Bis{4-[(4H-1,2,4-triazol-4-yl)iminomethyl]pyridinium} diaquapentanitratocerate(III)

Qiaozhen Sun; Feng Zheng; Xiaodan Sun; Wei Wang

doi:10.1107/S1600536808043109

. 2008 Dec 24;65(Pt 1):m124. doi: 10.1107/S1600536808043109

Bis{4-[(4H-1,2,4-triazol-4-yl)iminomethyl]pyridinium} diaquapentanitratocerate(III)

Qiaozhen Sun ^a,^*, Feng Zheng ^a, Xiaodan Sun ^a, Wei Wang ^a

PMCID: PMC2968024 PMID: 21581488

Abstract

The asymmetric unit of the title compound, (C₈H₈N₅)₂[Ce(NO₃)₅(H₂O)₂], contains one independent protonated 4-pyridylmethyleneamino-1,2,4-triazole cation and half of a centrosymmetric [Ce(NO₃)₅(H₂O)₂]²⁻ anion. The Ce atom coordinated by five NO₃ ⁻ anions and two water molecules, exhibiting a distorted 10-coordination. In the crystal structure, intermolecular O—H⋯N and N—H⋯O hydrogen bonds result in the formation of a supramolecular structure.

Related literature

For related compounds based on 4-amido-1,2,4-triazoles Schiff base ligands, see: Drabent et al. (2003 ▶, 2004 ▶); Wang et al. (2006 ▶). For the preparation of the ligand, see: Colautti et al. (1971 ▶).

Experimental

Crystal data

(C₈H₈N₅)₂[Ce(NO₃)₅(H₂O)₂]
M _r = 834.59
Monoclinic,
a = 10.322 (4) Å
b = 16.126 (6) Å
c = 17.595 (7) Å
β = 100.107 (4)°
V = 2883.2 (19) Å³
Z = 4
Mo Kα radiation
μ = 1.69 mm⁻¹
T = 293 (2) K
0.20 × 0.18 × 0.15 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2000 ▶) T _min = 0.682, T _max = 0.781
5464 measured reflections
2374 independent reflections
2164 reflections with I > 2σ(I)
R _int = 0.039

Refinement

R[F ² > 2σ(F ²)] = 0.024
wR(F ²) = 0.051
S = 1.02
2374 reflections
231 parameters
3 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.47 e Å⁻³
Δρ_min = −0.39 e Å⁻³

Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I. DOI: 10.1107/S1600536808043109/wk2094sup1.cif

e-65-0m124-sup1.cif^{(21.4KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808043109/wk2094Isup2.hkl

e-65-0m124-Isup2.hkl^{(116.8KB, 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
OW1—HW1A⋯N7	0.85 (2)	1.96 (2)	2.805 (3)	176 (3)
OW1—HW1B⋯N8ⁱ	0.85 (2)	2.03 (3)	2.876 (3)	178 (3)
N4—H4B⋯O4ⁱⁱ	0.86	1.95	2.804 (3)	172
N4—H4B⋯N2ⁱⁱ	0.86	2.69	3.518 (4)	162

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Symmetry codes: (i) Inline graphic ; (ii) .

Acknowledgments

The authors acknowledge financial support from the Innovation Program for College Students of Central South University (grant No. 081053308).

supplementary crystallographic information

Comment

In recent decades, metal coordination polymers containing 1,2,4-triazoles and their derivatives have been studied widely due to their versatile bridging modes with metal ions. Relatively few structurally characterized compounds based on 4-amido-1,2,4-triazoles Schiff base ligands have been reported (Drabent et al., 2004 and 2003; Wang et al., 2006) and these compounds exhibit dinuclear and tetranuclear structures. In this work, 4-Pyridylmethyleneamino-1,2,4-triazole coordinated with metal cerium is shown to generate a new coordination compound and its crystal structure reported.

As depicted in Fig.1, the Ce ion in this complex is ligated by eight oxygen atoms from five NO₃^- anions and two from H₂O molecules. And three NO₃^- anions are bound to Ce ion in bidentate fashion, while the other two in monodentate one. The nitrogen atoms of Schiff base ligand are not involved in the coordination to the Ce center as we supposed. The [Ce(NO₃)₅(H₂O)]^2- unit and the ligands are linked through the O—H···N and N—H···O hydrogen bonds, forming a three dimensional network.

Experimental

The ligand was prepared according to the reported literature (Colautti et al., 1971). The ligand (0.1 mmol, 0.017 g) and (NH₄)₂Ce(NO₃)₆ (0.1 mmol, 0.055 g) were mixed in acetonitrile and methanol of 1:1. After stirring at room temperature for four hours, the yellow solution was filtered and evaporated at room temperature. A few days later the red block crystals were obtained.