Synthesis and Properties of Phenylsilsesquioxanes with Ladder and Double-Decker Structures
Endo, Hisayuki; Takeda, Nobuhiro; Unno, Masafumi; Organometallics 33 (2014) 4148–; doi:10.1021/om500010y

data_4084126
_publ_section_title
;
 Synthesis and Properties of Phenylsilsesquioxanes with Ladder and
 Double-Decker Structures
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4148
_journal_paper_doi               10.1021/om500010y
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C72 H60 O10 Si8, 0.5(C7H8)'
_chemical_formula_sum            'C75.5 H64 O10 Si8'
_chemical_formula_weight         1355.99
_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                90.768(4)
_cell_angle_beta                 94.007(4)
_cell_angle_gamma                90.360(4)
_cell_formula_units_Z            4
_cell_length_a                   10.7054(9)
_cell_length_b                   13.9916(11)
_cell_length_c                   47.955(4)
_cell_measurement_reflns_used    36268
_cell_measurement_temperature    180.1500
_cell_measurement_theta_max      25.6806
_cell_measurement_theta_min      1.9229
_cell_volume                     7164.6(10)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180.1500
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            47636
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2836
_exptl_crystal_size_max          0.3000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.1000
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1717
_refine_ls_number_reflns         24775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0929
_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^)+(0.0685P)^2^+19.0035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2166
_refine_ls_wR_factor_ref         0.2228
_reflns_number_gt                22366
_reflns_number_total             24775
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500010y_si_001.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

 Adding full bibliography for 4084125--4084127.cif.
;
_cod_original_cell_volume        7164.6(11)
_cod_original_formula_sum        'C75.50 H64 O10 Si8'
_cod_database_code               4084126