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The title compound, C8H12O8Si, previously reported by Kamenar & Bruvo [Z. Kristallogr. (1975). 141, 97-103], has been rerefined against new intensity data. Geometric parameters agree quite well. However, our results are of significantly higher precision. The Si atom is located on a special position of site symmetry \overline 4.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802012916/ob6152sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802012916/ob6152Isup2.hkl
Contains datablock I

CCDC reference: 193777

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.001 Å
  • R factor = 0.023
  • wR factor = 0.063
  • Data-to-parameter ratio = 27.3

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Red Alert Alert Level A:
DIFF_019 Alert A _diffrn_standards_number is missing Number of standards used in measurement.
Author response: The data have been collected on an area detector.
DIFF_020  Alert A _diffrn_standards_interval_count and
          _diffrn_standards_interval_time are missing. Number of measurements
          between standards or time (min) between standards.
Author response: The data have been collected on an area detector.
DIFF_022  Alert A _diffrn_standards_decay_% is missing
          Percentage decrease in standards intensity.
Author response: The data have been collected on an area detector.

Amber Alert Alert Level B:
ABSTM_02 Alert B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75 Tmin and Tmax reported: 0.659 0.952 Tmin' and Tmax expected: 0.897 0.952 RR' = 0.735 Please check that your absorption correction is appropriate. General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 32.74 From the CIF: _reflns_number_total 1091 Count of symmetry unique reflns 650 Completeness (_total/calc) 167.85% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 441 Fraction of Friedel pairs measured 0.678 Are heavy atom types Z>Si present yes Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.
3 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
0 Alert Level C = Please check

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991).

Silicon(iv) acetate top
Crystal data top
C8H12O8SiDx = 1.463 Mg m3
Mr = 264.27Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P421cCell parameters from 10715 reflections
a = 7.3086 (6) Åθ = 3.8–32.6°
c = 11.2295 (12) ŵ = 0.22 mm1
V = 599.83 (9) Å3T = 173 K
Z = 2Block, colourless
F(000) = 2760.48 × 0.24 × 0.22 mm
Data collection top
Stoe IPDS II two-circle
diffractometer
1091 independent reflections
Radiation source: fine-focus sealed tube1059 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.040
ω scansθmax = 32.7°, θmin = 3.9°
Absorption correction: empirical (using intensity measurements)
(MULABS; Spek, 1990; Blessing, 1995)
h = 1110
Tmin = 0.659, Tmax = 0.952k = 1111
7495 measured reflectionsl = 1717
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.023 w = 1/[σ2(Fo2) + (0.0407P)2 + 0.0161P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.063(Δ/σ)max < 0.001
S = 1.10Δρmax = 0.15 e Å3
1091 reflectionsΔρmin = 0.20 e Å3
40 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.084 (16)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack (1983), 441 Friedel pairs
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.07 (13)
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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Si11.00001.00000.00000.02785 (10)
O10.85017 (9)0.91606 (9)0.09372 (5)0.03344 (14)
C10.69252 (11)0.82883 (11)0.06204 (6)0.03103 (15)
C20.59766 (13)0.74777 (15)0.16648 (7)0.0424 (2)
H2A0.47180.71600.14450.064*
H2B0.59590.83660.23190.064*
H2C0.66270.63720.19200.064*
O20.64357 (11)0.82040 (12)0.03984 (6)0.0483 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Si10.03295 (13)0.03295 (13)0.01765 (14)0.0000.0000.000
O10.0347 (3)0.0431 (3)0.0226 (2)0.0052 (2)0.00045 (19)0.0004 (2)
C10.0364 (3)0.0315 (3)0.0252 (3)0.0015 (2)0.0015 (2)0.0009 (2)
C20.0445 (4)0.0523 (5)0.0304 (3)0.0148 (4)0.0008 (3)0.0057 (3)
O20.0596 (4)0.0586 (4)0.0267 (2)0.0143 (3)0.0091 (3)0.0015 (3)
Geometric parameters (Å, º) top
Si1—O1i1.6380 (6)C1—O21.2002 (8)
Si1—O11.6380 (6)C1—C21.4857 (11)
Si1—O1ii1.6380 (6)C2—H2A0.9800
Si1—O1iii1.6381 (6)C2—H2B0.9800
O1—C11.3640 (10)C2—H2C0.9800
O1i—Si1—O1100.04 (4)O2—C1—C2126.36 (8)
O1i—Si1—O1ii114.38 (2)O1—C1—C2112.00 (6)
O1—Si1—O1ii114.38 (2)C1—C2—H2A109.5
O1i—Si1—O1iii114.38 (2)C1—C2—H2B109.5
O1—Si1—O1iii114.38 (2)H2A—C2—H2B109.5
O1ii—Si1—O1iii100.04 (4)C1—C2—H2C109.5
C1—O1—Si1124.90 (5)H2A—C2—H2C109.5
O2—C1—O1121.63 (7)H2B—C2—H2C109.5
O1i—Si1—O1—C1179.65 (9)Si1—O1—C1—O26.42 (13)
O1ii—Si1—O1—C156.92 (9)Si1—O1—C1—C2172.66 (6)
O1iii—Si1—O1—C157.63 (9)
Symmetry codes: (i) x+2, y+2, z; (ii) y, x+2, z; (iii) y+2, x, z.
 

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