Download citation
Download citation
link to html
The title compound, C3H6S4, is a cyclic polysulfane containing one disulfane S2 group and two single S atoms bridged by three CH2 groups, thus forming a seven-membered ring. The ring exhibits a chair conformation.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806026973/hk2082sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806026973/hk2082Isup2.hkl
Contains datablock I

CCDC reference: 618238

Key indicators

  • Single-crystal X-ray study
  • T = 294 K
  • Mean [sigma](S-C)= 0.004 Å
  • R factor = 0.066
  • wR factor = 0.138
  • Data-to-parameter ratio = 31.5

checkCIF/PLATON results

No syntax errors found


No errors found in this datablock

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1996); software used to prepare material for publication: SHELXL97.

1,2,4,6-tetrathiacycloheptane top
Crystal data top
C3H6S4F(000) = 352
Mr = 170.32Dx = 1.711 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 3865 reflections
a = 11.1285 (4) Åθ = 2.5–30.0°
b = 5.2653 (2) ŵ = 1.31 mm1
c = 11.7399 (4) ÅT = 294 K
β = 105.963 (1)°Prism, colorless
V = 661.37 (4) Å30.20 × 0.18 × 0.15 mm
Z = 4
Data collection top
Siemens SMART CCD area-detector
diffractometer
1622 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.090
Graphite monochromatorθmax = 30.6°, θmin = 2.2°
ω scansh = 1215
5831 measured reflectionsk = 77
2018 independent reflectionsl = 1611
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.066Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.138H-atom parameters constrained
S = 1.46 w = 1/[σ2(Fo2) + (0.0288P)2 + 0.65P]
where P = (Fo2 + 2Fc2)/3
2018 reflections(Δ/σ)max < 0.001
64 parametersΔρmax = 0.61 e Å3
0 restraintsΔρmin = 0.64 e Å3
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
S10.6479 (1)0.7137 (2)0.39086 (9)0.0381 (3)
S20.66833 (9)0.3404 (2)0.35810 (8)0.0317 (2)
S30.90117 (9)0.2125 (2)0.56458 (9)0.0350 (2)
S40.69318 (9)0.4823 (2)0.64219 (8)0.0323 (2)
C10.8373 (4)0.2947 (7)0.4111 (3)0.0335 (8)
H1A0.86030.16220.36360.040*
H1B0.87740.45000.39620.040*
C20.8564 (3)0.4824 (7)0.6402 (3)0.0318 (8)
H2A0.87270.63700.60210.038*
H2B0.90880.48510.72130.038*
C30.6301 (4)0.7360 (7)0.5409 (4)0.0341 (8)
H3A0.66880.89320.57570.041*
H3B0.54150.74920.53450.041*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
S10.0499 (6)0.0299 (5)0.0349 (5)0.0059 (4)0.0122 (4)0.0066 (4)
S20.0335 (5)0.0315 (4)0.0276 (4)0.0035 (4)0.0043 (3)0.0041 (3)
S30.0314 (5)0.0320 (5)0.0387 (5)0.0045 (4)0.0047 (4)0.0004 (4)
S40.0353 (5)0.0351 (5)0.0282 (4)0.0031 (4)0.0116 (4)0.0010 (4)
C10.034 (2)0.037 (2)0.034 (2)0.001 (2)0.015 (2)0.003 (2)
C20.027 (2)0.033 (2)0.032 (2)0.006 (1)0.004 (1)0.005 (2)
C30.035 (2)0.028 (2)0.041 (2)0.000 (1)0.014 (2)0.005 (2)
Geometric parameters (Å, º) top
S3—C11.798 (4)C1—H1A0.9700
S3—C21.816 (4)C1—H1B0.9700
S2—C11.827 (4)C3—H3A0.9700
S2—S12.028 (1)C3—H3B0.9700
S4—C31.798 (4)C2—H2A0.9700
S4—C21.823 (4)C2—H2B0.9700
S1—C31.829 (4)
C1—S3—C2102.5 (2)S4—C3—H3A107.9
C1—S2—S1102.8 (1)S1—C3—H3A107.9
C3—S4—C2101.6 (2)S4—C3—H3B107.9
C3—S1—S2107.0 (1)S1—C3—H3B107.9
S3—C1—S2117.3 (2)H3A—C3—H3B107.2
S3—C1—H1A108.0S3—C2—S4114.5 (2)
S2—C1—H1A108.0S3—C2—H2A108.6
S3—C1—H1B108.0S4—C2—H2A108.6
S2—C1—H1B108.0S3—C2—H2B108.6
H1A—C1—H1B107.2S4—C2—H2B108.6
S4—C3—S1117.6 (2)H2A—C2—H2B107.6
C1—S2—S1—C389.4 (2)S2—S1—C3—S424.1 (3)
C2—S3—C1—S260.2 (3)C1—S3—C2—S477.2 (2)
S1—S2—C1—S388.4 (2)C3—S4—C2—S3108.6 (2)
C2—S4—C3—S156.6 (3)
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds