Facile Conversion of Bis-Silylene to Cyclic Silylene Isomers: Unexpected C-N and C-H Bond Cleavage.
Wang, Yuzhong; Hickox, Hunter P.; Xie, Yaoming; Wei, Pingrong; Schaefer, Henry F.; Robinson, Gregory H.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b10325

data_4126693
_publ_section_title
;
 Facile Conversion of Bis-Silylene to Cyclic Silylene Isomers: Unexpected
 C-N and C-H Bond Cleavage.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b10325
_journal_year                    2017
_chemical_formula_sum            'C95 H122 N6 S4 Si2'
_chemical_formula_weight         1532.40
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
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_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7211(15)
_cell_length_b                   27.855(2)
_cell_length_c                   18.2418(16)
_cell_measurement_reflns_used    9756
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.35
_cell_volume                     8993.4(13)
_computing_cell_refinement       'Bruker SAINT'
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_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest PHOTON 100 CMOS'
_diffrn_measurement_method       'Phi\Omega scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
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_diffrn_reflns_limit_k_max       33
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_diffrn_reflns_limit_l_min       -21
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_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
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_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.141
_diffrn_source                   Imus
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            colorless
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_exptl_crystal_description       plate
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_exptl_crystal_size_min          0.120
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     998
_refine_ls_number_reflns         16265
_refine_ls_number_restraints     205
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0857P)^2^+13.8780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.1883
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_reflns_number_gt                12920
_reflns_number_total             16265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10325_si_003.cif
_cod_data_source_block           j1_a
_cod_original_cell_volume        8993.6(13)
_cod_database_code               4126693
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              32550
_shelx_hkl_checksum              22943