Synthesis of Kinetically Stabilized 1,2-Dihydrodisilenes
Tomohiro Agou; Yusuke Sugiyama; Takahiro Sasamori; Heisuke Sakai; Yukio Furukawa; Nozomi Takagi; Jing-Dong Guo; Shigeru Nagase; Daisuke Hashizume; Norihiro Tokitoh; Journal of the American Chemical Society 134 (2012) 4120–4123; doi:10.1021/ja300694p

data_4117618
_publ_contact_author_address
;Institute for Chemical Resarch,
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        'Tokitoh, Norihiro'
_publ_contact_author_phone       +81-774-38-3200
_publ_section_title
;
 Synthesis of Kinetically Stabilized 1,2-Dihydrodisilenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4120
_journal_page_last               4123
_journal_paper_doi               10.1021/ja300694p
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C40 H84 Si10'
_chemical_formula_sum            'C40 H84 Si10'
_chemical_formula_weight         845.97
_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_method           SHELXL-97
_cell_angle_alpha                73.449(10)
_cell_angle_beta                 76.985(10)
_cell_angle_gamma                65.272(8)
_cell_formula_units_Z            2
_cell_length_a                   12.692(3)
_cell_length_b                   12.756(2)
_cell_length_c                   19.255(4)
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.78
_cell_volume                     2694.0(10)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_molecular_graphics
;
Yadokari-XG 2009 (Wakita Nemoto et al., 2009)
;
_computing_publication_material
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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     0.71075
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26694
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.9239
_exptl_absorpt_correction_T_min  0.8776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.043
_exptl_crystal_description       prism
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         12150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0644P)^2^+0.7015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1205
_reflns_number_gt                10478
_reflns_number_total             12150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja300694p_si_004.cif
_cod_data_source_block           100401
_cod_original_cell_volume        2694.1(9)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               4117618