Oxidative Addition of Ammonia at a Silicon(II) Center and an Unprecedented Hydrogenation Reaction of Compounds with Low-Valent Group 14 Elements Using Ammonia Borane
Anukul Jana; Carola Schulzke; Herbert W. Roesky; Journal of the American Chemical Society 131 (2009) 4600–4601; doi:10.1021/ja900880z

data_4104146
_publ_contact_author_name        'Herbert W. Roesky'
_publ_section_title
;
 Oxidative Addition of Ammonia at a Silicon(II) Center and an
 Unprecedented Hydrogenation Reaction of Compounds with Low-Valent Group
 14 Elements Using Ammonia Borane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4600
_journal_page_last               4601
_journal_paper_doi               10.1021/ja900880z
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C29 H43 N3 Si'
_chemical_formula_weight         461.75
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.529(3)
_cell_length_b                   17.296(4)
_cell_length_c                   20.897(4)
_cell_measurement_reflns_used    54219
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      54.0
_cell_measurement_theta_min      3.1
_cell_volume                     5613(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  IPDSII
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51543
_diffrn_reflns_theta_full        26.98
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.9482
_exptl_absorpt_correction_T_min  0.8855
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         6091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+3.8627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1523
_reflns_number_gt                5078
_reflns_number_total             6091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja900880z_si_002.cif
_cod_data_source_block           ja44
_cod_database_code               4104146