Synthesis of a Silene from 1,1-Dilithiosilole and 2-Adamantanone
Irina S. Toulokhonova; Ilia A. Guzei; Robert West; Journal of the American Chemical Society 126 (2004) 5336–5337; doi:10.1021/ja0318176

data_4112523
_publ_section_title
;
 Synthesis of a Silene from 1,1-Dilithiosilole and 2-Adamantanone
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5336
_journal_page_last               5337
_journal_paper_doi               10.1021/ja0318176
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C48 H48 O Si'
_chemical_formula_weight         668.95
_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                97.471(2)
_cell_angle_beta                 104.111(2)
_cell_angle_gamma                115.452(2)
_cell_formula_units_Z            4
_cell_length_a                   14.2755(17)
_cell_length_b                   15.4092(18)
_cell_length_c                   19.496(2)
_cell_measurement_temperature    173(2)
_cell_volume                     3618.0(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0598
_diffrn_reflns_av_sigmaI/netI    0.1379
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18719
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.9929
_exptl_absorpt_correction_T_min  0.9779
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_meas      0
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         10989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1539
_refine_ls_R_factor_gt           0.0849
_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^)+(0.1001P)^2^+1.3317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2005
_refine_ls_wR_factor_ref         0.2221
_reflns_number_gt                6089
_reflns_number_total             10989
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0318176si20040503_121356_3.cif
_cod_data_source_block           product10
_cod_database_code               4112523