A newvic-dioxime, [N,N′-Bis(3′,4′-didodecyloxyphenyl)diaminoglyoxime](H2L) has been prepared from 3,4-didodecyloxyaniline and(E.E)-dichloroglyoxime. The(E,E)- and(E,Z)-forms of Ni(II) complex have been isolated, but palladium complex could be isolated only as(E,E)-isomer. The mesomorphic properties of these complexes were investigated by polarizing microscopy, differential scanning calorimetry (DSC) and X-ray diffraction analysis. These complexes form columnar hexagonal disordered (Colhd) mesophases. All complexes are very soluble in common organic solvents.1H and13C NMR, IR, MS and UV/Vis data are presented.