Single-crystalline rhenium trioxide (ReO3) nanocubes have been prepared for the first time without the need of surfactants via controlled reduction of rhenium (VII) oxide (Re2O7), sandwiched between silicon wafers at 250 degrees C. The metallic ReO3 nanocubes are magnetic and possess surface plasmon resonance (SPR) bands down to the NIR region. The nanocubes also show very high catalytic activity toward the photodegradation of methyl orange (MO) under ambient conditions. A mechanism has been proposed to account for the photodegradation process. (C) 2013 Elsevier Inc. All rights reserved.