Synthesis and Structural Verification of an ArI(OTf) 2 , NO 2 -Ph-I(OTf) 2 .

PhI(OTf) 2 and related ArI(OTf) 2 species have been incorrectly invoked as intermediates in oxidation reactions for many years. We recently established that such compounds did not yet exist but remain an attractive target. Here we describe the synthesis, isolation, and structural characterization of NO 2 -PhI(OTf) 2, which is resistant to decomposition and more reactive than PhI(OTf)(OAc), the species previously misidentified as PhI(OTf) 2 .