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_4084127
_publ_section_title
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 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 O14 Si10'
_chemical_formula_sum            'C72 H60 O14 Si10'
_chemical_formula_weight         1430.10
_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                101.281(2)
_cell_angle_beta                 103.206(2)
_cell_angle_gamma                95.940(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3673(11)
_cell_length_b                   15.8156(15)
_cell_length_c                   18.8138(19)
_cell_measurement_reflns_used    25314
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      28.2812
_cell_measurement_theta_min      2.2831
_cell_volume                     3470.8(6)
_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      173.1500
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_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  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24294
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.3000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.1000
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         12048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0443P)^2^+2.3152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1061
_reflns_number_gt                11467
_reflns_number_total             12048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500010y_si_001.cif
_cod_data_source_block           3
_cod_depositor_comments
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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.
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_cod_database_code               4084127