Synthesis, Structure, and Facile Ring Flipping of a Bicyclo[1.1.0]tetrasilane
Ueba-Ohshima, Kiyomi; Iwamoto, Takeaki; Kira, Mitsuo; Organometallics 27 (2008) 320–; doi:10.1021/om7011375

data_4070936
_publ_section_title
;
 Synthesis, Structure, and Facile Ring Flipping of a
 Bicyclo[1.1.0]tetrasilane
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              320
_journal_paper_doi               10.1021/om7011375
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C36 H90 Si10'
_chemical_formula_weight         803.98
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0
_cell_angle_beta                 111.0415(10)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   12.114(3)
_cell_length_b                   33.003(7)
_cell_length_c                   13.766(3)
_cell_measurement_reflns_used    16501
_cell_measurement_temperature    123.2
_cell_measurement_theta_max      27.5
_cell_volume                     5137(2)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        CRYSTALCLEAR
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 28.57
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku/MSC Saturn CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            54872
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.278
_exptl_absorpt_correction_T_max  0.9595
_exptl_absorpt_correction_T_min  0.9212
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.040
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.321
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         11748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.321
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0719
_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^)+(0.0335P)^2^+5.3211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1349
_reflns_number_gt                11302
_reflns_number_total             11748
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7011375-file003.cif
_cod_data_source_block           bicyclotetrasilane
_cod_original_cell_volume        5136(2)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4070936