Axially Chiral Spirosilanes via Catalytic Asymmetric Intramolecular Hydrosilation
Kohei Tamao; Kazunori Nakamura; Hiroyuki Ishii; Shigehiro Yamaguchi; Motoo Shiro; Journal of the American Chemical Society 118 (1996) 12469–12470; doi:10.1021/ja962754c

data_4117216
_publ_contact_author             'Kohei Tamao'
_publ_contact_author_email       tamao@scl.kyoto-u.ac.jp
_publ_section_title
;
 Axially Chiral Spirosilanes via Catalytic Asymmetric Intramolecular
 Hydrosilation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12469
_journal_page_last               12470
_journal_paper_doi               10.1021/ja962754c
_journal_volume                  118
_journal_year                    1996
_chemical_formula_sum            'C14 H16 S2 Si'
_chemical_formula_weight         276.49
_chemical_melting_point          366(1)
_chemical_name_systematic
(4R,6S,6'S)-6,6'-Dimethyl-4,4'-spirobi(siloleno[3,2-b]thiophene)
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_date             'Fri Aug  9 00:43:53 1996'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 108.424(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4.00
_cell_length_a                   11.4251(8)
_cell_length_b                   8.0931(8)
_cell_length_c                   16.441(2)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    25.0
_cell_measurement_theta_max      59.88
_cell_measurement_theta_min      57.83
_cell_volume                     1442.3(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_publication_material  'teXsan: FINISH (MSC)'
_computing_structure_refinement  'teXsan: LS (MSC)'
_diffrn_ambient_temperature      25.0
_diffrn_measurement_device       AFC5R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      -0.02637
_diffrn_orient_matrix_UB_12      -0.08672
_diffrn_orient_matrix_UB_13      -0.01718
_diffrn_orient_matrix_UB_21      -0.02584
_diffrn_orient_matrix_UB_22      -0.01587
_diffrn_orient_matrix_UB_23      0.11978
_diffrn_orient_matrix_UB_31      -0.06267
_diffrn_orient_matrix_UB_32      0.00017
_diffrn_orient_matrix_UB_33      -0.01350
_diffrn_radiation_monochromator  filter
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           CuKalpha
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  3.19
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2402
_diffrn_reflns_theta_max         60.0483
_diffrn_standards_decay_%        -1.75
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu_cm 39.310
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             584.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         -0.20150
_refine_diff_density_min         0.20220
_refine_ls_extinction_coef       42.68782
_refine_ls_extinction_method     Zachariasen_type_2_gaussian_isotropic
_refine_ls_goodness_of_fit_obs   1.350
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         1423
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0330
_refine_ls_shift/esd_max         0.0150
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0460
_cod_data_source_file            ja962754c.cif
_cod_data_source_block           JA962754C-254
_cod_original_cell_volume        1442.3(2)
_cod_original_sg_symbol_H-M      'P 21 '
_cod_original_formula_sum        C14H16SiS2
_cod_database_code               4117216