Application of the sila-Friedel-Crafts reaction to the synthesis of π-extended silole derivatives and their properties.
Furukawa, Shunsuke; Kobayashi, Junji; Kawashima, Takayuki; Dalton transactions (Cambridge, England : 2003) 39 (2010) 9329–9336; doi:10.1039/c0dt00136h

data_7030410
_publ_section_title
;
 Application of the sila-Friedel-Crafts reaction to the synthesis of
 \p-extended silole derivatives and their properties.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9329
_journal_page_last               9336
_journal_paper_doi               10.1039/c0dt00136h
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C78 H84 O6 Si3'
_chemical_formula_weight         1201.72
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0000(14)
_cell_angle_beta                 102.6957(16)
_cell_angle_gamma                90.0000(14)
_cell_formula_units_Z            8
_cell_length_a                   27.695(8)
_cell_length_b                   15.054(5)
_cell_length_c                   32.739(11)
_cell_measurement_reflns_used    22060
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0402
_cell_volume                     13316(7)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 14.5666
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device
;
Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0956
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            59312
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           40.0000
_diffrn_source_power             2.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  0.9755
_exptl_absorpt_correction_T_min  0.9755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R. (1998), Rigaku, Private communication
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5136
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         5.742
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.593
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1570
_refine_ls_number_reflns         22060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.593
_refine_ls_R_factor_all          0.1983
_refine_ls_R_factor_gt           0.1509
_refine_ls_shift/su_max          0.773
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3891
_refine_ls_wR_factor_ref         0.4583
_reflns_number_gt                12809
_reflns_number_total             22060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00136h.txt
_cod_data_source_block           si3triph4
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               7030410