Potential Protecting Group Strategy for Disila Analogues of Vinyllithiums: Synthesis and Reactivity of a 2,4,6-Trimethoxyphenyl-Substituted Disilene
Meltzer, Antje; Majumdar, Moumita; White, Andrew J. P.; Huch, Volker; Scheschkewitz, David; Organometallics 32 (2013) 6844–; doi:10.1021/om400545w

data_4081794
_publ_section_title
;
 Potential Protecting Group Strategy for Disila Analogues of
 Vinyllithiums: Synthesis and Reactivity of a
 2,4,6-Trimethoxyphenyl-Substituted Disilene
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6844
_journal_paper_doi               10.1021/om400545w
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C54 H80 O3 Si2'
_chemical_formula_sum            'C54 H80 O3 Si2'
_chemical_formula_weight         833.36
_chemical_name_common            Tip2Si=SiTipTMOP
_chemical_name_systematic
;
 1,1,2-Tris(2,4,6-triisopropylphenyl)-2-(2,4,6-trimethoxyphenyl)disilene
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                93.628(3)
_cell_angle_beta                 100.148(3)
_cell_angle_gamma                115.006(3)
_cell_formula_units_Z            2
_cell_length_a                   13.4402(4)
_cell_length_b                   14.0958(6)
_cell_length_c                   15.3783(5)
_cell_measurement_reflns_used    10000
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.6417
_cell_measurement_theta_min      2.8694
_cell_volume                     2567.85(18)
_computing_cell_refinement       CrysAlisPro,
_computing_data_collection       CrysAlisPro,
_computing_data_reduction        CrysAlisPro,
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 15.9825
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19728
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.705
_diffrn_reflns_theta_min         3.165
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.965
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) 
(compiled Aug  2 2010,13:00:58) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_description       blocks
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         10974
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+1.4607P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8643
_reflns_number_total             10974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400545w_si_010.cif
_cod_data_source_block           2
_cod_database_code               4081794
_shelxl_version_number           2013-2