Unexpected Reaction of an Overcrowded 9,10-Dihydroanthrylchlorosilane Leading to the Formation of a Dibenzo-7-silanorbornadiene Derivative
Sasamori, Takahiro; Ozaki, Shuhei; Tokitoh, Norihiro; Chemistry Letters 36 (2007) 588–; doi:10.1246/cl.2007.588

data_8000165
_publ_section_title
;
 Unexpected Reaction of an Overcrowded 9,10-Dihydroanthrylchlorosilane
 Leading to the Formation of a Dibenzo-7-silanorbornadiene Derivative
;
_journal_issue                   5
_journal_name_full               'Chemistry Letters'
_journal_page_first              588
_journal_paper_doi               10.1246/cl.2007.588
_journal_volume                  36
_journal_year                    2007
_chemical_formula_moiety         'C41 H70 Si7'
_chemical_formula_sum            'C41 H70 Si7'
_chemical_formula_weight         759.60
_chemical_name_common            dibenzo-7-silanorbornadiene
_chemical_name_systematic
; 
 dibenzo-7-silanorbornadiene 
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-08-18
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.369(5)
_cell_angle_beta                 92.3857(1)
_cell_angle_gamma                115.551(4)
_cell_formula_units_Z            2
_cell_length_a                   12.6722(12)
_cell_length_b                   14.2473(19)
_cell_length_c                   14.8856(13)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      3.43
_cell_volume                     2363.5(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Rigaku Mercury'
_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  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20008
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.43
_exptl_absorpt_coefficient_mu    0.227
_exptl_absorpt_correction_T_max  0.9350
_exptl_absorpt_correction_T_min  0.9146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         8664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0511P)^2^+0.9390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                7946
_reflns_number_total             8664
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            36-588sup1.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        2363.4(4)
_cod_original_sg_symbol_Hall     '    -P 1'
_cod_database_code               8000165