High Yield Access to Silylene RSiCl (R = PhC(NtBu)2) and Its Reactivity toward Alkyne: Synthesis of Stable Disilacyclobutene
Sakya S. Sen; Herbert W. Roesky; Daniel Stern; Julian Henn; Dietmar Stalke; Journal of the American Chemical Society 132 (2010) 1123–1126; doi:10.1021/ja9091374

data_4101820
_publ_section_title
;
 High Yield Access to Silylene RSiCl (R = PhC(NtBu)2) and Its Reactivity
 toward Alkyne: Synthesis of Stable Disilacyclobutene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1123
_journal_page_last               1126
_journal_paper_doi               10.1021/ja9091374
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C44 H56 Cl2 N4 Si2'
_chemical_formula_sum            'C44 H56 Cl2 N4 Si2'
_chemical_formula_weight         768.01
_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                 94.5010(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1830(4)
_cell_length_b                   13.2275(4)
_cell_length_c                   24.4548(8)
_cell_measurement_reflns_used    9702
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.267
_cell_measurement_theta_min      2.188
_cell_volume                     4251.2(2)
_computing_cell_refinement       'SAINT V7.46A (Bruker, 2008)'
_computing_data_collection       'APEX2 v2.2-0 (Bruker, 2008)'
_computing_data_reduction        'SAINT V7.46A (Bruker, 2008)'
_computing_molecular_graphics    'XSHELL v4.01 (Bruker, 2000)'
_computing_publication_material  'XSHELL v4.01 (Bruker, 2000)'
_computing_structure_refinement  'XL in SHELXTL v2008/2(Sheldrick, 2008)'
_computing_structure_solution    'XS in SHELXTL v2008/2(Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX2 with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'Quazar multilayer mirror optics'
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            287828
_diffrn_reflns_theta_full        39.39
_diffrn_reflns_theta_max         39.39
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.6657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/2 (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         25354
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+1.5989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                21202
_reflns_number_total             25354
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9091374_si_002.cif
_cod_data_source_block           p21c
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4101820