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_4117617
_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        '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 H86 Si10'
_chemical_formula_sum            'C40 H86 Si10'
_chemical_formula_weight         847.99
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                63.7540(7)
_cell_angle_beta                 81.2453(6)
_cell_angle_gamma                74.1312(7)
_cell_formula_units_Z            1
_cell_length_a                   9.49590(10)
_cell_length_b                   12.18070(10)
_cell_length_c                   13.4345(2)
_cell_measurement_reflns_used    142504
_cell_measurement_temperature    100
_cell_measurement_theta_max      58.27
_cell_measurement_theta_min      1.92
_cell_volume                     1339.72(3)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'ORTEP-3 for Windows'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Rigaku AFC-10 with Saturn70 CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            121039
_diffrn_reflns_theta_full        50.00
_diffrn_reflns_theta_max         50.00
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.270
_exptl_absorpt_correction_T_max  0.93025
_exptl_absorpt_correction_T_min  0.91912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 MULABS - empirical Correction for Absorption Anisotropy.
 R. H. Blessing, Acta Crystallogr. 1995, A51, 33-38.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.051
_exptl_crystal_description       block
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.142
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         27219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+0.1012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1114
_reflns_number_gt                22732
_reflns_number_total             27219
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja300694p_si_003.cif
_cod_data_source_block           Disilane
_cod_database_code               4117617