Dipotassium 4,4′-(hexane-3,4-di­yl)bis­(benzene­sulfonate) dihydrate

Orola, L.; Veidis, M.V.; Belyakov, S.; Actins, A.

doi:10.1107/S160053680802120X

Volume 64
Part 8
Page m1027
August 2008

Received 4 July 2008
Accepted 8 July 2008
Online 16 July 2008

Key indicators
Single-crystal X-ray study
T = 298 K
Mean (C-C) = 0.005 Å
R = 0.052
wR = 0.122
Data-to-parameter ratio = 14.0
Details

Dipotassium 4,4'-(hexane-3,4-diyl)bis(benzenesulfonate) dihydrate

Liana Orola,^a Mikelis V. Veidis,^a ^* Sergey Belyakov ^b and Andris Actins ^a

^aUniversity of Latvia, Kr. Valdemara 48, Riga, LV 1013, Latvia, and ^bLatvian Institute of Organic Synthesis, Aizkraukles 21, Riga, LV 1006, Latvia
Correspondence e-mail: veidis@lu.lv

The anion of the title compound, also called sygethin dihydrate, 2K⁺·C₁₈H₂₀O₆S₂^2-·2H₂O, has crystallographic inversion symmetry. The K⁺ cation is surrounded by eight O atoms in a distorted cubic coordination geometry, forming extended K-O-S networks. There are also O-HO hydrogen bonds.

Related literature

For the synthesis, see: Torf & Khromov-Borisov (1961). For general background, see: Svergun (1979). For a related structure, see: Weeks et al. (1973).

Experimental

Crystal data

2K⁺·C₁₈H₂₀O₆S₂^2-·2H₂O
M_r = 255.36
Triclinic, $[P \overline 1]$
a = 5.8741 (5) Å
b = 6.5684 (5) Å
c = 15.2335 (14) Å
= 84.272 (4)°
= 83.768 (5)°
= 76.522 (6)°
V = 566.51 (8) Å³
Z = 1
Mo K radiation
= 0.64 mm^-1
T = 298 K
0.27 × 0.19 × 0.14 mm

Data collection

Nonius KappaCCD diffractometer
Absorption correction: none
4330 measured reflections
2576 independent reflections
1918 reflections with I > 2(I)
R_int = 0.027

Refinement

R[F² > 2(F²)] = 0.051
wR(F²) = 0.122
S = 0.89
1918 reflections
137 parameters
H-atom parameters constrained
_max = 1.49 e Å^-3
_min = -0.42 e Å^-3

Table 1
Selected bond lengths (Å)

K14-O9ⁱ	2.733 (3)
K14-O7ⁱⁱ	2.736 (3)
K14-O15ⁱⁱ	2.816 (3)
K14-O7ⁱⁱⁱ	2.834 (3)
K14-O9	2.934 (3)
K14-O15	2.937 (3)
K14-O8ⁱⁱⁱ	2.970 (3)
K14-O7	3.211 (3)
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) -x+1, -y, -z+1; (iii) x+1, y, z.

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O15-H5O8^iv	0.84	2.00	2.790 (2)	156
Symmetry code: (iv) -x, -y+1, -z+1.

Data collection: COLLECT (Nonius, 2001); cell refinement: DENZO/SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO/SCALEPACK; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: CRYSTALS.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: CF2208 ).

Acknowledgements

Financial aid was provided by Latvia Science Council grant 05.1737.

References

Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. & Watkin, D. J. (2003). J. Appl. Cryst. 36, 1487.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.
Svergun, V. T. (1979). Biull. Eksp. Biol. Med. 87, 151-153.
Torf, S. F. & Khromov-Borisov, N. V. (1961). Med. Radiol. 15, 13-14.
Weeks, C. M., Pokrywiecki, S. & Duax, W. (1973). Acta Cryst. B29, 1729-1731.

metal-organic compounds