A New Disilene with π-Accepting Groups from the Reaction of Disilyne RSi\τbSiR (R = SiiPr[CH(SiMe3)2]) with Isocyanides
Katsuhiko Takeuchi; Masaaki Ichinohe; Akira Sekiguchi; Journal of the American Chemical Society 134 (2012) 2954–2957; doi:10.1021/ja212065a

data_4117494
_publ_section_title
;
 A New Disilene with \p-Accepting Groups from the Reaction of Disilyne
 RSi\\tbSiR (R = SiiPr[CH(SiMe3)2]) with Isocyanides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2954
_journal_page_last               2957
_journal_paper_doi               10.1021/ja212065a
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C49 H120 N2 Si12'
_chemical_formula_weight         1074.55
_chemical_name_systematic
; 
 1,1,4,4-Tetrakis[bis(trimethylsilyl)methyl]-2,3-bis(tert-butyliminomethylene)- 
 1,4-diisopropyltetrasilane 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.13
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0491(4)
_cell_length_b                   13.3708(4)
_cell_length_c                   40.9566(13)
_cell_measurement_reflns_used    9175
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.18
_cell_volume                     7141.0(4)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            39997
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_T_max  0.9682
_exptl_absorpt_correction_T_min  0.9183
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
SADABS Sheldrick 1996 
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    0.999
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.395
_refine_diff_density_min         -1.184
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.0011(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   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         16347
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.318
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          2.341
_refine_ls_shift/su_mean         0.042
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1130P)^2^+9.4206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2113
_refine_ls_wR_factor_ref         0.2325
_reflns_number_gt                11695
_reflns_number_total             16347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja212065a_si_001.cif
_cod_data_source_block           tbuncadd_0m
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4117494