Bis acetonitrile decacarbonyltriosmium

This solid is suspended in 2 mL of acetonitrile and transferred by pipette to a 25-mL round-bottomed flask. The supernatant liquid is returned to the original flask and the procedure repeated as many times as is necessary to transfer all the solid. At this stage, evaporation of the solvent gives slightly impure Os3(CO)10(CH3CN)2 in yields between 85 and 95%. The trace brown 

Infrared absorptions in the carbonyl region for Os3(CO)10(CH3CN)2 in CH2C12 are 2079(w), 2025(sh), 2021 (vs), 1983(m), 1960(w)cm-1. The acetonitrile ligands are readily displaced by other donor ligands See Ref. 2. 

The complex Os4H4(CO)12 was first synthesized in low yield by acidification of the anions formed in the reaction of methanolic potassium hydroxide and 

A suspension of Os3(CO)12 (2g) in hexane (60 mL) is placed into a stirred stainless steel autoclave (450-mL total capacity), under a nitrogen atmosphere.5 After the autoclave is sealed, the gases are evacuated and the autoclave is pressurized to 25 atm of hydrogen. The autoclave is then heated with stirring to 140 °C for 24 h. After cooling, the gas is slowly vented. After coming to atmospheric pressure the autoclave is flushed with an atmosphere of nitrogen, and opened. 

Pale yellow crystals of Os4 H4(CO)j 2 are separated by decantation of the supernatant solution. The sample thus obtained is sufficiently pure for most purposes. The yield of the Os4H4(CO)12 is usually in the range from 80 to 85% (1.8 g). Checkers report a yield of 45% for a smaller scale reaction, namely, 1 g Os3(CO)12 in 30 mL of solvent in an autoclave of 125-mL total capacity. 

Further purification may be carried out by extracting the solids with chloroform (200 mL) in a Soxhlet extractor. 

Using the apparatus and sublimation procedure for trimethylamine oxide described in Section A a suspension of Os3(COj2) (0.5 g, 0.55 mmol) is 

Johnson and J. Lewis, Inorg. Synth., 13,93 (1972). See also section 57 in this volume. 

Inorganic Syntheses, Volume 28 Edited by Robert J. Aagebci 1990 by Inorganic Syntheses, Inc. 

The water should be added with care since too much will precipitate some (PPh3)2NCl. The suspension is stirred further for 1 h. The precipitate is then filtered in air, washed with 5 mL of distilled water and 5 mL of cold methanol, and dried in vacuo overnight to give 58%, 0.414 g, (0.292 mmol) of / -nitrido bis(triphenylphosphorusXl +) /i-carbonyl-decarbonyl-/ -hydrido-triosmate(l —). 

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