Amine-Promoted Disproportionation and Redistribution of Trichlorosilane: Formation of Tetradecachlorocyclohexasilane Dianion1
Seok-Bong Choi; Beon-Kyu Kim; Philip Boudjouk; Dean G. Grier; Journal of the American Chemical Society 123 (2001) 8117–8118; doi:10.1021/ja002831a

data_4115650
_publ_section_title
;
 Amine-Promoted Disproportionation and Redistribution of Trichlorosilane:
 Formation of Tetradecachlorocyclohexasilane Dianion1
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8117
_journal_page_last               8118
_journal_paper_doi               10.1021/ja002831a
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C28 H70 Cl16 N6 Si8'
_chemical_formula_weight         1282.82
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_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.7106(18)
_cell_length_b                   22.1508(19)
_cell_length_c                   27.130(2)
_cell_measurement_temperature    295(2)
_cell_volume                     11845.1(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            57160
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.933
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_F_000             5312
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         10437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1329
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+17.4639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     >2sigma(I)
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