Twist of a Silicon-Silicon Double Bond: Selective Anti-Addition of Hydrogen to an Iminodisilene.
Wendel, Daniel; Szilvási, Tibor; Jandl, Christian; Inoue, Shigeyoshi; Rieger, Bernhard; Journal of the American Chemical Society 139 (2017) 9156–9159; doi:10.1021/jacs.7b05335

data_4131429
_publ_section_title
;
 Twist of a Silicon-Silicon Double Bond: Selective Anti-Addition of
 Hydrogen to an Iminodisilene.
;
_journal_issue                   27
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9156
_journal_page_last               9159
_journal_paper_doi               10.1021/jacs.7b05335
_journal_volume                  139
_journal_year                    2017
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C40 H96 N6 Si10'
_chemical_formula_sum            'C40 H96 N6 Si10'
_chemical_formula_weight         942.13
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 113.931(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3289(13)
_cell_length_b                   13.9624(9)
_cell_length_c                   22.7699(16)
_cell_measurement_reflns_used    9725
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.0769
_cell_measurement_theta_min      2.6025
_cell_volume                     5907.4(7)
_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 0.999
_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  0.0459
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            87418
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5, Bruker, 2014'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.519
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.158
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         11190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0054P)^2^+7.4860P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0864
_reflns_number_gt                9950
_reflns_number_total             11190
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja7b05335_si_002.cif
_cod_data_source_block           compound_3a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4131429
_shelx_res_checksum              57989
_shelx_hkl_checksum              57340