Acetonitrile Complexes of Selected Transition Metal Cations

ACETONITRILE COMPLEXES OF SELECTED TRANSITION METAL CATIONS 

Since these cationic, weakly solvated transition metal complexes are reactive towards atmospheric moisture, all manipulations should be performed using standard inert atmosphere techniques. 

The compound [Pd(CH3CN)4][BF4]2 is a moisture-sensitive pale yellow crystalline material. It is very soluble in acetonitrile and nitromethane but virtually insoluble in less polar organic solvents such as diethyl ether, chloroform, and benzene. The HNMR spectrum in CD3N02 exhibits a 

The apparatus and techniques used are similar to those for the synthesis of tetrakis(acetonitrile)palladium(II) bis[tetrafluoroborate(l —)]. A 100-mL round-bottomed flask (B) is charged with 2.0 g (7.6 mmol) of hexacar-bonylmolybdenum (Alfa) and 1.77 g (15.2 mmol) of nitrosyl tetrafluorobo-rate (Aldrich, sublimed 220°C, 10-3torr). Dry acetonitrile (50mL) is added and the solution is allowed to stir at 25 °C until no hexacar-bonylmolybdenum remains (6 h). 

The resulting dark emerald green solution is filtered and the filtrate is concentrated to near dryness in vacuum. Diethyl ether (40 mL) is added and the solution is vigorously stirred to cause precipitation of the dark green molybdenum complex. The solution is filtered and the solid washed with two 5-mL portions of diethyl ether. The precipitate is dried in vacuum (10 3 torr, 25 °C) to afford 3.36 g (90%) of dark emerald green cis-tetrakis(acetonitrile)-dinitrosylmolybdenum(II) bis[tetrafluoroborate(l —)]. 

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Acetonitrile Complexes of Selected Transition Metal Cations 129... 

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