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The apparent Sc(3+) adduct of [Fe(IV)(O)(TMC)](2+) (1, TMC = 1,4,8,11-tetramethyl-1,4,8,11-tetraazacyclotetradecane) has been synthesized in amounts sufficient to allow its characterization by various spectroscopic techniques. Contrary to the earlier assignment of a +4 oxidation state for the iron center of 1, we establish that 1 has a high-spin iron(III) center based on its Mössbauer and EPR spectra and its quantitative reduction by 1 equiv of ferrocene to [Fe(II)(TMC)](2+). Thus, 1 is best described as a Sc(III)-O-Fe(III) complex, in agreement with previous DFT calculations (Swart, M. Chem. Commun. 2013, 49, 6650.). These results shed light on the interaction of Lewis acids with high-valent metal-oxo species.

journal of the american chemical society

Spectroscopic Identification of an FeIII Center, not FeIV, in the Crystalline Sc–O–Fe Adduct Derived from [FeIV(O)(TMC)]2+