Kinetic resolution of donor-functionalised tertiary alcohols by Cu–H-catalysed stereoselective silylation using a strained silicon-stereogenic silane
Karatas, Betül; Rendler, Sebastian; Fröhlich, Roland; Oestreich, Martin; Organic & Biomolecular Chemistry 6 (2008) 1435–1440; doi:10.1039/b802186d

data_7150901
_publ_section_title
;
 Kinetic resolution of donor-functionalised tertiary alcohols by
 Cu--H-catalysed stereoselective silylation using a strained
 silicon-stereogenic silane
;
_journal_issue                   8
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              1435
_journal_page_last               1440
_journal_paper_doi               10.1039/b802186d
_journal_volume                  6
_journal_year                    2008
_chemical_formula_sum            'C31 H39 N O2 Si2'
_chemical_formula_weight         513.81
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.885(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.6545(4)
_cell_length_b                   21.6938(6)
_cell_length_c                   19.1708(5)
_cell_measurement_reflns_used    14170
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     5964.0(3)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SCHAKAL (Keller, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \ 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  0.068
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            55533
_diffrn_reflns_theta_full        68.00
_diffrn_reflns_theta_max         68.00
_diffrn_reflns_theta_min         3.69
_exptl_absorpt_coefficient_mu    1.279
_exptl_absorpt_correction_T_max  0.7840
_exptl_absorpt_correction_T_min  0.7003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         10655
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0522P)^2^+3.9486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1384
_reflns_number_gt                8195
_reflns_number_total             10655
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b802186d.txt
_cod_data_source_block           ost4341
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7150901