Synthesis of Pd(II)-NHC complexes <i>via</i> C-H oxidative addition of triazolium salts to Pd(0).
Kovacevic, Anes; Parkin, Sean; Baltisberger, Jay H.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13863–13868; doi:10.1039/d5dt01695a

data_7719463
_publ_section_title
;
 Synthesis of Pd(II)-NHC complexes <i>via</i> C-H oxidative addition of
 triazolium salts to Pd(0).
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13863
_journal_page_last               13868
_journal_paper_doi               10.1039/d5dt01695a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C20 H22 Br2 N6 Pd'
_chemical_formula_sum            'C20 H22 Br2 N6 Pd'
_chemical_formula_weight         612.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2019/3 and CIFFIX'
_audit_update_record
;
2025-07-04 deposited with the CCDC.	2025-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.53(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.124(2)
_cell_length_b                   9.3713(19)
_cell_length_c                   11.796(2)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.81
_cell_volume                     1083.4(4)
_computing_cell_refinement       '<i>APEX5</i> (Bruker-AXS, 2023)'
_computing_data_collection       '<i>APEX5</i> (Bruker-AXS, 2023)'
_computing_data_reduction        '<i>APEX5</i> (Bruker-AXS, 2023)'
_computing_molecular_graphics    '<i>XP in SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material
'<i>SHELX</i> (Sheldrick, 2008) and <i>CIFFIX</i> (Parkin, 2013)'
_computing_structure_refinement  '<i>SHELXL-2019/3</i> (Sheldrick, 2015b)'
_computing_structure_solution    '<i>SHELXT</i> (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture dual source'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15508
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.299
_diffrn_reflns_theta_min         2.812
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    4.564
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>SADABS</i> (Krause <i>et al</i>., 2015)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_description       'wedge-shaped shard'
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
; 
Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.024(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2627
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0155
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.0144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0392
_refine_ls_wR_factor_ref         0.0401
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_full    0.936
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                2451
_reflns_number_total             2627
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01695a2.cif
_cod_data_source_block           m25192
_cod_depositor_comments
'Adding full bibliography for 7719463--7719465.cif.'
_cod_original_sg_symbol_H-M      'I 2'
_cod_database_code               7719463
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.462
_shelx_estimated_absorpt_t_max   0.804
_exptl_absorpt_special_details
; 
In addition to absorption, multi-scan techniques also correct other slowly 
varying changes in scale factor over reciprocal space, such as those caused 
by X-ray beam inhomogeneity, goniometer imperfection, crystal decomposition, 
crystal longer than the X-ray beam cross section, absorption by the crystal 
mount, scan truncation etc. These account, by and large, for the difference 
between SHELX estimates of Tmin and Tmax and the _exptl_absorpt_correction_ 
values. 
;
_shelx_res_checksum              76177