Abstract
A new vanadium(III) phosphate, (NH 4)[V(PO 4)F], has been synthesized by using mild hydrothermal conditions under autogeneous pressure. The crystal structure has been solved from X-ray single crystal data. The compound crystallizes in the Pnna orthorhombic space group, with the unit-cell parameters a=12.982(2), b=10.608(1), c=6.4789(6) Å and Z=8. The final R factors were R 1=0.077 [all data] and w R 2=0.068. The crystal structure consists of a three-dimensional framework formed by VO 4F 2 octahedra and tetrahedral (PO 4) 3− phosphate anions. The vanadium(III) cations from the VO 4F 2 octahedra are linked through the fluorine atoms giving rise to zig-zag chains. The ammonium cations are located in the cavities of the structure compensating the anionic charge of the [V(PO 4)F] − inorganic skeleton. The IR spectrum shows the characteristic bands of the phosphate anion. The diffuse reflectance spectroscopy allowed us to calculate the Dq and Racah parameters. The values are Dq=1540, B=505 and C=2460 cm −1. Magnetic measurements indicate the existence of weak ferromagnetic interactions.
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