Synthesis and crystal structure of Na1+xV4P4O17(OH) (x ≈ 1.44)

Abstract Hydrothermal synthesis starting from Na0.46VOPO4 · 1.58H2O leads to a new mixed-valence sodium vanadium phosphate: Na2.44V4P4O17(OH) (orthorhombic, space group Pnma; Z = 4; a = 13.723(5) A, b = 6.314(2) A, c = 16.139(4) A; R = 0.032 for 2659 reflections). In this phase, the interconnection of three complex types of infinite chains, built from VO6 octahedra and PO4 tetrahedra, sometimes edgeshared, defines tunnels partly occupied by a portion of the sodium atoms.