Hydrothermal synthesis and structure determination of 1,4-diaminobutane metavanadate

Abstract

N2C4H14, (VO3)2 is a metavanadate intercalated by organic molecules. It has been hydrothermally prepared (453 K, 24 hr, autogenous pressure) from a mixture of V2O5:HF:1,4-diaminobutane:H2O in the molar ratio 1:2:1.5:80. Its structure was solved by single crystal X-ray diffraction. It is monoclinic (space group P 21/n (No. 14)) with lattice parameters a = 6.8389(4) Å, b = 5.5550(3) Å, c = 14.345(1) Å, β = 99.922(6)°, V = 536.82(6) Å3, Z = 2. The refinement, led from 2423 unique reflections (I > 2σ(I)), converges to R1(F) = 0.024 and wR2(F2) = 0.071. N2C4H14, (VO3)2 crystallizes in a pyroxene-related structure; the new type of tetrahedral (VO3)∞ chains is compared to those already described in the literature. © 1996 Academic Press, Inc.