Potassium N-bromo-2-nitro­benzene­sulfonamidate monohydrate

Gowda, B.T.; Foro, S.; Spandana, H.S.

doi:10.1107/S1600536812042080

Volume 68
Part 11
Page m1358
November 2012

Received 4 October 2012
Accepted 8 October 2012
Online 13 October 2012

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.007 Å
R = 0.053
wR = 0.145
Data-to-parameter ratio = 14.7
Details

Potassium N-bromo-2-nitrobenzenesulfonamidate monohydrate

B. Thimme Gowda,^a ^* Sabine Foro ^b and H. S. Spandana ^a

^aDepartment of Chemistry, Mangalore University, Mangalagangotri 574 199, Mangalore, India, and ^bInstitute of Materials Science, Darmstadt University of Technology, Petersenstrasse 23, D-64287 Darmstadt, Germany
Correspondence e-mail: gowdabt@yahoo.com

In the title compound, K⁺·C₆H₄BrN₂O₄S^-·H₂O, the K⁺ ion is hepta-coordinated by two O atoms from two different water molecules, three sulfonyl O atoms from three N-bromo-2-nitro-benzenesulfonamidate anions and two nitro O atoms from two N-bromo-2-nitro-benzenesulfonamidate anions. The S-N distance of 1.576 (4) Å is consistent with an S=N double bond. The crystal structure is stabilized by intermolecular O-HN and O-HBr hydrogen bonds which link the molecules into polymeric layers running parallel to the bc plane.

Related literature

For the preparation of metal salts of N-haloarylsulfonamides, see: Gowda & Mahadevappa (1983); Usha & Gowda (2006). For studies on the effect of substituents and metal ions on the structures of N-haloarylsulfonamides, see: George et al. (2000); Gowda et al. (2011a,b); Olmstead & Power (1986). For positioning of water H atoms, see: Nardelli (1999).

Experimental

Crystal data

K⁺·C₆H₄BrN₂O₄S^-·H₂O
M_r = 337.20
Monoclinic, P 2₁ /c
a = 13.034 (2) Å
b = 12.815 (2) Å
c = 6.7741 (9) Å
= 100.65 (1)°
V = 1112.0 (3) Å³
Z = 4
Mo K radiation
= 4.27 mm^-1
T = 293 K
0.48 × 0.48 × 0.24 mm

Data collection

Oxford Diffraction Xcalibur diffractometer with Sapphire CCD detector
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2009 $[Oxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ) T_min = 0.234, T_max = 0.428
3896 measured reflections
2236 independent reflections
1847 reflections with I > 2(I)
R_int = 0.042

Refinement

R[F² > 2(F²)] = 0.053
wR(F²) = 0.145
S = 1.06
2236 reflections
152 parameters
3 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 0.79 e Å^-3
_min = -1.21 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O5-H51N1ⁱ	0.84 (2)	2.13 (3)	2.926 (5)	157 (5)
O5-H52Br1ⁱⁱ	0.84 (2)	2.85 (4)	3.509 (4)	137 (4)
Symmetry codes: (i) -x, -y, -z+1; (ii) $[-x, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]$ .

Data collection: CrysAlis CCD (Oxford Diffraction, 2009 $[Oxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ); cell refinement: CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2009 $[Oxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: PLATON (Spek, 2009); software used to prepare material for publication: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: ZL2509 ).

Acknowledgements

BTG thanks the University Grants Commission, Government of India, New Delhi, for a one-time grant to Faculty/Professors under UGC-BSR.

References

George, E., Vivekanandan, S. & Sivakumar, K. (2000). Acta Cryst. C56, 1208-1209.
Gowda, B. T., Foro, S. & Shakuntala, K. (2011a). Acta Cryst. E67, m926.
Gowda, B. T., Foro, S. & Shakuntala, K. (2011b). Acta Cryst. E67, m1015.
Gowda, B. T. & Mahadevappa, D. S. (1983). Talanta, 30, 359-362.
Nardelli, M. (1999). J. Appl. Cryst. 32, 563-571.
Olmstead, M. M. & Power, P. P. (1986). Inorg. Chem. 25, 4057-4058.
Oxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148-155.
Usha, K. M. & Gowda, B. T. (2006). J. Chem. Sci. 118, 351-359.

metal-organic compounds