Cyclooctadiene bis pyridine iridium I Hexafluorophosphate

The more volatile acetone is then largely removed by evaporating the solution gently at room temperature on a vacuum line for 10 min or until the volume of the mixture falls to about 10 mL. The yellow solid [Ir(cod)py2][PF6] precipitates during this process and can be isolated by filtration through a frit under nitrogen. The solid is washed with three portions of 5 mL of degassed water, and dried under vacuum. Yield 0.73 g (97%). 

The complex is slightly air-sensitive even in the solid state and should be kept under nitrogen or used immediately for the following preparation. The product 

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In a 100-mL Schlenk tube equipped with a stirring bar, 0.30 g (0.5 mmol) of (T] -l,5-cyclooctadiene)bis(pyridine)iridium(I) hexafluorophosphate is dissolved in 20 mL of deoxygenated methanol under nitrogen. To this solution is added 0.17 g (0.6 mmol) of tricyclohexylphosphine (tcyp) [Strem Chemical]. The orange solution is stirred for 15 min at room temperature, during which time the product begins to crystallize from the solution. The mixture must not be heated. The methanol is removed under reduced pressure at room temperature until about 5 mL remains. Diethyl ether (10 mL) is added, and the reaction mixture is cooled in an ice bath for 30 min. The orange crystalline product is isolated by filtration, washed three times with 5-mL portions of diethyl ether, and dried under vacuum. Yield 0.39 g (97%). 

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