Abstract: The complex [Re(CO)₃(bipy)(ClO₄)] (bipy = 2,2ʹ-bipyridine) was prepared by the reaction of [Re(CO)₃(H₂O,EtOH)₃](ClO₄) with bipy in aqueous ethanol, followed by crystallization from dichloromethane. The composition and structure of the complex were determined by single crystal X-ray diffraction analysis. The complex has a molecular octahedral structure with bidentate coordination of bipy and inner-sphere monodentate coordination of perchlorate ion in the fac-position to bipy. The complex was also characterized by IR and UV-visible absorption spectroscopy.