Chemoselective Oxidation of Polyols with Chiral Palladium Catalysts
De Crisci, Antonio G.; Chung, Kevin; Oliver, Allen G.; Solis-Ibarra, Diego; Waymouth, Robert M.; Organometallics 32 (2013) 2257–; doi:10.1021/om4001549

data_4080636
_publ_section_title
;
 Chemoselective Oxidation of Polyols with Chiral Palladium Catalysts
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2257
_journal_paper_doi               10.1021/om4001549
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C30 H42 N4 O6 Pd2, 2(C F3 O3 S)'
_chemical_formula_sum            'C32 H42 F6 N4 O12 Pd2 S2'
_chemical_formula_weight         1065.62
_space_group_IT_number           1
_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                71.972(2)
_cell_angle_beta                 70.386(2)
_cell_angle_gamma                85.060(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8875(9)
_cell_length_b                   10.6135(10)
_cell_length_c                   10.6892(9)
_cell_measurement_reflns_used    6844
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.90
_cell_measurement_theta_min      2.18
_cell_volume                     1004.57(16)
_computing_cell_refinement       'Bruker SAINT v7.66A'
_computing_data_collection       'Bruker APEX-II v2011-4.1'
_computing_data_reduction        'Bruker SAINT v7.66A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa X8-APEX-II'
_diffrn_measurement_method       'combination of \w and \f-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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19114
_diffrn_reflns_theta_full        26.56
_diffrn_reflns_theta_max         26.56
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    1.091
_exptl_absorpt_correction_T_max  0.9377
_exptl_absorpt_correction_T_min  0.8541
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS, Sheldrick, 2008'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.006(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         7464
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0236P)^2^+0.1943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0570
_reflns_number_gt                6746
_reflns_number_total             7464
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4001549_si_002.cif
_cod_data_source_block           6d
_cod_database_code               4080636