Oxygen-deficient molybdenum trioxide nanorods of composition MoO 2.987 (orthorhombic, a = 3.951(2) Å, b = 13.856(1) Å, c = 3.700(1) Å) were synthesized by a hydrothermal process (150–180°C, 30–50 h). MoO 3 − δ particles were 60–90 nm in diameter; their lengths were several micrometers. X-ray photoelectron and IR spectra of these nanorods were studied, The nanorods had weak paramagnetism, signifying the existence of molybdenum(V) ions in their structure.