Two triple-decker dinuclear sandwich dysprosium complexes, which are represented as Dy-2[Pc(OC5H11)(8)](2)[Cor(FPh)(3)] (1) and Dy-2[Pc(OC5H11)(8)](2)Cor(ClPh)(3)] (2), were synthesized and characterized by spectroscopic and electrochemical methods in nonaqueous media. Their electronic structures were also investigated on the basis of TD-DFT calculations. The sandwich triple-decker nature with the molecular conformation of [Pc(OC5H11)(8)]Dy[Cor(FPh)(3)]Dy[Pc(OC5H11)(8)] for compound 1 was unambiguously revealed by single-crystal X-ray diffraction analysis and showed each dyprosium ion to be octacoordinated by the isoindole and pyrrole nitrogen atoms of an outer phthalocyanine ring and the central corrole ring, respectively. In addition, the magnetic properties of both compounds have also been characterized for exploring the functionalities of these types of triple -decker complexes.