Discovery of and Mechanistic Insight into a Ligand-Modulated Palladium-Catalyzed Wacker Oxidation of Styrenes Using TBHP
Candace N. Cornell; Matthew S. Sigman; Journal of the American Chemical Society 127 (2005) 2796–2797; doi:10.1021/ja043203m

data_4111479
_publ_section_title
;
 Discovery of and Mechanistic Insight into a Ligand-Modulated
 Palladium-Catalyzed Wacker Oxidation of Styrenes Using TBHP
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2796
_journal_page_last               2797
_journal_paper_doi               10.1021/ja043203m
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety
'C27 H42 N2 O3 Pd,2(C F3 O3 S),2(H2 O),0.75(C2 H4 Cl2)'
_chemical_formula_sum            'C30.5 H49 Cl1.5 F6 N2 O11 Pd S2'
_chemical_formula_weight         957.41
_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                 95.9628(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0714(2)
_cell_length_b                   19.7126(5)
_cell_length_c                   17.3751(4)
_cell_measurement_reflns_used    7863
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      1.018
_cell_volume                     4452.84(17)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'WinGX, Ortep3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCd Diffractometer'
_diffrn_measurement_method       'Phi plus Omega scan'
_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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13961
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_T_max  0.8880
_exptl_absorpt_correction_T_min  0.7832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       prism
_exptl_crystal_F_000             1966
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         8101
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0602
_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^)+(0.0890P)^2^+8.7965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1587
_refine_ls_wR_factor_ref         0.1697
_reflns_number_gt                6476
_reflns_number_total             8101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja043203msi20041111_121032.cif
_cod_data_source_block           mss023
_cod_original_formula_sum        'C30.50 H49 Cl1.50 F6 N2 O11 Pd S2'
_cod_database_code               4111479