An Isolable Silanoic Ester by Oxygenation of a Stable Silylene
Shenglai Yao; Yun Xiong; Markus Brym; Journal of the American Chemical Society 129 (2007) 7268–7269; doi:10.1021/ja072425s

data_4109527
_publ_contact_author_address
;Institute of Chemistry: Metalorganics and Inorganic Materials,
Technische Universit\"at Berlin, 
Strasse des 17. Juni 135, Sekr. C2, D-10623 Berlin, Germany.
;
_publ_contact_author_email       matthias.driess@tu-berlin.de
_publ_contact_author_fax         0049-30-31429732
_publ_contact_author_name        'Matthias Driess'
_publ_contact_author_phone       0049-30-31422265
_publ_section_title
;
 An Isolable Silanoic Ester by Oxygenation of a Stable Silylene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7268
_journal_page_last               7269
_journal_paper_doi               10.1021/ja072425s
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C123 H172 N8 O6 Si4'
_chemical_formula_weight         1971.05
_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
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_cell_angle_alpha                99.44(3)
_cell_angle_beta                 94.68(4)
_cell_angle_gamma                115.22(4)
_cell_formula_units_Z            1
_cell_length_a                   11.627(5)
_cell_length_b                   13.155(4)
_cell_length_c                   21.083(11)
_cell_measurement_reflns_used    2711
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.7110
_cell_measurement_theta_min      3.0063
_cell_volume                     2836(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S Sapphire'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1129
_diffrn_reflns_av_sigmaI/netI    0.3550
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22375
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
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            colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       rod
_exptl_crystal_F_000             1070
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         9945
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      0.896
_refine_ls_R_factor_all          0.2156
_refine_ls_R_factor_gt           0.0734
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                3743
_reflns_number_total             9945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja072425ssi20070406_085440.cif
_cod_data_source_block           yao98
_cod_database_code               4109527