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_4084891
_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_sum            'C56 H120 O12 Si8'
_chemical_formula_weight         1210.24
_chemical_name_systematic
' octakis(1,1-dimethylpentyl)octasilsesquioxane'
_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           'manual edited SHELXL-97 .cif file'
_cell_angle_alpha                90.00
_cell_angle_beta                 97.065(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.1192(9)
_cell_length_b                   12.8237(5)
_cell_length_c                   20.1991(12)
_cell_measurement_reflns_used    19393
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.49
_cell_measurement_theta_min      1.67
_cell_volume                     3629.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      ' 178 frames, detector distance = 135 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1663
_diffrn_reflns_av_sigmaI/netI    0.1091
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22786
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.67
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           30
_diffrn_source_power             1.50
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  0.9868
_exptl_absorpt_correction_T_min  0.8735
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-red ver.1.31 (Stoe & Cie. 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         6395
_refine_ls_number_restraints     370
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0745
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1166P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1887
_refine_ls_wR_factor_ref         0.2028
_reflns_number_gt                4615
_reflns_number_total             6395
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5010918_si_002.cif
_cod_data_source_block           4d_i1113
_cod_depositor_comments
'Adding full bibliography for 4084885--4084891.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4084891