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New trinuclear rhodium(III) complexes, [Rh 3 (μ 3 -O)(μ-CH 3 COO) 6 (L) 3 ] +  (L = imidazole (Him), 1-methylimidazole (Meim), and 4-methylpyridine (Mepy)) have been prepared. The Him, Meim, and Mepy complexes show reversible one-electron oxidation waves at E 1/2  = +1.12, +1.12, and +1.28 V vs Ag/AgCl, respectively, in acetonitrile. Electronic absorption spectra of the one electron oxidized species of these complexes and [Rh 3 (μ3-O)(μ-CH 3 COO) 6 (py) 3 ] +  (py = pyridine) (E 1/2  = +1.32 V ) were obtained by spectroelectrochemical techniques. While the Rh 3 (III,III,III) states show no strong visible absorption, the Rh 3 (III,III,IV ) species give a band at ca. 700 nm (ε = 3390-5540 mol dm -3  cm -1 ). [Ir 3 (μ 3 -O)(μ-CH 3 COO) 6 (py) 3 ] +  with no strong absorption in the visible region, shows two reversible one-electron oxidation waves at +0.68 and +1.86 V in acetonitrile. The electronic absorption spectrum of the one-electron oxidized species (Ir 3 (III,III,IV )) also shows some absorption bands (688 nm (ε, 5119), 1093 (2325) and 1400 (ca. 1800)). It is suggested that the oxidation removes an electron from the fully occupied anti-bonding orbital based on metal-dπ-μ 3 -O-pπ interactions, the absorption bands of the (III,III,IV ) species being assigned to transitions to the anti-bonding orbital.

Spectroelectrochemical Study of some μ 3 -Oxo-μ-acetato Trinuclear Rhodium(III) and Iridium(III) Complexes