
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.747
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
;
_shelx_res_checksum              56869
_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 1.485
_oxdiff_exptl_absorpt_empirical_full_min 0.669