Photochemical and Thermal Reactions of a Kinetically Stabilized 9-Silaanthracene: The First Spectroscopic Observation of a 9,10-Dewar-9-silaanthracene Isomer
Akihiro Shinohara; Nobuhiro Takeda; Norihiro Tokitoh; Journal of the American Chemical Society 125 (2003) 10804–10805; doi:10.1021/ja036106m

data_4114138
_publ_contact_author_address
;
    Institute for Chemical Research, Kyoto University, Gokasho, Uji, 
    Kyoto 611-0011, Japan. 
;
_publ_contact_author_email       ' tokitoh@boc.kuicr.kyoto-u.ac.jp'
_publ_contact_author_fax         ' +81-774-38-3209 '
_publ_contact_author_name        'Norihiro Tokitoh'
_publ_contact_author_phone       ' +81-774-38-3200 '
_publ_section_title
;
 Photochemical and Thermal Reactions of a Kinetically Stabilized
 9-Silaanthracene: The First Spectroscopic Observation of a
 9,10-Dewar-9-silaanthracene Isomer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10804
_journal_page_last               10805
_journal_paper_doi               10.1021/ja036106m
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C80 H136 Si14, C6 H14'
_chemical_formula_sum            'C86 H150 Si14'
_chemical_formula_weight         1577.32
_chemical_melting_point          583
_chemical_name_common            '9-silaanthracene dimer'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'May 13 2003'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.422(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.155(6)
_cell_length_b                   22.181(11)
_cell_length_c                   18.561(10)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3.03
_cell_volume                     4748(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'RIGAKU/MSC Meacury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0861
_diffrn_reflns_av_sigmaI/netI    0.0987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28729
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.9775
_exptl_absorpt_correction_T_min  0.9346
_exptl_absorpt_correction_type   empilical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_description       prisum
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.223
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         8321
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0808
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+8.2793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1712
_reflns_number_gt                7327
_reflns_number_total             8321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja036106msi20030513_042423.cif
_cod_data_source_block           dimer
_cod_database_code               4114138