Bimetallic Palladium Catalysis: Direct Observation of Pd(III)-Pd(III) Intermediates
David C. Powers; Matthias A. L. Geibel; Johannes E. M. N. Klein; Tobias Ritter; Journal of the American Chemical Society 131 (2009) 17050–17051; doi:10.1021/ja906935c

data_4105403
_publ_section_title
;
 Bimetallic Palladium Catalysis: Direct Observation of Pd(III)-Pd(III)
 Intermediates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17050
_journal_page_last               17051
_journal_paper_doi               10.1021/ja906935c
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C32.38 H32.75 Cl4.75 N2 O8 Pd2'
_chemical_formula_weight         959.04
_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                95.217(2)
_cell_angle_beta                 90.019(2)
_cell_angle_gamma                95.349(2)
_cell_formula_units_Z            4
_cell_length_a                   13.0941(19)
_cell_length_b                   14.506(2)
_cell_length_c                   19.684(3)
_cell_measurement_reflns_used    4101
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.31
_cell_volume                     3707.0(9)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_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  0.0688
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20684
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    1.363
_exptl_absorpt_correction_T_max  0.7915
_exptl_absorpt_correction_T_min  0.7269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       block
_exptl_crystal_F_000             1911
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.719
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1021
_refine_ls_number_reflns         20691
_refine_ls_number_restraints     1270
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0241P)^2^+10.3349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                17004
_reflns_number_total             20691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906935c_si_002.cif
_cod_data_source_block           09238
_cod_original_cell_volume        3707.2(9)
_cod_database_code               4105403