The new dioxo(semicarbazone)vanadium(V) complexes cis-VO 2 L, where L = salicylaldehyde semicarbazone (L 1 ), salicylaldehyde 4-n-butylsemicarbazone (L 2 ), or salicylaldehyde 4-(2-naphthyl)semicarbazone (L 3 ), have been synthesized, characterized by 1 H and 13 C NMR and FTIR spectroscopy and tested for bioactivity as potential insulin-mimetic agents. All dioxovanadium(V) complexes exhibited essentially no in vitro insulin-mimetic activity, but the VO 2 L 2 complex developed activity in the presence of ascorbic acid, similar to that of vanadyl sulfate. The molecular structure of the novel
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