From Si(II) to Si(IV) and Back: Reversible Intramolecular Carbon-Carbon Bond Activation by an Acyclic Iminosilylene.
Wendel, Daniel; Porzelt, Amelie; Herz, Fabian A. D.; Sarkar, Debotra; Jandl, Christian; Inoue, Shigeyoshi; Rieger, Bernhard; Journal of the American Chemical Society 139 (2017) 8134–8137; doi:10.1021/jacs.7b05136

data_4131415
_publ_section_title
;
 From Si(II) to Si(IV) and Back: Reversible Intramolecular Carbon-Carbon
 Bond Activation by an Acyclic Iminosilylene.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8134
_journal_page_last               8137
_journal_paper_doi               10.1021/jacs.7b05136
_journal_volume                  139
_journal_year                    2017
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C36 H63 N3 Si5'
_chemical_formula_sum            'C36 H63 N3 Si5'
_chemical_formula_weight         678.34
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                77.90(2)
_cell_angle_beta                 88.71(4)
_cell_angle_gamma                89.63(3)
_cell_formula_units_Z            4
_cell_length_a                   12.015(17)
_cell_length_b                   16.37(2)
_cell_length_c                   22.31(3)
_cell_measurement_reflns_used    9466
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.0604
_cell_measurement_theta_min      2.4047
_cell_volume                     4289(10)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX III Control Software (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'
_computing_structure_refinement
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 ' CMOS plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker Photon CMOS '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  'Helios optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'IMS microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            185048
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5, Bruker, 2014'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.116
_platon_squeeze_details
;
The unit cell contains 2 disordered molecules of benzene on special positions
which were treated as a diffuse contribution to the overall scattering without
specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.850
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         15686
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0975
_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^)+(0.0745P)^2^+27.1114P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2348
_refine_ls_wR_factor_ref         0.2445
_reflns_number_gt                13200
_reflns_number_total             15686
_reflns_threshold_expression     i>2\s(i)
_cod_data_source_file            ja7b05136_si_002.cif
_cod_data_source_block           compound_2
_cod_original_cell_volume        4290(10)
_cod_database_code               4131415
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              20567
_shelx_hkl_checksum              54271
_shelx_fab_checksum              62874