Abstract
The syntheses of Os(SO 3F) 3 and Rh(SO 3F) 3 by the oxidation of osmium and rhodium metal powder with bis(fluorosulfuryl) peroxide, S 2O 6F 2, are reported. The conditions required for metal oxidation, extremely mild for osmium, and severe for rhodium, and the reaction times represent two extremes in the behaviour of noble metals towards S 2O 6F 2. For Os(SO 3F) 3 evidence from diffuse reflectance and infrared spectra as well as from bulk magnetic susceptibility measurements suggests polymorphism with a slow conversion occurring at room temperature in an excess of S 2O 6F 2.
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