Under the action of CS2 and KOH in dioxane solution, calixarene derivative 2 was converted into calixarene derivative containing xanthate salt (3) and its Ni2+ complex compound 4 was prepared by self-assembled reaction with NiSO4 further. The structures of new compounds were confirmed by elemental analyses, IR, UV, 1H NMR, MS techniques. The Ni2+ of complex compound 4 was in high-spin state by its ESR spectrum.
