The paramagnetic complex of $(CO)_4ReL_2[L_2=$ 2,3-Bis(diphenylphosphino)maleic anhydride] was prepared both by the photochemically induced homolytic splitting of $Re_2(CO)_10withL_2and$ by the chemical reduction of $[(CO)_4ReL_2]SO_3CF_3.$ The $(CO)_4ReL_2$ compound was characterized by ESR spectrum. The spectrum exhibits three group of sextets arising from one $^{185.187}Re$ nucleus (Ⅰ= 5/2) and two equivalent $^31P$ nuclei (Ⅰ= 1/2). Infrared, ESR, and cyclic voltammetric data are reported for all of the complexes prepared in this study.