Formation of a Donor-Stabilized Tetrasilacyclobutadiene Dication by a Lewis Acid Assisted Reaction of an N-Heterocyclic Chloro Silylene
Shigeyoshi Inoue; Jan D. Epping; Elisabeth Irran; Matthias Driess; Journal of the American Chemical Society 133 (2011) 8514–8517; doi:10.1021/ja2033475

data_4106225
_publ_section_title
;
 Formation of a Donor-Stabilized Tetrasilacyclobutadiene Dication by a
 Lewis Acid Assisted Reaction of an N-Heterocyclic Chloro Silylene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8514
_journal_page_last               8517
_journal_paper_doi               10.1021/ja2033475
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety
'C60 H92 Cl2 N8 Si6, 2(C20 H30 Cl7 Zr2), 2(C6 H6)'
_chemical_formula_sum            'C112 H164 Cl16 N8 Si6 Zr4'
_chemical_formula_weight         2723.13
_chemical_name_systematic
; 
 ? 
;
_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
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.835(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4280(5)
_cell_length_b                   16.2309(6)
_cell_length_c                   32.2578(14)
_cell_measurement_reflns_used    4969
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.3608
_cell_measurement_theta_min      3.2429
_cell_volume                     6429.8(5)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_sigmaI/netI    0.1740
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            24733
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.9220
_exptl_absorpt_correction_T_min  0.7384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       plate
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.826
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     778
_refine_ls_number_reflns         11303
_refine_ls_number_restraints     374
_refine_ls_restrained_S_all      0.818
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0229P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                6190
_reflns_number_total             11303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2033475_si_002.cif
_cod_data_source_block           inou24
_cod_original_cell_volume        6429.8(4)
_cod_database_code               4106225