Reactivity of the Disilyne RSi\τbSiR (R = SiiPr[CH(SiMe3)2]2) toward Silylcyanide: Two Pathways To Form the Bis-Adduct [RSiSiR(CNSiMe3)2] with Some Silaketenimine Character and a 1,4-Diaza-2,3-disilabenzene Analogue
Katsuhiko Takeuchi; Masaaki Ichinohe; Akira Sekiguchi; Journal of the American Chemical Society 130 (2008) 16848–16849; doi:10.1021/ja807974a

data_4108851
_publ_section_title
;
 Reactivity of the Disilyne RSi\\tbSiR (R = SiiPr[CH(SiMe3)2]2) toward
 Silylcyanide: Two Pathways To Form the Bis-Adduct [RSiSiR(CNSiMe3)2] with
 Some Silaketenimine Character and a 1,4-Diaza-2,3-disilabenzene Analogue
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16848
_journal_page_last               16849
_journal_paper_doi               10.1021/ja807974a
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C42 H108 N2 Si14'
_chemical_formula_weight         1034.56
_chemical_name_systematic
; 
 1,1,4,4-Tetrakis[bis(trimethylsilyl)methyl]-1,4-diisopropyl-2-tetrasilyne
 bis(trimethysilylisocyanide) complex
;
_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                 101.8650(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5160(2)
_cell_length_b                   20.9880(4)
_cell_length_c                   18.3770(3)
_cell_measurement_reflns_used    68740
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.05
_cell_volume                     6611.52(18)
_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      150.0(1)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            68740
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Ruby
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.0097(5)
_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   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         15800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0783P)^2^+5.7059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                13402
_reflns_number_total             15800
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja807974a_si_001.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4108851