Hexamethyldisilazanes mediated one-pot intramolecular Michael addition–olefination reactions leading to exo-olefinated bicyclo[6.4.0]dodecanes
Fujishima, Hiroshi; Takeshita, Hiroshi; Suzuki, Shuichi; Toyota, Masahiro; Ihara, Masataka; Journal of the Chemical Society, Perkin Transactions 1  (1999) 2609–; doi:10.1039/a904484a

data_7213127
_publ_contact_author
;
    ENTER NAME
 ENTER ADDRESS
;
_publ_section_title
;
 Hexamethyldisilazanes mediated one-pot intramolecular Michael
 addition--olefination reactions leading to exo-olefinated
 bicyclo[6.4.0]dodecanes
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2609
_journal_paper_doi               10.1039/a904484a
_journal_year                    1999
_chemical_formula_moiety         'C27 H42 O4 S Si '
_chemical_formula_sum            'C27 H42 O4 S Si'
_chemical_formula_weight         490.77
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_date             'Tue Jun 10 10:37:25 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90.00(2)
_cell_angle_beta                 97.02(2)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   15.048(4)
_cell_length_b                   11.327(3)
_cell_length_c                   16.988(4)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    286.2
_cell_measurement_theta_max      22.8
_cell_measurement_theta_min      20.1
_cell_volume                     2873.9(13)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      286.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.00282
_diffrn_orient_matrix_UB_12      -0.04587
_diffrn_orient_matrix_UB_13      -0.05054
_diffrn_orient_matrix_UB_21      0.04993
_diffrn_orient_matrix_UB_22      0.04875
_diffrn_orient_matrix_UB_23      -0.01654
_diffrn_orient_matrix_UB_31      0.04452
_diffrn_orient_matrix_UB_32      -0.05757
_diffrn_orient_matrix_UB_33      0.02626
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
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_diffrn_reflns_av_R_equivalents  4.99
_diffrn_reflns_av_sigmaI/netI    0.068
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5248
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         64.09
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        -5.78
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.617
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   '\DF (DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_density_meas      1.000
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1064.00
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.20
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   3.008
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     340
_refine_ls_number_reflns         2964
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0631
_refine_ls_shift/esd_max         1.8690
_refine_ls_shift/esd_mean        0.1090
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0634
_reflns_number_observed          2964
_reflns_number_total             5032
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            904484asup1.cif
_cod_data_source_block           ihara971
_cod_original_cell_volume        2873(1)
_cod_original_sg_symbol_H-M      'P 21/a     '
_cod_original_formula_sum        'C27 H42 O4 S Si '
_cod_database_code               7213127