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_4112812
_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            'C36 H84 Si6'
_chemical_formula_weight         685.57
_chemical_name_systematic
;
  Tetrakis[di-tert-butyl(methyl)silyl] disilene
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.783(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.702(1)
_cell_length_b                   11.470(1)
_cell_length_c                   18.3010(9)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.89
_cell_measurement_theta_min      2.10
_cell_volume                     4539.7(5)
_computing_cell_refinement       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      295
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device       'MacScience DIP2030 Image plate'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.00247
_diffrn_orient_matrix_UB_12      0.05013
_diffrn_orient_matrix_UB_13      0.02198
_diffrn_orient_matrix_UB_21      -0.00106
_diffrn_orient_matrix_UB_22      -0.03493
_diffrn_orient_matrix_UB_23      0.07980
_diffrn_orient_matrix_UB_31      0.04622
_diffrn_orient_matrix_UB_32      0.00143
_diffrn_orient_matrix_UB_33      0.00124
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1177
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10848
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.205
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.003
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.400
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0046(7)
_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   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         10337
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1673
_refine_ls_R_factor_gt           0.0877
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1069P)^2^+11.1422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2077
_refine_ls_wR_factor_ref         0.2560
_reflns_number_gt                5694
_reflns_number_total             10337
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja040079y_s1_1.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        4539.7(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4112812