#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2012837.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2012837
loop_
_publ_author_name
'Bowes, Katharine F.'
'Glidewell, Christopher'
'Low, John N.'
_publ_section_title
;
 Tetrameric triphenylsilanol, (Ph~3~SiOH)~4~, and the adduct
 (Ph~3~SiOH)~2~--dimethyl sulfoxide, both at 120K, and the adduct
 (Ph~3~SiOH)~4~--1,4-dioxan at 150K: interplay of
 O---H···O and
 C---H···\p(arene) interactions
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o409
_journal_page_last               o415
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         '2C18 H16 O Si , C2 H6 O S'
_chemical_formula_sum            'C38 H38 O3 S Si'
_chemical_formula_weight         630.94
_chemical_name_systematic
;
Bis(triphenylsilanol) dimethyl sulfoxide solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 96.1310(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8842(3)
_cell_length_b                   8.5391(2)
_cell_length_c                   23.7053(6)
_cell_measurement_reflns_used    3808
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.12
_cell_volume                     3398.18(13)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'PLATON (Spek, 2002)'
_computing_publication_material  'SHELXL97 and  PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_av_sigmaI/netI    0.050
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            21226
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.27
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.071
_refine_ls_R_factor_gt           0.042
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0516P)^2^+2.3569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.097
_refine_ls_wR_factor_ref         0.109
_reflns_number_gt                2792
_reflns_number_total             3808
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    sk1558.cif
_[local]_cod_data_source_block   II
_[local]_cod_cif_authors_sg_H-M  C2/c
_cod_database_code               2012837
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Si1 0.13139(3) 0.41615(6) 0.357114(19) 0.02035(14) Uani d . 1 . . Si
O1 0.13029(7) 0.48115(15) 0.29238(5) 0.0264(3) Uani d . 1 . . O
C11 0.04453(10) 0.2838(2) 0.36374(7) 0.0207(4) Uani d . 1 . . C
C12 -0.02876(10) 0.3119(2) 0.33237(7) 0.0262(4) Uani d . 1 . . C
C13 -0.09327(11) 0.2134(2) 0.33604(8) 0.0310(4) Uani d . 1 . . C
C14 -0.08579(11) 0.0828(2) 0.37068(8) 0.0298(4) Uani d . 1 . . C
C15 -0.01394(11) 0.0518(2) 0.40199(8) 0.0291(4) Uani d . 1 . . C
C16 0.05022(10) 0.1513(2) 0.39863(7) 0.0254(4) Uani d . 1 . . C
C21 0.13235(10) 0.5825(2) 0.40832(7) 0.0216(4) Uani d . 1 . . C
C22 0.08744(11) 0.5835(2) 0.45440(7) 0.0242(4) Uani d . 1 . . C
C23 0.09262(11) 0.7061(2) 0.49301(8) 0.0302(4) Uani d . 1 . . C
C24 0.14239(11) 0.8306(2) 0.48615(8) 0.0299(4) Uani d . 1 . . C
C26 0.18275(10) 0.7100(2) 0.40263(7) 0.0271(4) Uani d . 1 . . C
C25 0.18776(11) 0.8330(2) 0.44069(8) 0.0303(4) Uani d . 1 . . C
C31 0.22556(10) 0.3029(2) 0.37190(7) 0.0211(4) Uani d . 1 . . C
C32 0.26853(10) 0.3012(2) 0.42553(7) 0.0240(4) Uani d . 1 . . C
C33 0.33784(11) 0.2143(2) 0.43617(8) 0.0295(4) Uani d . 1 . . C
C34 0.36536(12) 0.1268(2) 0.39349(8) 0.0355(5) Uani d . 1 . . C
C35 0.32367(12) 0.1253(3) 0.34011(8) 0.0384(5) Uani d . 1 . . C
C36 0.25466(11) 0.2129(2) 0.32953(7) 0.0307(4) Uani d . 1 . . C
O2 0.0000 0.6504(2) 0.2500 0.0330(4) Uani d S 1 . . O
S2 0.0168(5) 0.8102(7) 0.2199(3) 0.0301(4) Uani d P 0.25 A -1 S
C2 0.07645(16) 0.9123(3) 0.27250(9) 0.0488(6) Uani d P 0.50 A -1 C
S2A -0.0141(5) 0.8095(7) 0.2806(3) 0.0301(4) Uani d P 0.25 A -2 S
C2A 0.07645(16) 0.9123(3) 0.27250(9) 0.0488(6) Uani d P 0.50 A -2 C
H1 0.0910 0.5413 0.2769 0.032 Uiso d R 1 . . H
H12 -0.0346 0.4004 0.3080 0.031 Uiso calc R 1 . . H
H13 -0.1428 0.2357 0.3147 0.037 Uiso calc R 1 . . H
H14 -0.1299 0.0149 0.3729 0.036 Uiso calc R 1 . . H
H15 -0.0084 -0.0377 0.4259 0.035 Uiso calc R 1 . . H
H16 0.0993 0.1289 0.4206 0.030 Uiso calc R 1 . . H
H22 0.0526 0.4985 0.4595 0.029 Uiso calc R 1 . . H
H23 0.0617 0.7041 0.5242 0.036 Uiso calc R 1 . . H
H24 0.1457 0.9148 0.5125 0.036 Uiso calc R 1 . . H
H26 0.2144 0.7121 0.3718 0.033 Uiso calc R 1 . . H
H25 0.2221 0.9189 0.4358 0.036 Uiso calc R 1 . . H
H32 0.2500 0.3608 0.4553 0.029 Uiso calc R 1 . . H
H33 0.3664 0.2150 0.4729 0.035 Uiso calc R 1 . . H
H34 0.4130 0.0675 0.4008 0.043 Uiso calc R 1 . . H
H35 0.3423 0.0643 0.3107 0.046 Uiso calc R 1 . . H
H36 0.2265 0.2116 0.2926 0.037 Uiso calc R 1 . . H
H2A 0.0761 0.8578 0.3089 0.059 Uiso calc PR 0.50 A -1 H
H2B 0.0556 1.0186 0.2758 0.059 Uiso calc PR 0.50 A -1 H
H2C 0.1311 0.9176 0.2623 0.059 Uiso calc PR 0.50 A -1 H
H2D 0.1211 0.8589 0.2943 0.059 Uiso calc PR 0.50 A -2 H
H2E 0.0725 1.0197 0.2864 0.059 Uiso calc PR 0.50 A -2 H
H2F 0.0853 0.9143 0.2323 0.059 Uiso calc PR 0.50 A -2 H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Si1 0.0197(2) 0.0215(3) 0.0200(2) 0.00171(19) 0.00262(18) 0.00043(18)
O1 0.0271(6) 0.0295(7) 0.0226(6) 0.0032(5) 0.0031(5) 0.0041(5)
C11 0.0214(8) 0.0207(9) 0.0202(8) 0.0018(7) 0.0041(7) -0.0032(7)
C12 0.0246(9) 0.0263(10) 0.0280(9) 0.0028(7) 0.0038(7) 0.0026(7)
C13 0.0209(9) 0.0397(12) 0.0319(10) 0.0000(8) 0.0004(7) -0.0023(8)
C14 0.0281(10) 0.0319(11) 0.0306(9) -0.0083(8) 0.0087(8) -0.0066(8)
C15 0.0342(10) 0.0245(10) 0.0296(9) -0.0019(8) 0.0071(8) 0.0006(7)
C16 0.0246(9) 0.0254(10) 0.0260(9) 0.0012(7) 0.0016(7) -0.0015(7)
C21 0.0203(8) 0.0201(9) 0.0238(8) 0.0037(7) -0.0007(7) 0.0021(7)
C22 0.0252(9) 0.0207(9) 0.0267(9) 0.0010(7) 0.0024(7) 0.0009(7)
C23 0.0348(10) 0.0279(10) 0.0284(9) 0.0038(8) 0.0054(8) -0.0026(8)
C24 0.0362(10) 0.0221(10) 0.0300(9) 0.0043(8) -0.0030(8) -0.0044(7)
C26 0.0252(9) 0.0259(10) 0.0304(9) 0.0015(8) 0.0039(8) 0.0030(7)
C25 0.0285(9) 0.0207(10) 0.0408(11) -0.0023(8) -0.0007(8) 0.0008(8)
C31 0.0189(8) 0.0203(9) 0.0246(8) -0.0015(7) 0.0049(7) 0.0013(7)
C32 0.0253(9) 0.0231(9) 0.0238(9) -0.0003(7) 0.0040(7) 0.0003(7)
C33 0.0276(9) 0.0322(11) 0.0274(9) 0.0020(8) -0.0023(8) 0.0042(8)
C34 0.0277(10) 0.0403(12) 0.0387(11) 0.0119(9) 0.0044(8) 0.0050(9)
C35 0.0360(11) 0.0476(13) 0.0329(10) 0.0166(10) 0.0099(9) -0.0023(9)
C36 0.0295(9) 0.0382(11) 0.0242(9) 0.0078(8) 0.0013(8) -0.0026(8)
O2 0.0338(10) 0.0193(10) 0.0437(11) 0.000 -0.0062(8) 0.000
S2 0.0429(8) 0.0228(6) 0.0246(6) 0.013(3) 0.0042(5) 0.014(2)
C2 0.0668(16) 0.0334(12) 0.0446(12) -0.0188(11) -0.0016(11) 0.0000(10)
S2A 0.0429(8) 0.0228(6) 0.0246(6) 0.013(3) 0.0042(5) 0.014(2)
C2A 0.0668(16) 0.0334(12) 0.0446(12) -0.0188(11) -0.0016(11) 0.0000(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Si1 C31 . 106.12(7) no
O1 Si1 C21 . 110.57(7) no
C31 Si1 C21 . 108.95(8) no
O1 Si1 C11 . 110.76(7) no
C31 Si1 C11 . 109.37(7) no
C21 Si1 C11 . 110.93(7) no
Si1 O1 H1 . 121.4 no
C12 C11 C16 . 117.09(16) no
C12 C11 Si1 . 120.67(13) no
C16 C11 Si1 . 122.22(13) no
C13 C12 C11 . 121.37(17) no
C13 C12 H12 . 119.3 no
C11 C12 H12 . 119.3 no
C14 C13 C12 . 120.27(17) no
C14 C13 H13 . 119.9 no
C12 C13 H13 . 119.9 no
C15 C14 C13 . 119.61(17) no
C15 C14 H14 . 120.2 no
C13 C14 H14 . 120.2 no
C14 C15 C16 . 120.00(17) no
C14 C15 H15 . 120.0 no
C16 C15 H15 . 120.0 no
C15 C16 C11 . 121.67(16) no
C15 C16 H16 . 119.2 no
C11 C16 H16 . 119.2 no
C22 C21 C26 . 117.29(16) no
C22 C21 Si1 . 123.10(13) no
C26 C21 Si1 . 119.55(13) no
C23 C22 C21 . 121.33(17) no
C23 C22 H22 . 119.3 no
C21 C22 H22 . 119.3 no
C24 C23 C22 . 120.12(17) no
C24 C23 H23 . 119.9 no
C22 C23 H23 . 119.9 no
C23 C24 C25 . 119.88(17) no
C23 C24 H24 . 120.1 no
C25 C24 H24 . 120.1 no
C25 C26 C21 . 121.67(16) no
C25 C26 H26 . 119.2 no
C21 C26 H26 . 119.2 no
C26 C25 C24 . 119.71(17) no
C26 C25 H25 . 120.1 no
C24 C25 H25 . 120.1 no
C32 C31 C36 . 117.50(15) no
C32 C31 Si1 . 121.82(12) no
C36 C31 Si1 . 120.66(13) no
C33 C32 C31 . 121.21(16) no
C33 C32 H32 . 119.4 no
C31 C32 H32 . 119.4 no
C34 C33 C32 . 120.08(17) no
C34 C33 H33 . 120.0 no
C32 C33 H33 . 120.0 no
C33 C34 C35 . 119.94(17) no
C33 C34 H34 . 120.0 no
C35 C34 H34 . 120.0 no
C34 C35 C36 . 119.86(18) no
C34 C35 H35 . 120.1 no
C36 C35 H35 . 120.1 no
C35 C36 C31 . 121.42(17) no
C35 C36 H36 . 119.3 no
C31 C36 H36 . 119.3 no
C2 S2 C2 2 97.4(4) no
C2A S2A C2A 2 97.5(4) no
O2 S2 C2 . 103.1(4) no
O2 S2 C2A . 103.1(4) no
O2 S2A C2 . 101.6(4) no
O2 S2A C2A . 101.6(4) no
S2 C2 H2A . 109.5 no
S2 C2 H2B . 109.5 no
H2A C2 H2B . 109.5 no
S2 C2 H2C . 109.5 no
H2A C2 H2C . 109.5 no
H2B C2 H2C . 109.5 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Si1 O1 1.6300(12) y
Si1 C31 1.8621(17) no
Si1 C21 1.8673(17) no
Si1 C11 1.8713(17) no
O1 H1 0.890 no
C11 C12 1.395(2) no
C11 C16 1.399(2) no
C12 C13 1.386(3) no
C12 H12 0.9500 no
C13 C14 1.382(3) no
C13 H13 0.9500 no
C14 C15 1.379(3) no
C14 H14 0.9500 no
C15 C16 1.385(3) no
C15 H15 0.9500 no
C16 H16 0.9500 no
C21 C22 1.395(2) no
C21 C26 1.397(2) no
C22 C23 1.387(2) no
C22 H22 0.9500 no
C23 C24 1.375(3) no
C23 H23 0.9500 no
C24 C25 1.387(3) no
C24 H24 0.9500 no
C26 C25 1.382(3) no
C26 H26 0.9500 no
C25 H25 0.9500 no
C31 C32 1.395(2) no
C31 C36 1.395(2) no
C32 C33 1.386(2) no
C32 H32 0.9500 no
C33 C34 1.378(3) no
C33 H33 0.9500 no
C34 C35 1.381(3) no
C34 H34 0.9500 no
C35 C36 1.385(3) no
C35 H35 0.9500 no
C36 H36 0.9500 no
O2 S2 1.579(7) no
O2 S2A 1.570(7) no
S2 C2 1.750(8) no
S2A C2 1.791(8) no
C2 H2A 0.9800 no
C2 H2B 0.9800 no
C2 H2C 0.9800 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1 O2 . 0.89 1.85 2.7320(15) 172 y
C14 H14 Cg3 5_445 0.95 2.88 3.757(2) 154 y
C23 H23 Cg1 3_566 0.95 2.90 3.767(2) 152 y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
O1 Si1 C11 C12 -34.66(15) no
C31 Si1 C11 C12 -151.28(13) no
C21 Si1 C11 C12 88.52(15) no
O1 Si1 C11 C16 143.53(13) no
C31 Si1 C11 C16 26.92(15) no
C21 Si1 C11 C16 -93.29(14) no
C16 C11 C12 C13 0.5(2) no
Si1 C11 C12 C13 178.83(14) no
C11 C12 C13 C14 -0.9(3) no
C12 C13 C14 C15 0.6(3) no
C13 C14 C15 C16 0.0(3) no
C14 C15 C16 C11 -0.3(3) no
C12 C11 C16 C15 0.1(2) no
Si1 C11 C16 C15 -178.20(13) no
O1 Si1 C21 C22 138.88(14) no
C31 Si1 C21 C22 -104.86(15) no
C11 Si1 C21 C22 15.59(16) no
O1 Si1 C21 C26 -44.23(15) no
C31 Si1 C21 C26 72.03(15) no
C11 Si1 C21 C26 -167.52(13) no
C26 C21 C22 C23 0.0(3) no
Si1 C21 C22 C23 176.96(13) no
C21 C22 C23 C24 0.4(3) no
C22 C23 C24 C25 -0.3(3) no
C22 C21 C26 C25 -0.5(3) no
Si1 C21 C26 C25 -177.54(13) no
C21 C26 C25 C24 0.5(3) no
C23 C24 C25 C26 -0.1(3) no
O1 Si1 C31 C32 144.87(14) no
C21 Si1 C31 C32 25.79(16) no
C11 Si1 C31 C32 -95.62(15) no
O1 Si1 C31 C36 -36.74(16) no
C21 Si1 C31 C36 -155.81(14) no
C11 Si1 C31 C36 82.78(15) no
C36 C31 C32 C33 0.5(3) no
Si1 C31 C32 C33 178.90(14) no
C31 C32 C33 C34 -0.3(3) no
C32 C33 C34 C35 -0.3(3) no
C33 C34 C35 C36 0.6(3) no
C34 C35 C36 C31 -0.4(3) no
C32 C31 C36 C35 -0.1(3) no
Si1 C31 C36 C35 -178.61(16) no