Palladium(ii) complexes with electron-poor, 4,5-disubstituted diimidazol-2-ylidene ligands: synthesis, characterization and catalytic activity.
Pinter, Piermaria; Biffis, Andrea; Tubaro, Cristina; Tenne, Mario; Kaliner, Maria; Strassner, Thomas; Dalton transactions (Cambridge, England : 2003) 44 (2015) 9391–9399; doi:10.1039/c5dt01067e

data_7034817
_publ_section_title
;
 Palladium(ii) complexes with electron-poor, 4,5-disubstituted
 diimidazol-2-ylidene ligands: synthesis, characterization and catalytic
 activity.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9391
_journal_page_last               9399
_journal_paper_doi               10.1039/c5dt01067e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         '3(C9 H8 Br2 Cl4 N4 Pd), C2 H3 N'
_chemical_formula_sum            'C9.66667 H9 Br2 Cl4 N4.33333 Pd'
_chemical_formula_weight         593.90
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-03-16 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   19.767(5)
_cell_length_b                   15.478(10)
_cell_length_c                   34.001(9)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      20.899
_cell_measurement_theta_min      4.166
_cell_volume                     10403(8)
_computing_cell_refinement       'Dirax/lsq (Duisenberg, 1992)'
_computing_data_collection       'Collect (Nonius BV, 1999)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 2012)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      198(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1558
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            177002
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    6.292
_exptl_absorpt_correction_T_max  0.4215
_exptl_absorpt_correction_T_min  0.1521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             6752
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.134
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.353
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         7462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+30.9607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                5210
_reflns_number_total             7462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01067e2.cif
_cod_data_source_block           compound_3a
_cod_depositor_comments
'Adding full bibliography for 7034817--7034820.cif.'
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7034817