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_4112873
_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            'C49 H56 N4 O2 Pd'
_chemical_formula_weight         839.38
_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                 98.1911(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3902(11)
_cell_length_b                   14.6410(12)
_cell_length_c                   22.6735(18)
_cell_measurement_reflns_used    ****
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.17
_cell_volume                     4399.7(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0271
_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       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36033
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.464
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.8255
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_meas      0
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         8990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0522P)^2^+0.7051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                8108
_reflns_number_total             8990
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046884usi20040526_064424.cif
_cod_data_source_block           sta10
_cod_database_code               4112873