Reaction of metal free homobinuclear phthalocyanine H2Pc(OR)(6)-H2Pc(OR)6 with M(OAc)(2) (M = Co, Ni) in refluxing dimethyl formamide led to the isolation of the binuclear phthalocyaninato metal complexes MPc(OR)(6)-MPc(OR)6 (M = Co, Ni) (1, 2). These binuclear phthalocyanine compounds were characterized by a series of spectroscopic methods including mass, H-1 NMR, electronic absorption, and IR spectroscopy in addition to elemental analysis. In particular, their binuclear phthalocyanine nature has been directly revealed on the basis of single crystal X-ray diffraction analysis of the homo-dicobalt species CoPe(OR)(6)-CoPc(OR)(6) (1) for the first time. In addition, their electrochemical data over these binuclear phthalocyanine compounds have also been provided by cyclic voltammetry measurements. (C) 2014 Elsevier Ltd. All rights reserved.