Silanetriols as Powerful Starting Materials for Selective Condensation to Bulky POSS Cages.
Hurkes, Natascha; Bruhn, Clemens; Belaj, Ferdinand; Pietschnig, Rudolf; Organometallics 33 (2014) 7299–7306; doi:10.1021/om5010918

data_4084889
_publ_section_title
;
 Silanetriols as Powerful Starting Materials for Selective Condensation to
 Bulky POSS Cages.
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7299
_journal_page_last               7306
_journal_paper_doi               10.1021/om5010918
_journal_volume                  33
_journal_year                    2014
_chemical_compound_source        'synthetical product'
_chemical_formula_moiety         'C40 H88 O12 Si8'
_chemical_formula_sum            'C40 H88 O12 Si8'
_chemical_formula_weight         985.81
_chemical_name_systematic
' octakis(1,1-dimethylpropyl)octasilsesquioxane'
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual edited SHELXL-97 .cif file'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.2192(4)
_cell_length_b                   13.2192(4)
_cell_length_c                   53.3347(18)
_cell_measurement_reflns_used    9715
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.03
_cell_measurement_theta_min      2.34
_cell_volume                     8071.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -75
_diffrn_reflns_number            14563
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.34
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2623
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0725P)^2^+12.2905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1280
_reflns_number_gt                2265
_reflns_number_total             2623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5010918_si_002.cif
_cod_data_source_block           4b_NH235B
_cod_depositor_comments
'Adding full bibliography for 4084885--4084891.cif.'
_cod_original_cell_volume        8071.4(5)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4084889