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_7719464
_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         'C26 H34 Br2 N6 Pd'
_chemical_formula_sum            'C26 H34 Br2 N6 Pd'
_chemical_formula_weight         696.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 98.478(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5704(2)
_cell_length_b                   11.0703(3)
_cell_length_c                   14.3824(4)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      3.19
_cell_volume                     1349.65(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0276
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26867
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.296
_diffrn_reflns_theta_min         3.027
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    3.675
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>SADABS</i> (Krause <i>et al</i>., 2015)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       shard
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3361
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0165
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0105P)^2^+1.0337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0358
_refine_ls_wR_factor_ref         0.0367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3093
_reflns_number_total             3361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01695a2.cif
_cod_data_source_block           m25190
_cod_depositor_comments
'Adding full bibliography for 7719463--7719465.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7719464
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.527
_shelx_estimated_absorpt_t_max   0.710
_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              4175