Di-μ-aqua-bis­{triaqua­[5-(1-oxopyridin-4-yl)tetra­zol-1-ido]sodium}

Jing Dai; Xin-Yuan Chen

doi:10.1107/S1600536810052566

. 2010 Dec 24;67(Pt 1):m111. doi: 10.1107/S1600536810052566

Di-μ-aqua-bis{triaqua[5-(1-oxopyridin-4-yl)tetrazol-1-ido]sodium}

Jing Dai ^a,^*, Xin-Yuan Chen ^a

PMCID: PMC3050412 PMID: 21522524

Abstract

In the title compound, [Na₂(C₆H₄N₅O)₂(H₂O)₈], the Na^I atom is in a distorted octahedral environment defined by six O atoms, one from the 5-(1-oxopyridin-4-yl)tetrazolide anion and five from water molecules. Two water molecules act as bridging ligands, resulting in the formation of dimeric units organized around inversion centers. In the organic anion, the pyridine and tetrazole rings are nearly coplanar, forming a dihedral angle of 4.62 (1)°. The dimeric units and organic anions are connected by O—H⋯O and O—H⋯N hydrogen bonds, leading to the formation of a three-dimensional network.

Related literature

For tetrazole derivatives, see: Zhao et al. (2008 ▶); Fu et al. (2008 ▶, 2009 ▶). For the structures and properties of related compounds, see: Fu et al. (2007 ▶, 2009 ▶); Fu & Xiong (2008 ▶).

Experimental

Crystal data

[Na₂(C₆H₄N₅O)₂(H₂O)₈]
M _r = 514.39
Triclinic,
a = 6.887 (2) Å
b = 7.5200 (15) Å
c = 12.258 (5) Å
α = 78.16 (4)°
β = 83.42 (4)°
γ = 66.68 (3)°
V = 570.2 (3) Å³
Z = 1
Mo Kα radiation
μ = 0.16 mm⁻¹
T = 298 K
0.25 × 0.15 × 0.10 mm

Data collection

Rigaku Mercury2 diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005 ▶) T _min = 0.913, T _max = 1.000
5833 measured reflections
2594 independent reflections
1933 reflections with I > 2σ(I)
R _int = 0.028

Refinement

R[F ² > 2σ(F ²)] = 0.041
wR(F ²) = 0.108
S = 1.05
2594 reflections
154 parameters
H-atom parameters constrained
Δρ_max = 0.23 e Å⁻³
Δρ_min = −0.25 e Å⁻³

Data collection: CrystalClear (Rigaku, 2005 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEPIII (Burnett & Johnson, 1996 ▶), ORTEP-3 for Windows (Farrugia, 1997 ▶) and PLATON (Spek, 2009 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶).

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810052566/dn2636sup1.cif

e-67-0m111-sup1.cif^{(16.2KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810052566/dn2636Isup2.hkl

e-67-0m111-Isup2.hkl^{(127.4KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1WA⋯N2ⁱ	0.85	1.98	2.832 (2)	178
O1W—H1WB⋯N4ⁱⁱ	0.86	1.97	2.817 (2)	167
O2W—H2WA⋯O3Wⁱⁱⁱ	0.85	2.02	2.857 (2)	169
O2W—H2WB⋯N3ⁱⁱ	0.87	2.02	2.878 (2)	169
O3W—H3WA⋯O4W^iv	0.85	1.93	2.754 (2)	163
O3W—H3WB⋯O1^iv	0.85	2.07	2.836 (2)	150
O4W—H4WA⋯O1W^v	0.86	1.96	2.812 (2)	172
O4W—H4WB⋯O1^iv	0.85	1.95	2.7233 (19)	151

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Symmetry codes: (i) Inline graphic ; (ii) ; (iii) ; (iv) ; (v) .

Acknowledgments

This work was supported by a start-up grant from Southeast University.

supplementary crystallographic information

Comment

Tetrazole compounds attracted more attention as phase transition dielectric materials for its application in micro-electronics, memory storage. With the purpose of obtaining phase transition crystals of tetrazol-pyridine compounds, its interaction with various metal ions has been studied and a series of new materials have been elaborated with this organic molecule (Zhao et al., 2008; Fu et al., 2008; Fu et al., 2007; Fu & Xiong 2008). In this paper, we describe the crystal structure of the title compound, tetraaquabis[5-(1-oxopyridin-4-yl)tetrazol-1-ide]sodium(I).

In the title compound, the asymmetric unit is composed of one organic anion, four H₂O molecules and one Na⁺ cation. The Na^I center, with slightly distorted octahedral geometry, is surrounded by six oxygen atoms. Two water molecules act as abridging ligand, resulting in the formation of dimeric unit (Fig. 1) organized around inversion center. In the organic anion, the tetrazole N atoms are deprotonated. The pyridine and tetrazole rings are nearly coplanar and only twisted from each other by a dihedral angle of 4.62 (1)°. The geometric parameters of the tetrazole rings are comparable to those in related molecules (Zhao et al., 2008; Fu et al., 2009).

In crystal structure, the intermolecular hydrogen bonds are formed by all H atoms of the water molecules with tetrazole N atoms or with the O atoms. The complex dinuclear cation units, [Na₂(H₂O)₈]²⁺, are linked in the crystal through O–H···O H-bonds into broad infinite cation-cation sheet parallel to the (0 0 1) plane. The two-dimensional sheets are linked by organic anions through O—H···N and O—H···O H-bonds into a three-dimensional framework (Table 1 and Fig.2).

Experimental

A mixture of 4-(1H-tetrazol-5-yl)pyridine 1-oxide (0.4 mmol) and NaOH (0.4 mmol), ethanol (1 ml) and a few drops of water sealed in a glass tube was maintained at 373 K. Colorless needle crystals suitable for X-ray analysis were obtained after 3 days.

While the permittivity measurement shows that there is no phase transition within the temperature range (from 100 K to 400 K), and the permittivity is 8.4 at 1 MHz at room temperature.