Tetrasilane-bridged bicyclo[4.1.0]heptasil-1(6)-ene.
Tsurusaki, Akihiro; Kamiyama, Jun; Kyushin, Soichiro; Journal of the American Chemical Society 136 (2014) 12896–12898; doi:10.1021/ja507279z

data_4122593
_publ_section_title
;
 Tetrasilane-bridged bicyclo[4.1.0]heptasil-1(6)-ene.
;
_journal_issue                   37
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12896
_journal_page_last               12898
_journal_paper_doi               10.1021/ja507279z
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C20 H48 Cl4 Si6'
_chemical_formula_sum            'C20 H48 Cl4 Si6'
_chemical_formula_weight         598.92
_chemical_melting_point          502.1(10)
_chemical_name_systematic
; 
1,1,4,4-Tetra-tert-butyl-2,2,3,3-tetrachloro-5,5,6,6-tetramethylcyclohexasilane
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.6520(8)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   9.1903(5)
_cell_length_b                   21.5113(11)
_cell_length_c                   16.6086(10)
_cell_measurement_reflns_used    20667
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.2812
_cell_measurement_theta_min      0.9466
_cell_volume                     3261.3(3)
_computing_cell_refinement       <i>CrystalClear</i>
_computing_data_collection       '<i>CrystalClear</i> (Rigaku, 2003)'
_computing_data_reduction        <i>CrystalClear</i>
_computing_molecular_graphics    '<i>ORTEP-3</i> (Farrugia, 1997)'
_computing_publication_material
'<i>SHELXL97</i> and <i>Yadokari-XG 2009</i> (Kabuto <i>et al.</i>, 2009)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28885
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.9431
_exptl_absorpt_correction_T_min  0.8907
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(R. Jacobson, private communication, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         8064
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.280
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0129P)^2^+3.1815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0826
_reflns_number_gt                7880
_reflns_number_total             8064
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja507279z_si_002.cif
_cod_data_source_block           compound_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '228-230 \%C' was changed to
'502.1(10)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4122592--4122593.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4122593