Unusually Stable Palladium(IV) Complexes: Detailed Mechanistic Investigation of C-O Bond-Forming Reductive Elimination
Allison R. Dick; Jeff W. Kampf; Melanie S. Sanford; Journal of the American Chemical Society 127 (2005) 12790–12791; doi:10.1021/ja0541940

data_4111948
_publ_section_title
;
 Unusually Stable Palladium(IV) Complexes: Detailed Mechanistic
 Investigation of C-O Bond-Forming Reductive Elimination
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12790
_journal_page_last               12791
_journal_paper_doi               10.1021/ja0541940
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C36 H24 N4 O8 Pd, C H2 Cl2'
_chemical_formula_sum            'C37 H26 Cl2 N4 O8 Pd'
_chemical_formula_weight         831.92
_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                91.950(4)
_cell_angle_beta                 109.062(3)
_cell_angle_gamma                92.205(4)
_cell_formula_units_Z            2
_cell_length_a                   11.287(3)
_cell_length_b                   12.574(3)
_cell_length_c                   12.667(3)
_cell_measurement_reflns_used    8233
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      2.95
_cell_volume                     1695.8(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32168
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  0.9205
_exptl_absorpt_correction_T_min  0.8141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38
  Sheldrick, G.  SADABS (Version 2.10) Bruker/Siemens area
  detector absorption and other corrections, University of
  Gottingen, Germany 2003.'
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.956
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         8390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0621P)^2^+3.7010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                7460
_reflns_number_total             8390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0541940si20050629_121746.cif
_cod_data_source_block           ad213
_cod_original_cell_volume        1695.8(6)
_cod_database_code               4111948