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_4080634
_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         'C13 H18 Cl2 N2 O Pd, C H2 Cl2'
_chemical_formula_sum            'C14 H20 Cl4 N2 O Pd'
_chemical_formula_weight         480.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4035(4)
_cell_length_b                   11.5964(4)
_cell_length_c                   17.0774(6)
_cell_measurement_reflns_used    7532
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.16
_cell_measurement_theta_min      4.68
_cell_volume                     1862.23(12)
_computing_cell_refinement       'Bruker SAINT v7.68A'
_computing_data_collection       'Bruker APEX-II v2010-7'
_computing_data_reduction        'Bruker SAINT v7.68A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18310
_diffrn_reflns_theta_full        69.92
_diffrn_reflns_theta_max         69.92
_diffrn_reflns_theta_min         4.61
_exptl_absorpt_coefficient_mu    13.335
_exptl_absorpt_correction_T_max  0.4754
_exptl_absorpt_correction_T_min  0.1427
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS, Sheldrick, 2008'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0179
_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^)+(0.0217P)^2^+0.3659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0444
_reflns_number_gt                3398
_reflns_number_total             3464
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4001549_si_002.cif
_cod_data_source_block           4d
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4080634