Abstract
A new mixed-valence vanadium diphosphate, KV 3P 4O 16, was synthesized by solid-state reaction and its structure was determined from single-crystal X-ray diffraction data. Brown crystal of KV 3P 4O 16 crystallizes in the monoclinic space group P2 1/ m (No. 11) with a = 5.201(1), b = 12.661(2), c = 9.476(2) Å, β = 94.11(2)°, V = 622.4(2) Å 3, Z = 2, R = 0.0293, R w = 0.0333 for 1108 unique reflections with I > 2.5 σ( I). Edge-sharing pairs of VO 6 octahedra are connected by sharing corners to form strings along the b axis. The strings formally contain V 3.5+ (one V 3+ and one V 4+) and are connected through P 2O 7 groups such that layers in the ab plane are formed. Adjacent layers are linked in three dimensions by VO 2+ vanadyl groups. The structure consists of tunnels where the K + cations are located. The structural formula is K(V 2O)(VO)(P 2O 7) 2. Variable-temperature powder magnetic susceptibility data confirm the presence of one V 3+ and two V 4+ ions per formula unit.
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