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The title compound, C42H42O7Si2, was obtained as a by-product from the reaction of (p-Tol-O)3SiCl with [PhC(S)S]2Mg·2THF (p-Tol is p-tolyl and THF is tetra­hydro­furan). The mol­ecule has \overline{3} symmetry and is an example of a compound with an Si-O-Si valence angle of 180°. The distribution of this angle within disiloxanes is briefly described and discussed.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806044059/ez2044sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806044059/ez2044Isup2.hkl
Contains datablock I

CCDC reference: 627646

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma](C-C) = 0.002 Å
  • R factor = 0.047
  • wR factor = 0.124
  • Data-to-parameter ratio = 22.9

checkCIF/PLATON results

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Alert level B PLAT396_ALERT_2_B Deviating Si-O-Si Angle from 150 Deg for O1 180.00 Deg.
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 0 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2005); cell refinement: CrysAlis RED (Oxford Diffraction, 2005); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Hexakis(4-methylphenoxy)disiloxane top
Crystal data top
C42H42O7Si2Dx = 1.272 Mg m3
Mr = 714.94Mo Kα radiation, λ = 0.71073 Å
Hexagonal, R3Cell parameters from 1223 reflections
Hall symbol: -R 3θ = 2.6–32.6°
a = 14.1520 (18) ŵ = 0.15 mm1
c = 16.149 (2) ÅT = 120 K
V = 2801.0 (6) Å3Prism, colourless
Z = 30.5 × 0.3 × 0.18 mm
F(000) = 1134
Data collection top
Oxford Diffraction KM-4-CCD
diffractometer
Rint = 0.038
ω scansθmax = 29.9°, θmin = 2.9°
6943 measured reflectionsh = 1819
1810 independent reflectionsk = 1519
1705 reflections with I > 2σ(I)l = 2222
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.047 w = 1/[σ2(Fo2) + (0.0687P)2 + 2.6331P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.124(Δ/σ)max = 0.001
S = 1.07Δρmax = 0.44 e Å3
1810 reflectionsΔρmin = 0.24 e Å3
79 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.10502 (9)0.11280 (9)0.60890 (7)0.0233 (2)
C20.04689 (10)0.21491 (10)0.64574 (8)0.0292 (3)
H20.00540.22810.68760.035*
C30.06634 (11)0.29740 (11)0.62044 (8)0.0314 (3)
H30.02690.36720.64580.038*
C40.14204 (10)0.28065 (10)0.55894 (8)0.0275 (3)
C50.19861 (9)0.17764 (10)0.52273 (8)0.0253 (2)
H50.25020.16460.48030.03*
C60.18088 (9)0.09329 (9)0.54761 (7)0.0235 (2)
H60.22050.02330.52270.028*
C70.16192 (13)0.37181 (12)0.53334 (10)0.0388 (3)
H7A0.2120.34820.4860.047*
H7B0.09250.43590.51770.047*
H7C0.19420.39060.57970.047*
O1000.50.0234 (4)
O20.09017 (7)0.02751 (8)0.63562 (5)0.0277 (2)
Si1000.59925 (3)0.02169 (16)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0225 (5)0.0248 (5)0.0219 (5)0.0113 (4)0.0053 (4)0.0011 (4)
C20.0283 (6)0.0314 (6)0.0242 (5)0.0120 (5)0.0029 (4)0.0070 (4)
C30.0323 (6)0.0259 (6)0.0307 (6)0.0107 (5)0.0001 (5)0.0103 (4)
C40.0256 (5)0.0245 (5)0.0330 (6)0.0131 (4)0.0056 (4)0.0037 (4)
C50.0193 (5)0.0261 (5)0.0301 (5)0.0110 (4)0.0010 (4)0.0043 (4)
C60.0208 (5)0.0214 (5)0.0260 (5)0.0088 (4)0.0029 (4)0.0046 (4)
C70.0379 (7)0.0290 (6)0.0544 (9)0.0203 (6)0.0037 (6)0.0030 (6)
O10.0253 (6)0.0253 (6)0.0197 (8)0.0127 (3)00
O20.0301 (4)0.0316 (4)0.0247 (4)0.0179 (4)0.0068 (3)0.0042 (3)
Si10.0236 (2)0.0236 (2)0.0178 (2)0.01180 (10)00
Geometric parameters (Å, º) top
C1—C61.3827 (16)C5—H50.95
C1—C21.3893 (16)C6—H60.95
C1—O21.3932 (14)C7—H7A0.98
C2—C31.3882 (19)C7—H7B0.98
C2—H20.95C7—H7C0.98
C3—C41.3916 (19)O1—Si1i1.6027 (6)
C3—H30.95O1—Si11.6027 (5)
C4—C51.3931 (16)O2—Si11.6192 (9)
C4—C71.5092 (18)Si1—O2ii1.6192 (9)
C5—C61.3960 (16)Si1—O2iii1.6192 (9)
C6—C1—C2120.73 (11)C1—C6—H6120.4
C6—C1—O2119.15 (10)C5—C6—H6120.4
C2—C1—O2120.07 (11)C4—C7—H7A109.5
C3—C2—C1119.04 (12)C4—C7—H7B109.5
C3—C2—H2120.5H7A—C7—H7B109.5
C1—C2—H2120.5C4—C7—H7C109.5
C2—C3—C4121.75 (11)H7A—C7—H7C109.5
C2—C3—H3119.1H7B—C7—H7C109.5
C4—C3—H3119.1Si1i—O1—Si1180
C3—C4—C5117.94 (11)C1—O2—Si1125.05 (7)
C3—C4—C7120.43 (11)O1—Si1—O2ii111.27 (4)
C5—C4—C7121.62 (12)O1—Si1—O2iii111.27 (4)
C4—C5—C6121.27 (11)O2ii—Si1—O2iii107.61 (4)
C4—C5—H5119.4O1—Si1—O2111.27 (4)
C6—C5—H5119.4O2ii—Si1—O2107.61 (4)
C1—C6—C5119.27 (10)O2iii—Si1—O2107.61 (4)
Symmetry codes: (i) x, y, z+1; (ii) y, xy, z; (iii) x+y, x, z.
 

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