Structural Features and Reactivity of (Sparteine)PdCl2: A Model for Selectivity in the Oxidative Kinetic Resolution of Secondary Alcohols
Raissa M. Trend; Brian M. Stoltz; Journal of the American Chemical Society 130 (2008) 15957–15966; doi:10.1021/ja804955e

data_4108706
_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
;
 Structural Features and Reactivity of (Sparteine)PdCl2: A Model for
 Selectivity in the Oxidative Kinetic Resolution of Secondary Alcohols
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15957
_journal_page_last               15966
_journal_paper_doi               10.1021/ja804955e
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C20 H31 Cl F6 N3 Pd Sb'
_chemical_formula_weight         691.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'Patterson method'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.3020(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3598(2)
_cell_length_b                   22.2422(3)
_cell_length_c                   10.8117(2)
_cell_measurement_reflns_used    54240
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.64
_cell_measurement_theta_min      2.19
_cell_volume                     2414.07(7)
_computing_cell_refinement       'Bruker SAINT v6.022'
_computing_data_collection       'Bruker SMART v5.054'
_computing_data_reduction        'Bruker SAINT v6.022'
_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 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       '\w scans at 7 \f and 2 2\q settings'
_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  0.0717
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            110239
_diffrn_reflns_theta_full        40.92
_diffrn_reflns_theta_max         40.92
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    2.034
_exptl_absorpt_correction_T_max  0.6986
_exptl_absorpt_correction_T_min  0.6520
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_description       Block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         5.743
_refine_diff_density_min         -4.948
_refine_diff_density_rms         0.187
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.018(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.664
_refine_ls_hydrogen_treatment    Constrained
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     577
_refine_ls_number_reflns         29947
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.664
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/s^2^(Fo^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0864
_reflns_number_gt                22793
_reflns_number_total             29947
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja804955e_si_002.cif
_cod_data_source_block           rmt03
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Geometric positions' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4108706