Facile reduction of early transition metal halides with nonconventional, mild reductants. 6. A new, lower-temperature, solid-state synthesis of the cluster hexamolybdenum dodecachloride Mo6Cl12 from MoCl5, via chloromolybdic acid, (H3O)(2)[Mo-6(mu(3)

摘要

Reduction of MoCl5 with Bi in a seated borosilicate ampule at 350 degreesC, followed by sublimation of by-product BiCl3 and addition of aqueous hydrochloric acid, yielded chloromolybdic acid, (H3O)(2)Mo-6(mu(3)-Cl)(8)Cl-6 (.) 6H(2)O, in 80% yield (unoptimized) after double recrystallization. Chloromolybdic acid was thermolyzed to Mo6Cl12 in 95% yield. (C) 2003 Elsevier B.V. All rights reserved. [References: 82]