[HN(n‐C4H9)3]3M(CN)8 4 H2O, where M = Mo or W, is formed as a light yellow or white water insoluble precipitate by adding tri‐n‐butylammonium ions to M(CN) 83−, obtained by oxidation of K4Mo(CN)8· 2H2O or K4W(CN)8·2H2O with concentrated nitric acid. The precipitates are soluble in methyl and ethyl alcohol, benzene and acetonitrile. Crystal data were determined for crystals of the Wv compound. The tri‐n‐butylammonium compound can be nearly quantitatively converted to Cs3M(CN)8· 2H2O with CsCl, which is fairly soluble in methyl alcohol. Crystal data were determined for light yellow crystals obtained by recrystallization. The potassium complex of Wv can be prepared by using potassium acetate instead of CsCl.
K4W(CN)8 · 2 H2O was prepared by the reduction of WO 42− (in potassium cyanide medium) by KBH4. The reduction proceeds on the slow, drop‐by‐drop addition of concentrated acetic acid. The synthesis is simple and efficient because the reduction and complexation are accomplished at the same time.
K4Mo(CS)8 · 2 H2O was prepared by the reduction of MOO2− by KBH4 in potassium cyanide medium. The reduction proceeds during the slow addition of concentrated acetic acid. The synthesis is efficient because reduction and complexation are accomplished at the same time.
scite is a Brooklyn-based organization that helps researchers better discover and understand research articles through Smart Citations–citations that display the context of the citation and describe whether the article provides supporting or contrasting evidence. scite is used by students and researchers from around the world and is funded in part by the National Science Foundation and the National Institute on Drug Abuse of the National Institutes of Health.