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The hydrothermal synthesis, single-crystal structure, and some physical properties of (CN 3 H 6 ) 2 ‚(VO 2 ) 3 (PO 4 )-(HPO 4 ), a new guanidinium vanadium(V) phosphate, are reported. This phase is built up from vertex-sharing layers of VO 6 octahedra, which adopt the hexagonal tungsten oxide motif. These octahedral layers are capped by P-O and P-OH entities resulting in anionic layers of stoichiometry [(VO) 3 (PO 4 )(HPO 4 )] 2-. Pairs of guanidinium cations are arrayed in the interlayer regions in a manner that suggests interactions may occur between these species. Crystal data consists of the following: (CN 3 H 6 ) 2 ‚(VO 2 ) 3 (PO 4 )(HPO 4 ), monoclinic, C2/c (No. 15), a ) 12.446 (3) Å, b ) 7.287(2) Å, c ) 17.819(5) Å, ) 97.23(3)°, Z ) 4.

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