1,4-Disila(Dewar-benzene) and 1,4-Disilabenzene: Valence Isomerization of Bis(alkylsilacyclopropenyl)s
Yoshio Kabe; Kenichi Ohkubo; Hitomi Ishikawa; Wataru Ando; Journal of the American Chemical Society 122 (2000) 3775–3776; doi:10.1021/ja9930061

data_4115974
_publ_contact_author_address
;
    Department of chemistry
    University of Tsukuba
    Tsukuba Ibaraki 305-8571
    Japan
;
_publ_contact_author_email       ' kabe@staff.chem.tsukuba.ac.jp '
_publ_contact_author_fax         ' 81 298 53 6503 '
_publ_contact_author_name        ' Yoshio Kabe'
_publ_contact_author_phone       ' 81 298 53 4207 '
_publ_section_title
;
 1,4-Disila(Dewar-benzene) and 1,4-Disilabenzene: Valence Isomerization of
 Bis(alkylsilacyclopropenyl)s
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3775
_journal_page_last               3776
_journal_paper_doi               10.1021/ja9930061
_journal_volume                  122
_journal_year                    2000
_chemical_formula_moiety         'C18 H42 O Si6 '
_chemical_formula_sum            'C18 H42 O Si6'
_chemical_formula_weight         443.04
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                103.671(6)
_cell_angle_beta                 92.809(7)
_cell_angle_gamma                111.622(7)
_cell_formula_units_Z            2
_cell_length_a                   10.1856(10)
_cell_length_b                   12.0125(8)
_cell_length_c                   13.0143(10)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      9.0
_cell_volume                     1422.0(2)
_computing_cell_refinement       'Enraf-Nonius CAD4 Diffractometer Control'
_computing_data_collection       'Enraf-Nonius CAD4 Diffractometer Control'
_computing_data_reduction        'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'teXsan for Windows (MSC, 1997)'
_computing_structure_solution
;
SIR97 (Altomare, et. al. 1997)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.01734
_diffrn_orient_matrix_UB_12      -0.08067
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_diffrn_orient_matrix_UB_21      0.03841
_diffrn_orient_matrix_UB_22      0.04589
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_diffrn_orient_matrix_UB_31      -0.09816
_diffrn_orient_matrix_UB_32      -0.00747
_diffrn_orient_matrix_UB_33      0.01394
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.00000
_diffrn_reflns_av_sigmaI/netI    0.067
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5293
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         18.81
_diffrn_standards_decay_%        -10.94
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.299
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.997
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.035
_exptl_crystal_description       none
_exptl_crystal_F_000             484.00
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.31
_refine_ls_extinction_coef       0.00000331(12)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   3.282
_refine_ls_goodness_of_fit_ref   3.280
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3207
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.0200
_refine_ls_shift/su_mean         0.0021
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     '\w = 1/[\s^2^(Fo) + 0.00005|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0640
_refine_ls_wR_factor_ref         0.0640
_reflns_number_gt                3207
_reflns_number_total             4985
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ja9930061_1.cif
_cod_data_source_block           '_Disila(Dewar-benzene)oxid(5a)'
_cod_original_cell_volume        1422.0(3)
_cod_original_formula_sum        'C18 H42 O Si6 '
_cod_database_code               4115974