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

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 2(1)/n (No. 14)) with lattice parameters a = 6.8389(4) Angstrom, b = 5.5550(3) Angstrom, c = 14.345(1) Angstrom, beta = 99.922(6)degrees, V = 536.82(6) Angstrom(3), Z = 2. The refinement, led from 2423 unique reflections (I > 2 sigma(I)), converges to R(1)(F) = 0.024 and wR(2)(F-2) = 0.071. N2C4H14, (VO3)(2) crystallizes in a pyroxene-related structure; the new type of tetrahedral (VO3)(infinity) chains is compared to those already described in the literature. (C) 1996 Academic Press, Inc.