Pentacarbonylchlororhenium Alternate Procedure

Reagent-grade CCI4 is stirred for 2 h over P4O10 (50 mLCCl4/0.5 g P4O10), and then distilled (25 mL) into a 50-mL Schlenk flask equipped with a Teflon- 

The solvent and excess chlorine are removed under continuous vacuum (0.1 mm) at room temperature. The white solid is transferred to a sublimator and sublimed at 80-85° and 0.1 nun. Yield 0.30 g (84.4%, based on [Re2(CO)io] [Checkers yield 75%]. 

---