Two 2D metal–calixarene aggregates were designed and assembled by M₄-TC₄A (M = Fe, Co; TC₄A = p-tert-butylthiacalix[4]arene) SBUs and {MCl₂} units with isonicotinic acid molecules, which presents a possible way to build the extended metal–calixarene assemblies incorporating pre-designed nanocages using multifunctional linkers.