In this study, anti-1-acetyl-l-cyclohexenylchloroglyoxime (C8H U C1N2O2) has been synthesized by chlorination of anti-1-acetyl-1-cyclohexeneglyoxime. As a result of the reaction of C8HnC1N2O2with aryl- or arylalkylamines in ethanol between -10 °C and -15 °C , unsymmetrical vic-dioximes were obtained and the obtained products were named as: anilino-1-acetyl-1-cyclohexeneglyoxime (C14H17N3O2), benzylamino -1-acetyl-1-cyclohexeneglyoxime (C15H19N3O2), p-toluidino -1-acetyl-1-cyclohexeneglyoxime (C15H19N3O2) respectively. Their transition metal complexes have been synthesized. The form of the obtained Ni(II) and Cu(II) complexes were found as square-planer as it is known usually. 'H n.m.r, conductivity measurements, magnetic properties, i.r spectra and elemental analyses data of ligands and complexes are given. In addition to this, thermal characterizations of the ligands and their complexes have been investigated.