Characterization of Peroxo and Hydroperoxo Intermediates in the Aerobic Oxidation of N-Heterocyclic-Carbene-Coordinated Palladium(0)
Michael M. Konnick; Ilia A. Guzei; Shannon S. Stahl; Journal of the American Chemical Society 126 (2004) 10212–10213; doi:10.1021/ja046884u

data_4112874
_publ_section_title
;
 Characterization of Peroxo and Hydroperoxo Intermediates in the Aerobic
 Oxidation of N-Heterocyclic-Carbene-Coordinated Palladium(0)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10212
_journal_page_last               10213
_journal_paper_doi               10.1021/ja046884u
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C46 H54 N4 O4 Pd'
_chemical_formula_weight         833.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.1275(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.0229(13)
_cell_length_b                   9.9968(10)
_cell_length_c                   16.3609(16)
_cell_measurement_temperature    100(2)
_cell_volume                     2046.2(4)
_computing_cell_refinement       'Bruker SMART'
_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_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48596
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  0.8977
_exptl_absorpt_correction_T_min  0.8132
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_meas      0
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         5094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0537P)^2^+1.6666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                4848
_reflns_number_total             5094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046884usi20040526_064439.cif
_cod_data_source_block           sta15
_cod_database_code               4112874