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_4108709
_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            'C25 H36 Cl5 F3 N2 O Pd'
_chemical_formula_weight         721.21
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.5410(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8633(3)
_cell_length_b                   13.4427(3)
_cell_length_c                   15.0189(3)
_cell_measurement_reflns_used    30297
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.68
_cell_measurement_theta_min      2.35
_cell_volume                     2967.54(11)
_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 0.937
_diffrn_measured_fraction_theta_max 0.937
_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  0.0654
_diffrn_reflns_av_sigmaI/netI    0.1028
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            79009
_diffrn_reflns_theta_full        40.44
_diffrn_reflns_theta_max         40.44
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  0.7600
_exptl_absorpt_correction_T_min  0.7094
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       Block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.26
_refine_diff_density_max         2.072
_refine_diff_density_min         -1.257
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.036(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     667
_refine_ls_number_reflns         33021
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.003
_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          0.0608
_refine_ls_wR_factor_ref         0.0669
_reflns_number_gt                21505
_reflns_number_total             33021
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja804955e_si_005.cif
_cod_data_source_block           rmt07
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_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               4108709