A new bis(dioxime) ligand (H4L) containing the diphenyl ether moiety has been prepared by reacting 3,3',4,4'-tetraaminodiphenyl ether (1) with 2,3-butanedione monoxime (2). Dinuclear copper(II) and cobalt(III) complexes of H4L exhibit a metal-ligand ratio of 2:1 and the ligand coordinates through the 4 nitrogen atoms, as do most bis(dioximes). The [Cu-2(H2L)](ClO4)(2) molecule coordinates to the other two copper(II) ions through the deprotonated oximate oxygens to yield a tetranuclear structure, doubly-bridged by the oximate groups in a cis arrangement. The structure of bis(dioxime) and its complexes were identified by elemental analyses, H-1-, C-13-n.m.r, i.r and m.s. spectral data.