Methylpalladium complexes with pyrimidine-functionalized N-heterocyclic carbene ligands.
Meyer, Dirk; Strassner, Thomas; Beilstein journal of organic chemistry 12 (2016) 1557–1565; doi:10.3762/bjoc.12.150

data_4032039
_publ_section_title
;
 Methylpalladium complexes with pyrimidine-functionalized N-heterocyclic
 carbene ligands.
;
_journal_name_full               'Beilstein journal of organic chemistry'
_journal_page_first              1557
_journal_page_last               1565
_journal_paper_doi               10.3762/bjoc.12.150
_journal_volume                  12
_journal_year                    2016
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C14 H12 Br Cl N4 Pd'
_chemical_formula_sum            'C14 H12 Br Cl N4 Pd'
_chemical_formula_weight         458.04
_chemical_melting_point          475
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 102.069(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0550(8)
_cell_length_b                   8.0500(5)
_cell_length_c                   17.9200(10)
_cell_measurement_reflns_used    112
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      20.621
_cell_measurement_theta_min      4.158
_cell_volume                     1559.50(18)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics
'Ortep III 1.0.3 (M.N.Burnett,C.K.Johnson,2000)'
_computing_publication_material  'XCIF 6.12 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      198(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18071
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         4.83
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.920
_exptl_absorpt_correction_T_max  0.8281
_exptl_absorpt_correction_T_min  0.5018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS 2.03.(Sheldrick,Bruker AXS Inc.,2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_recrystallization_method 'Acetonitrile/Diethyl ether'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                2358
_reflns_number_total             3175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1860-5397-12-150-S3.cif
_cod_data_source_block           str-307
_cod_depositor_comments
'Adding full bibliography for 4032038--4032040.cif.'
_cod_original_cell_volume        1559.50(17)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4032039