Utilization of industrial waste materials. Part 20. Stereoselective cycloaddition of silylenes and a disilene to an enantiomerically pure cyclic ketimine derived from an industrial waste material
von Keyserlingk, Nikolai Graf; Martens, Jürgen; Ostendorf, Detlev; Saak, Wolfgang; Weidenbruch, Manfred; Journal of the Chemical Society, Perkin Transactions 1  (2001) 706–; doi:10.1039/b008708o

data_7213449
_publ_section_title
;
 Utilization of industrial waste materials. Part 20. Stereoselective
 cycloaddition of silylenes and a disilene to an enantiomerically pure
 cyclic ketimine derived from an industrial waste material
;
_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              706
_journal_paper_doi               10.1039/b008708o
_journal_year                    2001
_chemical_formula_sum            'C36 H48 N2 Si'
_chemical_formula_weight         536.85
_space_group_IT_number           1
_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                96.862(8)
_cell_angle_beta                 100.249(7)
_cell_angle_gamma                100.163(7)
_cell_formula_units_Z            2
_cell_length_a                   9.7011(5)
_cell_length_b                   11.7040(8)
_cell_length_c                   14.5936(10)
_cell_measurement_temperature    193(2)
_cell_volume                     1585.37(19)
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_data_reduction        'XRED (Stoe, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Stoe IPDS'
_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  0.0722
_diffrn_reflns_av_sigmaI/netI    0.1461
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19376
_diffrn_reflns_theta_full        25.91
_diffrn_reflns_theta_max         25.91
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.9832
_exptl_absorpt_correction_T_min  0.9424
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       quader
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.792
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         11412
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.792
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.1025
_reflns_number_gt                5634
_reflns_number_total             11412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008708osup1.cif
_cod_data_source_block           sitimema
_cod_original_cell_volume        1585.37(17)
_cod_original_sg_symbol_H-M      P1
_cod_database_code               7213449