Dibenzo [e,k]-2,3-bis(hydroxyimino)-1,4-diaza-7,10-dithia-2,3,8,9-tetrahydrocyclododecine (LH4) has been prepared from cyanogendi-N-oxine and 1,2-bis(o-aminophenylthio)ethane (APT). The structure of this vic-dioxime has been determined as anti-isomer according to its 1H n.m.r, and i,r spectral data. The trinuclear complexes of this compound, (LH)2M3, where M = Cu(II), Ni(II) and Pd(II), have been obtained. In these complexes the metals coordinate to the sulfur atoms of thioethers and the nitrogen atoms of the aza and oxime groups. Also mononuclear complexes of this vic-dioxime, the using Ni(II), Co(II), Cu(II) and UO2(VI), have been isolated. The structures of these complexes and the vic-dioxime were identified by using 1H n.m.r, i,r, and uv-visible spectral data and elemental analysis.