Organometallic Complexes of Palladium(II) Derived from 2,6-Diacetylpyridine Dimethylketal
Vicente, José; Arcas, Aurelia; Juliá-Hernández, Francisco; Bautista, Delia; Jones, Peter G.; Organometallics 29 (2010) 3066–; doi:10.1021/om100079x

data_4065694
_publ_section_title
;
 Organometallic Complexes of Palladium(II) Derived from
 2,6-Diacetylpyridine Dimethylketal
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3066
_journal_paper_doi               10.1021/om100079x
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C13 H22 Cl3 N O4 Pd'
_chemical_formula_weight         469.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.138(2)
_cell_angle_beta                 99.345(2)
_cell_angle_gamma                115.648(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6256(11)
_cell_length_b                   9.9998(11)
_cell_length_c                   11.0056(12)
_cell_measurement_reflns_used    5424
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.96
_cell_measurement_theta_min      2.36
_cell_volume                     900.00(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w-scan
_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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10399
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    1.490
_exptl_absorpt_correction_T_max  0.9292
_exptl_absorpt_correction_T_min  0.7752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    'NH free, methyls rigid, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         4013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0199P)^2^+0.7414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0540
_refine_ls_wR_factor_ref         0.0553
_reflns_number_gt                3758
_reflns_number_total             4013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100079x_si_002.cif
_cod_data_source_block           2173nas
_cod_database_code               4065694