The novel (E,E)-dioxime 5,6:13,14-dibenzo-9,10-benzo(15-crown-5)-2,3-bis(hydroxyimino)-7,12-dioxo-1,4,8,11- tetraazacyclotetradecane (H(2)L) has been synthesized by the reaction of 4',5'-diaminobenzo(15-crown-5) with N,N'-bis(2-carbomethoxyphenyl)diaminoglyoxime (1). Only mononuclear Co-III and Ru-II complexes with a metal/ligand ratio of 1:2 have been isolated. The cobalt(III) complex bridged with BF2+ is achieved with H-bonded cobalt(III) complex and borontrifluoride ethyl ether complex. The reaction of BF2 bridged cobalt(III) complex with bis(benzonitril)palladium(II) chloride gives a trinuclear complex. The structures of dioxime and its complexes are proposed according to elemental analyses, H-1 and C-13-NMR, IR and mass spectral data.