Electron-Induced Conversion of Silylones to Six-Membered Cyclic Silylenes.
Roy, Sudipta; Mondal, Kartik Chandra; Krause, Lennard; Stollberg, Peter; Herbst-Irmer, Regine; Stalke, Dietmar; Meyer, Jann; Stückl, A Claudia; Maity, Bholanath; Koley, Debasis; Vasa, Suresh Kumar; Xiang, Sheng Qi; Linser, Rasmus; Roesky, Herbert W.; Journal of the American Chemical Society  (2014) 141119074807003–; doi:10.1021/ja510427r

data_4122967
_publ_section_title
;
 Electron-Induced Conversion of Silylones to Six-Membered Cyclic
 Silylenes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141119074807003
_journal_paper_doi               10.1021/ja510427r
_journal_year                    2014
_chemical_formula_moiety         'C46 H70 N2 Si'
_chemical_formula_sum            'C46 H70 N2 Si'
_chemical_formula_weight         679.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_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   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 93.00(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.533(2)
_cell_length_b                   18.139(2)
_cell_length_c                   22.863(3)
_cell_measurement_reflns_used    4898
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.0455
_cell_measurement_theta_min      2.2635
_cell_volume                     3948.0(11)
_computing_cell_refinement       'SAINT V8.30C'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V8.30C'
_computing_molecular_graphics    'Mercury CSD 3.3 (Build RC5)'
_computing_publication_material  'Mercury CSD 3.3 (Build RC5)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0870
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            61908
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         19.809
_diffrn_reflns_theta_min         1.663
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    0.057
_exptl_absorpt_correction_T_max  0.4249
_exptl_absorpt_correction_T_min  0.4004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/4
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+2.0326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5196
_reflns_number_total             7289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja510427r_si_003.cif
_cod_data_source_block           P21n_a
_cod_database_code               4122967
_shelx_estimated_absorpt_t_min   0.994
_shelx_estimated_absorpt_t_max   0.996
_shelxl_version_number           2014-3
_shelx_res_checksum              59324
_shelx_hkl_checksum              37196