Isolable Anion Radical of Blue Disilene (tBu2MeSi)2SiSi(SiMetBu2)2 Formed upon One-Electron Reduction: Synthesis and Characterization
Akira Sekiguchi; Shigeyoshi Inoue; Masaaki Ichinohe; Yoriko Arai; Journal of the American Chemical Society 126 (2004) 9626–9629; doi:10.1021/ja040079y

data_4112813
_publ_section_title
;
 Isolable Anion Radical of Blue Disilene (tBu2MeSi)2SiSi(SiMetBu2)2 Formed
 upon One-Electron Reduction: Synthesis and Characterization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9626
_journal_page_last               9629
_journal_paper_doi               10.1021/ja040079y
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C52 H116 Li O4 Si6'
_chemical_formula_weight         980.93
_chemical_name_systematic
;
  Tetrakis(tetrahydrofuran)lithium(I) 1,1,4,4-tetra-tert-butyl
  -2,3-Tetrakis[di-tert-butyl(methyl)silyl]-1,4-dimethyltetrasilane-2-yl-3-ide
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0720(3)
_cell_length_b                   21.5670(10)
_cell_length_c                   24.2500(11)
_cell_measurement_reflns_used    61161
_cell_measurement_temperature    200.0(1)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.07
_cell_volume                     6313.7(4)
_computing_cell_refinement       'HKL scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      200.0(1)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device       'MacScience DIP2030 Image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            61161
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.032
_exptl_crystal_description       Cube
_exptl_crystal_F_000             2188
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_coef       0.0076(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         7793
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.060
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+0.9517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1514
_reflns_number_gt                6308
_reflns_number_total             7793
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja040079y_s1_2.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               4112813