Control of up to Five Stereocenters in a Cascade Reaction: Synthesis of Highly Functionalized Five-Membered Rings
Hao Li; Teck-Peng Loh; Journal of the American Chemical Society 130 (2008) 7194–7195; doi:10.1021/ja801488z

data_4107878
_publ_section_title
;
 Control of up to Five Stereocenters in a Cascade Reaction: Synthesis of
 Highly Functionalized Five-Membered Rings
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7194
_journal_page_last               7195
_journal_paper_doi               10.1021/ja801488z
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C29 H49 Cl O3 Si'
_chemical_formula_sum            'C29 H49 Cl O3 Si'
_chemical_formula_weight         509.22
_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                105.455(2)
_cell_angle_beta                 109.497(2)
_cell_angle_gamma                98.896(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5848(4)
_cell_length_b                   10.8318(4)
_cell_length_c                   14.6865(5)
_cell_measurement_reflns_used    6120
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      2.12
_cell_volume                     1473.89(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20009
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.9525
_exptl_absorpt_correction_T_min  0.9433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         5712
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+0.6299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1794
_reflns_number_gt                4309
_reflns_number_total             5712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801488z-file002.cif
_cod_data_source_block           ltp66
_cod_original_cell_volume        1473.89(9)
_cod_database_code               4107878