Enhanced π-back-donation resulting in the <i>trans</i> labilization of a pyridine ligand in an N-heterocyclic carbene (NHC) Pd^II^ precatalyst: a case study
Karabıyık, Hande; Yiğit, Beyhan; Yiğit, Murat; Özdemir, İsmail; Karabıyık, Hasan; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619007745

data_2021672
_publ_section_title
;
 Enhanced \p-back-donation resulting in the <i>trans</i> labilization of a
 pyridine ligand in an N-heterocyclic carbene (NHC) Pd^II^ precatalyst: a
 case study
;
_journal_coeditor_code           FN3308
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619007745
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Pd Cl2 (C5 H5 N) (C23 H40 N4)]'
_chemical_formula_moiety         'C28 H45 Cl2 N5 Pd'
_chemical_formula_sum            'C28 H45 Cl2 N5 Pd'
_chemical_formula_weight         628.99
_chemical_name_systematic
'[1,3-Bis(2-diisopropylaminoethyl)benzimidazol-2-ylidene-\k<i>C</i>^2^]dichlorido(pyridine-\k<i>N</i>)palladium(II)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 100.640(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1029(4)
_cell_length_b                   15.9363(5)
_cell_length_c                   19.3855(8)
_cell_measurement_reflns_used    4189
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      28.2580
_cell_measurement_theta_min      3.6960
_cell_volume                     3067.5(2)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      297(2)
_diffrn_detector_area_resol_mean 8.0667
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku OD Xcalibur Eos'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9525
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         3.225
_exptl_absorpt_coefficient_mu    0.804
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Rigaku OD, 2015), based on expressions derived by
Clark & Reid (1995)]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.294
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5780
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0247P)^2^+1.0500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0740
_reflns_number_gt                4563
_reflns_number_total             5780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fn3308sup1.cif
_cod_data_source_block           I
_cod_database_code               2021672
_shelx_estimated_absorpt_t_min   0.771
_shelx_estimated_absorpt_t_max   0.805
_shelx_hkl_checksum              2088
_shelx_res_checksum              21216
_cod_database_fobs_code 2021672