SYNTHESIS AND CRYSTAL-STRUCTURE OF A NEW VIV VV MIXED-VALENCE MICROPOROUS COMPOUND V3P2O13(H2O)2, H3N(CH2)3NH3/

Hitherto unknown vanado(IV, V)phosphate, ideally V(IV)V2(V)P2O13 (H2O) 2, H3N(CH2)3NH3 was obtained by hydrothermal synthesis (453 K, 24 hr, autogeneous pressure) from a mixture of V2O5, P2O5, 1,3-diaminopropane , and H2O in the ratio 1:1:1.3:1:80. It is orthorhombic (space group P nma (No. 62)) with a = 10. 567(1) angstrom, b = 16.970(2) angstrom, c = 8.413(1) angstrom, V = 1508.1(7) angstrom3, Z = 4. The three-dimensi onal network is built up from the corner linkage of pentameric seconda ry building units based on two PO4 tetrahedra, one VO5 square pyramid, and two VO5(H2O) octahedra sharing vertices. The framework delimits l arge 10-membered ovoid zigzag tunnels along [100] and smaller eight-me mbered ones along [010]. The true composition of the solid is discusse d. The diprotonated amines are inserted in the 10-membered ovoid chann els, whose free aperture is 7.30 x 4.00 angstrom. (C) 1994 Academic Pr ess, Inc.