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_7213448
_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 H66 N2 Si3'
_chemical_formula_weight         611.18
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 105.905(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.2381(15)
_cell_length_b                   9.2920(3)
_cell_length_c                   16.1808(10)
_cell_measurement_temperature    193(2)
_cell_volume                     3793.9(4)
_computing_cell_refinement       'IPDS (Stoe, 1997)'
_computing_data_collection       'IPDS (Stoe, 1997)'
_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 0.937
_diffrn_measured_fraction_theta_max 0.937
_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  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14144
_diffrn_reflns_theta_full        25.95
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_T_max  0.9822
_exptl_absorpt_correction_T_min  0.8996
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       quader
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6894
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0459P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0854
_reflns_number_gt                5698
_reflns_number_total             6894
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008708osup1.cif
_cod_data_source_block           sitbuma
_cod_original_cell_volume        3793.9(3)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               7213448