[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.
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