An Experimentally Derived Model for Stereoselectivity in the Aerobic Oxidative Kinetic Resolution of Secondary Alcohols by (Sparteine)PdCl2
Raissa M. Trend; Brian M. Stoltz; Journal of the American Chemical Society 126 (2004) 4482–4483; doi:10.1021/ja039551q

data_4112418
_publ_contact_author
;       Michael W. Day
        Beckman Institute
        California Institute of Technology
        Pasadena, CA  91125
        USA
;
_publ_contact_author_email       mikeday@caltech.edu
_publ_contact_author_fax         '(818) 449 4159'
_publ_contact_author_phone       '(818) 395 2734'
_publ_section_title
;
 An Experimentally Derived Model for Stereoselectivity in the Aerobic
 Oxidative Kinetic Resolution of Secondary Alcohols by (Sparteine)PdCl2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4482
_journal_page_last               4483
_journal_paper_doi               10.1021/ja039551q
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C15 H26 Cl2 N2 Pd'
_chemical_formula_weight         411.68
_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                   9.2815(3)
_cell_length_b                   11.4873(4)
_cell_length_c                   15.1073(5)
_cell_measurement_reflns_used    24049
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.96
_cell_measurement_theta_min      2.22
_cell_volume                     1610.73(9)
_computing_cell_refinement       'Bruker SAINT v6.45'
_computing_data_collection       'Bruker SMART v5.054'
_computing_data_reduction        'Bruker SAINT v6.45'
_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 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       '\w scans at 7 \f settings'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0629
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            44470
_diffrn_reflns_theta_full        44.97
_diffrn_reflns_theta_max         44.97
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    1.476
_exptl_absorpt_correction_T_max  0.7372
_exptl_absorpt_correction_T_min  0.5968
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Maroon
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.557
_refine_diff_density_min         -1.497
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.042(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         11830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0542
_reflns_number_gt                9732
_reflns_number_total             11830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja039551qsi20031111_080814.cif
_cod_data_source_block           rmt08
_cod_database_code               4112418