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_7150902
_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 O Si2'
_chemical_formula_weight         497.81
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.213(2)
_cell_angle_beta                 81.203(2)
_cell_angle_gamma                61.845(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2158(3)
_cell_length_b                   10.5173(3)
_cell_length_c                   16.3911(5)
_cell_measurement_reflns_used    4711
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     1478.42(9)
_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 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\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  0.038
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18283
_diffrn_reflns_theta_full        68.09
_diffrn_reflns_theta_max         68.09
_diffrn_reflns_theta_min         4.91
_exptl_absorpt_coefficient_mu    1.249
_exptl_absorpt_correction_T_max  0.7883
_exptl_absorpt_correction_T_min  0.7058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0622P)^2^+0.5404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                4699
_reflns_number_total             5176
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b802186d.txt
_cod_data_source_block           ost4347
_cod_original_cell_volume        1478.42(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7150902