Synthesis and a combined experimental/theoretical structural study of a comprehensive set of Pd/NHC complexes with <i>o</i>-, <i>m</i>-, and <i>p</i>-halogen-substituted aryl groups (X = F, Cl, Br, CF<sub>3</sub>).
Pankov, Roman O.; Prima, Darya O.; Kostyukovich, Alexander Yu; Minyaev, Mikhail E.; Ananikov, Valentine P.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d2dt03665g

data_7712540
_publ_section_title
;
 Synthesis and a combined experimental/theoretical structural study of a
 comprehensive set of Pd/NHC complexes with <i>o</i>-, <i>m</i>-, and
 <i>p</i>-halogen-substituted aryl groups (X = F, Cl, Br, CF<sub>3</sub>).
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt03665g
_journal_year                    2023
_chemical_formula_moiety         'C20 H15 Br2.41 Cl1.59 N3 Pd'
_chemical_formula_sum            'C20 H15 Br2.41 Cl1.59 N3 Pd'
_chemical_formula_weight         652.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-11-06 deposited with the CCDC.	2023-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.1093(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0556(4)
_cell_length_b                   15.0381(3)
_cell_length_c                   6.98560(10)
_cell_measurement_reflns_used    9396
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.28
_cell_measurement_theta_min      3.12
_cell_volume                     2280.97(7)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       '<i>APEX3</i> (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)'
_computing_publication_material
'SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)'
_computing_structure_refinement
'SHELXL-2018 (Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_computing_structure_solution
'SHELXT (Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS D8 QUEST, Photon III detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            42511
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.351
_diffrn_reflns_theta_min         3.124
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30
_diffrn_source_power             1.5
_diffrn_source_size              '0.6 mm, fine-focus'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.230
_exptl_absorpt_correction_T_max  0.6471
_exptl_absorpt_correction_T_min  0.4765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS 2016/2 (Krause et al., J. Appl. Cryst. 2015, 48, 3-10)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_description       block
_exptl_crystal_F_000             1253.5
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         4772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0201P)^2^+3.0779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0495
_refine_ls_wR_factor_ref         0.0529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4059
_reflns_number_total             4772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03665g2.cif
_cod_data_source_block           3iA
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7712540
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.415
_shelx_estimated_absorpt_t_max   0.573
_shelx_res_checksum              5652
_shelx_hkl_checksum              90149