Hexakis(trialkylsilyl)cyclotrisilanes and photochemical generation of bis(trialkylsilyl)silylenes
Mitsuo Kira; Takeaki Iwamoto; Toyotaro Maruyama; Tsuyoshi Kuzuguchi; Dongzhu Yin; Chizuko Kabuto; Hideki Sakurai; J. Chem. Soc., Dalton Trans.  (2002) 1539–1544; doi:10.1039/b107905k

data_7011121
_publ_section_title
;
 Hexakis(trialkylsilyl)cyclotrisilanes and photochemical generation of
 bis(trialkylsilyl)silylenes
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1539
_journal_page_last               1544
_journal_paper_doi               10.1039/b107905k
_journal_year                    2002
_chemical_formula_sum            'C44 H100 Si9'
_chemical_formula_weight         882.05
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 123.9560(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.223(2)
_cell_length_b                   15.8148(18)
_cell_length_c                   11.7534(4)
_cell_measurement_reflns_used    5398
_cell_measurement_temperature    150.2
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      1.9
_cell_volume                     2809.6(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.2
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Rigaku/MSC Mercury 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  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13441
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         4.07
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.043
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.52(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         6579
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.6657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                5823
_reflns_number_total             6579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b107905k.txt
_cod_data_source_block           Hexasilylcyclotrisilane_1a
_cod_original_cell_volume        2809.7(5)
_cod_original_sg_symbol_H-M      C121
_cod_database_code               7011121