Chain Iridium Carbonyl Halides

Hieber et al.s originally isolated Ir(CO)3Cl l0 from the products of the reaction of finely divided IrCl3 H20 with CO (1 atm) at 150°C, but they formulated the compound as Ir(CO)3Cl. The preparation given below is due to Fischer and Brenner,6 who also assigned the integral stoichiometry. The method for prepar- 

K2IrCl6 + HCOOH conc HCI K0 6oIr(CO)2Cl2-0.5H20 

The following operations are all carried out under oxygen-free nitrogen using standard Schlenk techniques.9,10 Solvents and liquid reagents are degassed before use. 

A 100-mL, two-necked flask with 24/40 T joints is charged with potassium hexachloroiridate(IV) (2.0 g, 4.1 mmole), concentrated hydrochloric acid (10 

Shriver, The Manipulation of Air-Sensitive Compounds, McGraw-Hill Book Co., Inc., New York, 1969, Chap. 7. 

---