Hydrothermal synthesis and structure of one-dimensional Co(dien) 2(VO 3) 3·(H 2O) (dien=diethylenetriamine)

Abstract

One-dimensional Co(dien) 2(VO 3) 3·(H 2O) was prepared from the hydrothermal reaction of NH 4VO 3, Co 2O 3, diethylenetriamine (dien) and H 2O at 130 °C. The compound crystallizes in the monoclinic system, space group P2 1/ c with a=16.1581(6) Å, b=8.7006(3) Å, c=13.9893(4) Å, β=103.1483(11)°, V=1915.13(11) Å 3, Z=4, and R 1=0.0268 for 3060 observed reflections. Single crystal X-ray diffraction revealed that the structure is composed of infinite one-dimensional chains formed by corner-sharing VO 4 tetrahedra with Co(dien) 3+ complex cations and crystallization water molecules occupying the interchain positions, which are held together to a three-dimensional network via extensive hydrogen-bonding interactions. The compound, with a new zig-zag conformation of metavanadate chains, is the first example of vanadium oxides incorporating trivalent transition metal coordination groups. Other characterizations by elemental analysis, IR and thermal analysis are also described.