Addition of Amines and Hydroborane to the Disilyne RSi\τbSiR (R = SiiPr[CH(SiMe3)2]2) Giving Amino- and Boryl-Substituted Disilenes
Katsuhiko Takeuchi; Masao Ikoshi; Masaaki Ichinohe; Akira Sekiguchi; Journal of the American Chemical Society 132 (2010) 930–931; doi:10.1021/ja910157h

data_4101838
_publ_section_title
;
 Addition of Amines and Hydroborane to the Disilyne RSi\\tbSiR (R =
 SiiPr[CH(SiMe3)2]2) Giving Amino- and Boryl-Substituted Disilenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              930
_journal_page_last               931
_journal_paper_doi               10.1021/ja910157h
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C49 H113 B Si12'
_chemical_formula_weight         1050.28
_chemical_name_systematic
; 
 E-1,1,4,4-Tetrakis[bis(trimethylsilyl)methyl]-1,4-diisopropyl-
 2-(9-borabicyclo[3.3.1]nonan-9-yl]-2-tetrasilene 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 98.946(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4210(5)
_cell_length_b                   11.5920(4)
_cell_length_c                   37.1120(7)
_cell_measurement_reflns_used    56033
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      25.16
_cell_measurement_theta_min      2.00
_cell_volume                     6553.4(3)
_computing_cell_refinement       'HKL scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device       'MacScience DIP2030 Image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            56033
_diffrn_reflns_theta_full        25.16
_diffrn_reflns_theta_max         25.16
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.0048(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         11031
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+0.8809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1476
_reflns_number_gt                8280
_reflns_number_total             11031
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910157h_si_003.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4101838