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_4122592
_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         'C40 H96 Si11'
_chemical_formula_sum            'C40 H96 Si11'
_chemical_formula_weight         886.16
_chemical_name_systematic
; 
 spiro[2,2,5,5-tetra-tert-butyl-3,3,4,4-tetramethyl-bicyclo[4.1.0]heptasil-1(6)-
ene-7,1'-2,2,5,5-tetra-tert-butyl-3,3,4,4-tetramethylcyclopentasilane] 
;
_chemical_temperature_decomposition 511.15
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                101.875(3)
_cell_angle_beta                 97.825(2)
_cell_angle_gamma                111.173(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0612(16)
_cell_length_b                   14.318(2)
_cell_length_c                   18.484(2)
_cell_measurement_reflns_used    21246
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      28.2812
_cell_measurement_theta_min      1.6857
_cell_volume                     2834.3(6)
_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      183(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.920
_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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25462
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.277
_exptl_absorpt_correction_T_max  0.9596
_exptl_absorpt_correction_T_min  0.9339
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(R. Jacobson, private communication, 1998)'
_exptl_crystal_colour            Red-orange
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.365
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         12916
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0590P)^2^+2.4092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1355
_reflns_number_gt                12298
_reflns_number_total             12916
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja507279z_si_002.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been given
as '238 \%C, decomp.'. The value '238 \%C, decomp.' was changed to
'511.15' - it was converted from degrees Celsius(C) to Kelvins(K).

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

 Adding full bibliography for 4122592--4122593.cif.
;
_cod_original_cell_volume        2834.4(7)
_cod_database_code               4122592