Palladium Complexes with Pyrimidine-Functionalized N-Heterocyclic Carbene Ligands: Synthesis, Structure and Catalytic Activity
Meyer, Dirk; Taige, Maria A.; Zeller, Alexander; Hohlfeld, Konrad; Ahrens, Sebastian; Strassner, Thomas; Organometallics 28 (2009) 2142–; doi:10.1021/om8009238

data_4068544
_publ_section_title
;
 Palladium Complexes with Pyrimidine-Functionalized N-Heterocyclic Carbene
 Ligands: Synthesis, Structure and Catalytic Activity
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2142
_journal_paper_doi               10.1021/om8009238
_journal_volume                  28
_journal_year                    2009
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C16 H16 Cl N8 Pd, C2 H6 Cl3 O Pd S'
_chemical_formula_sum            'C18 H22 Cl4 N8 O Pd2 S'
_chemical_formula_weight         753.15
_chemical_name_systematic
;
Bis(1-(2-pyrimidyl)-3-(methyl)imidazoline-2-ylidene) palladium(II) chloride
dimethyl-sulfoxidotrichloro palladium(II)
;
_chemical_temperature_decomposition 463.15
_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                 102.27(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.247(1)
_cell_length_b                   28.120(3)
_cell_length_c                   8.434(1)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      19.245
_cell_measurement_theta_min      3.363
_cell_volume                     2606.5(5)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            25176
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.51
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.899
_exptl_absorpt_correction_T_max  0.8881
_exptl_absorpt_correction_T_min  0.3545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2.03.(Sheldrick,Bruker AXS Inc.,2002)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1480
_exptl_crystal_recrystallization_method
'slow evaporation of an acetonitrile solution'
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0114P)^2^+4.5053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0484
_reflns_number_gt                4019
_reflns_number_total             4483
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8009238_si_001.cif
_cod_data_source_block           str-153a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been given
as '190 \%C (Decomp.)'. The value '190 \%C (Decomp.)' was changed to
'463.15' - it was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4068544