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_4112521
_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            'C38 H36 O Si'
_chemical_formula_weight         536.76
_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                73.134(2)
_cell_angle_beta                 63.641(2)
_cell_angle_gamma                85.474(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8025(12)
_cell_length_b                   11.8154(12)
_cell_length_c                   11.9960(12)
_cell_measurement_temperature    100(2)
_cell_volume                     1432.0(3)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11763
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.9587
_exptl_absorpt_correction_T_min  0.9534
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_meas      0
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0639P)^2^+0.5508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1201
_reflns_number_gt                5341
_reflns_number_total             5801
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0318176si20040503_121356_1.cif
_cod_data_source_block           product5
_cod_database_code               4112521