Hydroboration of Disilyne RSi≡SiR (R = SiiPr[CH(SiMe3)2]2), Giving Boryl-Substituted Disilenes
Takeuchi, Katsuhiko; Ichinohe, Masaaki; Sekiguchi, Akira; Organometallics 30 (2011) 2044–; doi:10.1021/om200106h

data_4064433
_publ_section_title
;
 Hydroboration of Disilyne RSi\\tb SiR (R = SiiPr[CH(SiMe3)2]2), Giving
 Boryl-Substituted Disilenes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2044
_journal_paper_doi               10.1021/om200106h
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C40 H95 B O2 Si12'
_chemical_formula_weight         956.05
_chemical_name_systematic
; 
 E-1,1,4,4-Tetrakis[bis(trimethylsilyl)methyl]-1,4-isopropyl- 
 2-(catecoholboryl)-2-disilene 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.0390(10)
_cell_angle_beta                 90.5270(10)
_cell_angle_gamma                108.3180(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4283(6)
_cell_length_b                   15.1729(9)
_cell_length_c                   19.7512(11)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.25
_cell_volume                     2903.8(3)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120.0(1)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0777
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31308
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  0.9844
_exptl_absorpt_correction_T_min  0.9397
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
SADABS Sheldrick 1996 
;
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         12707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+2.9667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1436
_reflns_number_gt                8312
_reflns_number_total             12707
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200106h_si_002.cif
_cod_data_source_block           catbhadd_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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-1   '
_cod_database_code               4064433