Acid-Catalyzed Condensation Reaction of Phenylsilanetriol: Unexpected Formation ofcis,trans-1,3,5-Trihydroxy-1,3,5-triphenylcyclotrisiloxane as the Main Product and Its Isolation
Yagihashi, Fujio; Igarashi, Masayasu; Nakajima, Yumiko; Ando, Wataru; Sato, Kazuhiko; Yumoto, Yoshiyuki; Matsui, Chinami; Shimada, Shigeru; Organometallics 33 (2014) 6278–; doi:10.1021/om500691c

data_4084628
_publ_section_title
;
 Acid-Catalyzed Condensation Reaction of Phenylsilanetriol: Unexpected
 Formation ofcis,trans-1,3,5-Trihydroxy-1,3,5-triphenylcyclotrisiloxane as
 the Main Product and Its Isolation
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6278
_journal_paper_doi               10.1021/om500691c
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C18 H18 O6 Si3, C4 H10 O'
_chemical_formula_sum            'C22 H28 O7 Si3'
_chemical_formula_weight         488.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 92.181(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   6.370(5)
_cell_length_b                   17.942(5)
_cell_length_c                   21.769(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     2486(2)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 for windows'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      163(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11508
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  0.9555
_exptl_absorpt_correction_T_min  0.8938
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS; Sheldrick 2007
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4375
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0612
_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^)+(0.0635P)^2^+4.9030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.1628
_reflns_number_gt                4027
_reflns_number_total             4375
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500691c_si_001.cif
_cod_data_source_block           yagi5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--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 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 4084628.cif.
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4084628