Pentaammine dinitrogen osmium II Iodide

Commercial grade (NH4)2[OsCl6] (2.37 g) is added in small portions to ice-cold hydrazine hydrate (85 %, 23 ml). After the vigorous effervescence subsides, the solution is refluxed, with stirring, for 15 hr. A yellow precipitate of [Os(NH3)5(N2)]Cl2 is formed and is filtered from the cooled mixture, washed with ethanol and ether, and air-dried. To the filtrate is added solid potassium iodide until precipitation of [Os(NH3)5(N2)]l2 is complete. The product is collected on a filter and washed and dried as above. The chloride salt is converted to the iodide by metathesis using solid potassium iodide until precipitation is complete. Total yield of [Os(NH3)s(N2)]l2 2.36 g (78%). Anal. Calcd. for OSN7H15I2 N, 17.6. Found N, 17.0. Infrared spectrum, v(N2)(iodide salt) = 2033 (vs) 2043 (sh). 

Inorganic Syntheses, Volume XVI Edited by Fred Basolo Copyright 1976 by McGraw-Hill, Inc. 

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