Oxidatively Induced Reductive Elimination from (tBu2bpy)Pd(Me)2: Palladium(IV) Intermediates in a One-Electron Oxidation Reaction
Michael P. Lanci; Matthew S. Remy; Werner Kaminsky; James M. Mayer; Melanie S. Sanford; Journal of the American Chemical Society 131 (2009) 15618–15620; doi:10.1021/ja905816q

data_4105243
_publ_contact_author_address
;
Department of Chemistry, BOX 351700
University of Washington
Seattle, WA 98195
USA
;
_publ_contact_author_email       wernerka@u.washington.edu
_publ_contact_author_name        'Werner Kaminsky'
_publ_section_title
;
 Oxidatively Induced Reductive Elimination from (tBu2bpy)Pd(Me)2:
 Palladium(IV) Intermediates in a One-Electron Oxidation Reaction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15618
_journal_page_last               15620
_journal_paper_doi               10.1021/ja905816q
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety
'2(C63 H96 N6 O Pd3 Tl2), 0.5(C4 H10 O), 4(F6 P), 2(C3 H6 O)'
_chemical_formula_sum            'C134 H209 F24 N12 O4.5 P4 Pd6 Tl4'
_chemical_formula_weight         4095.89
_chemical_name_common            ML097_3
_chemical_name_systematic        ML097_3
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                90.5519(11)
_cell_angle_beta                 99.3054(11)
_cell_angle_gamma                103.8930(16)
_cell_formula_units_Z            1
_cell_length_a                   15.5080(4)
_cell_length_b                   16.1827(5)
_cell_length_c                   16.3415(6)
_cell_measurement_reflns_used    733
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     3923.7(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w 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  0.0744
_diffrn_reflns_av_sigmaI/netI    0.1325
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30628
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    4.880
_exptl_absorpt_correction_T_max  0.086
_exptl_absorpt_correction_T_min  0.080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2008
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       prism
_exptl_crystal_F_000             2009
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.50
_refine_diff_density_max         2.826
_refine_diff_density_min         -2.094
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         18676
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.1167
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1350
_reflns_number_gt                10845
_reflns_number_total             18676
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905816q_si_003.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C134 H209 F24 N12 O4.50 P4 Pd6 Tl4'
_cod_database_code               4105243