Rubidium 2,4,6-trioxo-1,3-diazinan-5-ide–1,3-diazinane-2,4,6-trione–water (1/1/1)

Gryl, M.; Stadnicka, K.

doi:10.1107/S1600536811012657

Volume 67
Part 5
Pages m571-m572
May 2011

Received 21 March 2011
Accepted 5 April 2011
Online 13 April 2011

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.003 Å
R = 0.024
wR = 0.059
Data-to-parameter ratio = 12.8
Details

Rubidium 2,4,6-trioxo-1,3-diazinan-5-ide-1,3-diazinane-2,4,6-trione-water (1/1/1)

Marlena Gryl ^a ^* and Katarzyna Stadnicka ^a

^aFaculty of Chemistry, Jagiellonian University, Ingardena 3, 30-060 Kraków, Poland
Correspondence e-mail: gryl@chemia.uj.edu.pl

The asymmetric unit of the title compound, Rb⁺·C₄H₃N₂O₃^-·C₄H₄N₂O₃·H₂O, consists of one rubidium cation, a barbituric acid molecule, a barbiturate anion and one water molecule. The rubidium ion has seven close-contact interactions with O atoms, with RbO distances ranging from 2.8594 (16) to 3.2641 (14) Å. These seven O atoms together with an eighth O atom at 3.492 (2) Å away from Rb form a distorted polyhedron with shape intermediate between an antiprism and a dodecahedron. The Rb⁺ ions connect layers built of organic components and water molecules linked via N-HO and O-HO hydrogen bonds.

Related literature

For the crystal structures of selected barbiturates, see: Xiong et al. (2003); Gryl et al. (2008, 2011); Braga et al. (2010); Garcia et al. (2010); Ivanova & Spiteller (2010) and for those of rubidium salts, see: Clegg & Liddle (2004); Yildirim et al. (2008). For classification of hydrogen-bond systems according to graph-set theory, see: Bernstein et al. (1995).

Experimental

Crystal data

Rb⁺·C₄H₃N₂O₃^-·C₄H₄N₂O₃·H₂O
M_r = 358.66
Monoclinic, P 2₁ /c
a = 9.8810 (1) Å
b = 19.6790 (5) Å
c = 6.4530 (3) Å
= 108.26 (2)°
V = 1191.59 (15) Å³
Z = 4
Mo K radiation
= 4.20 mm^-1
T = 293 K
0.43 × 0.23 × 0.21 mm

Data collection

Nonius KappaCCD diffractometer
Absorption correction: multi-scan (DENZO and SCALEPACK; Otwinowski & Minor, 1997) T_min = 0.266, T_max = 0.473
17623 measured reflections
2555 independent reflections
2239 reflections with I > 2(I)
R_int = 0.037

Refinement

R[F² > 2(F²)] = 0.024
wR(F²) = 0.059
S = 1.03
2555 reflections
199 parameters
6 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 0.27 e Å^-3
_min = -0.30 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N1A-H1AO6Bⁱ	0.88 (1)	1.90 (1)	2.769 (2)	172 (2)
N3A-H3AO4B	0.86 (1)	1.84 (1)	2.694 (2)	175 (2)
N1B-H1BO2Aⁱⁱ	0.88 (1)	1.94 (1)	2.820 (2)	175 (2)
N3B-H3BO4A	0.87 (1)	2.12 (1)	2.975 (2)	169 (2)
O1W-H1WO6Bⁱⁱⁱ	0.84 (1)	1.87 (1)	2.700 (2)	171 (2)
O1W-H2WO4A^iv	0.83 (1)	2.08 (1)	2.898 (2)	170 (3)
Symmetry codes: (i) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ii) $[-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iii) -x, -y, -z; (iv) -x+1, -y, -z.

Data collection: COLLECT (Nonius, 1998); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO (Otwinowski & Minor, 1997) and SCALEPACK; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: Mercury (Macrae et al., 2006) and ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97 and WinGX (Farrugia, 1999).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: VM2087 ).

Acknowledgements

The authors thank the X-ray Diffraction Laboratory. Faculty of Chemistry, Jagiellonian University, for making the Nonius KappaCCD diffractometer available. This work was partially supported by the Polish Ministry of Science and Higher Education: grant No. N N204 316537.

References

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