In this work, by the reaction of four different chloroglyoximes with 4’-Amminobenzo[15-Crown-5] in absolute ethanol, eight of new macrocylic glyoxime ether compounds and their Ni(II), Co(II) and Cu(II) complexes have been synthesized. For this, firstly chlorophenylglyoxime, p-tolylchloroglyoxime, p-chlorophenyl chloroglyoxime and 4’-biphenylchloroglyoxime were synthesized according to previously reported literatures. Then novel glyoxime derivatives with macrocyclic glyoxime ethers by the reactions between these compounds with 4’-amminobenzo[15-crown-5] were obtained. The complexes of these ligands with metal chlorid salts have been formed. Finally, the UV-VIS, IR, AAS and 1H NMR spectroscopic properties of these compounds were investigated and clarified by the help of the results of elemental analyses and the spectroscopic methods. The content of this book is based on an experimental study for my Ph.D thesis submitted to Selcuk University, Konya, Turkey in 2002.