The endohedral dimetalloftillerene having a non-IPR fullerene cage, Ce-2@C-72, is spectroscopically and theoretically characterized. The C-13 NMR measurements display large temperature-dependent signals caused by paramagnetic shifts, indicating that the Ce atoms are located near the two fused pentagons in the C-72 cage. Theoretical. calculations are performed to clarify the metal position, which are in good agreement with the result obtained by the paramagnetic C-13 NMR analysis. Electrochemical measurements reveal that Ce-2@C-72 has particularly lower oxidation and higher reduction potentials than other endohedral dimetallofullerenes.