Detailed Study of C-O and C-C Bond-Forming Reductive Elimination from Stable C2N2O2-Ligated Palladium(IV) Complexes
Joy M. Racowski; Allison R. Dick; Melanie S. Sanford; Journal of the American Chemical Society 131 (2009) 10974–10983; doi:10.1021/ja9014474

data_4104805
_publ_section_title
;
 Detailed Study of C-O and C-C Bond-Forming Reductive Elimination from
 Stable C2N2O2-Ligated Palladium(IV) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10974
_journal_page_last               10983
_journal_paper_doi               10.1021/ja9014474
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C26 H22 N2 O4 Pd, C6 H6'
_chemical_formula_sum            'C32 H28 N2 O4 Pd'
_chemical_formula_weight         610.96
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.00
_cell_angle_beta                 101.6540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0071(10)
_cell_length_b                   13.9633(11)
_cell_length_c                   15.6648(13)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.76
_cell_volume                     2572.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART-APEX'
_computing_data_reduction        'Bruker SAINT'
_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      85(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0565
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29142
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.9701
_exptl_absorpt_correction_T_min  0.9414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  SADABS (Version 2008/1) Bruker AXS area
  detector absorption and other corrections, University of
  Gottingen, Germany 2008.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.634
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3214
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0320P)^2^+4.9469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                2939
_reflns_number_total             3214
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9014474_si_001.cif
_cod_data_source_block           jr491
_cod_database_code               4104805