13569-59-0Relevant articles and documents
Chemistry of polynuclear metal halides. II. Preparation of polynuclear niobium chloride and bromide
Fleming, Peter B.,Mueller, Leta A.,McCarley, Robert E.
, p. 1 - 4 (2008/10/08)
Improved preparations leading to the compounds Nb6X14·8H2O (X = Cl, Br) are described. High yields of Nb6Cl122+ were obtained by the high-temperature reaction of KCl and Nb3Cl8 which proceeds via 14KCl + 5Nb3Cl8 = 2K4Nb6Cl18 + 3K2-NbCl6. Extraction of this reaction mixture with water provides a convenient route to Nb6Cl14·8H2O. The attempted formation of Nb6Cl14 via direct reduction of NbCl5 with aluminum was unsuccessful. However, aluminum reduction of NbBr5 provided an unidentified anhydrous product from which yields of up to 35% Nb6Br122+ were extracted. Equilibration reactions involving niobium and Nb3Br8 at temperatures up to 975° gave no evidence for phases having Br: Nb 6Cl122+ and Nb6Br122+ are given. Copyright 1967 by the American Chemical Society.