Homo and heterotrinuclear acetates are unique compounds having μ3-oxo bridge and many interesting properties of such compounds are derived from this structure. Some undergraduate inorganic textbooks discuss several aspects of these compounds and we present here an undergraduate experiment for the high-yield synthesis of [Fe2MO(CH3CO2)6(H 2O)3], with M = Fe3+, Co2+ and Ni2+, as well as their characterization using infrared spectroscopy and cyclic voltametry. The proposed experiment gives the opportunity to discuss several concepts of coordination chemistry that follow the characterization techniques, such as: types of acetate coordination, reversibility of electrochemical processes, quelate and trans effects and lability.18151820Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)