"Super Silyl" Group for Diastereoselective Sequential Reactions: Access to Complex Chiral Architecture in One Pot
Matthew B. Boxer; Hisashi Yamamoto; Journal of the American Chemical Society 129 (2007) 2762–2763; doi:10.1021/ja0693542

data_4109159
_publ_section_title
;
 "Super Silyl" Group for Diastereoselective Sequential Reactions: Access
 to Complex Chiral Architecture in One Pot
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2762
_journal_page_last               2763
_journal_paper_doi               10.1021/ja0693542
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C31 H76 O3 Si8'
_chemical_formula_weight         721.64
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 109.02(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.130(2)
_cell_length_b                   17.035(3)
_cell_length_c                   27.695(7)
_cell_measurement_temperature    293(2)
_cell_volume                     4518.3(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14174
_diffrn_reflns_theta_full        13.30
_diffrn_reflns_theta_max         13.30
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.9986
_exptl_absorpt_correction_T_min  0.9917
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         6437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0463P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                4808
_reflns_number_total             6437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0693542si20070105_052257.cif
_cod_data_source_block           cmc0493
_cod_original_cell_volume        4518.3(17)
_cod_database_code               4109159