Reactivity of the Disilyne RSiSiR (R = SiiPr[CH(SiMe3)2]2) toward Nitriles: Unexpected Formation of Triaza-1,4-disilabicyclo[2.2.2]octa-2,5,7-triene Derivatives
Takeuchi, Katsuhiko; Ichinohe, Masaaki; Sekiguchi, Akira; Guo, Jing-Dong; Nagase, Shigeru; Organometallics 28 (2009) 2658–; doi:10.1021/om900164h

data_4069378
_publ_section_title
;
 Reactivity of the Disilyne RSi&#xE5FC;SiR (R = SiiPr[CH(SiMe3)2]2) toward
 Nitriles: Unexpected Formation of
 Triaza-1,4-disilabicyclo[2.2.2]octa-2,5,7-triene Derivatives
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2658
_journal_paper_doi               10.1021/om900164h
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C65.5 H117 N3 Si12'
_chemical_formula_weight         1283.70
_chemical_name_systematic
; 
 1,2-Bis{bis[bis(trimethylsilyl)methyl]isopropylsilyl}-
 3,5,8-triphenyl-2,6,7-triaza-1,4-disila-
 bicyclo[2.2.2]oct-2,5,7-triene 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.498(2)
_cell_angle_beta                 79.296(3)
_cell_angle_gamma                75.670(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9370(6)
_cell_length_b                   18.2680(9)
_cell_length_c                   20.0380(7)
_cell_measurement_reflns_used    41143
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.12
_cell_volume                     3891.0(3)
_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 0.913
_diffrn_measured_fraction_theta_max 0.913
_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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.1051
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41143
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1398
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0051(4)
_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   0.888
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         17194
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                10110
_reflns_number_total             17194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900164h_si_001.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1          '
_cod_original_formula_sum        'C65.50 H117 N3 Si12'
_cod_database_code               4069378