Synthesis and Properties of Bridgehead-Functionalized Permethylbicyclo[2.2.2]octasilanes.
Stueger, Harald; Hasken, Bernd; Gross, Uwe; Fischer, Roland; Torvisco Gomez, Ana; Organometallics 32 (2013) 4490–4500; doi:10.1021/om400184y

data_4081227
_publ_section_title
;
 Synthesis and Properties of Bridgehead-Functionalized
 Permethylbicyclo[2.2.2]octasilanes.
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4490
_journal_page_last               4500
_journal_paper_doi               10.1021/om400184y
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C19 H54 O3 Si9'
_chemical_formula_weight         583.43
_chemical_name_systematic
; 
Dodecamethyl-4-trimethylsilylbicyclo[2,2,2]octasilanyl-1-carboxylic acid
;
_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                66.895(7)
_cell_angle_beta                 90.051(7)
_cell_angle_gamma                65.335(8)
_cell_formula_units_Z            2
_cell_length_a                   9.7433(14)
_cell_length_b                   10.3424(14)
_cell_length_c                   22.040(3)
_cell_measurement_temperature    200(2)
_cell_volume                     1820.1(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6737
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    0.345
_exptl_absorpt_correction_T_max  0.9533
_exptl_absorpt_correction_T_min  0.9311
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         6737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+1.6529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1308
_reflns_number_gt                5216
_reflns_number_total             6737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400184y_si_001.cif
_cod_data_source_block           twin5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1820.0(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4081227