Reaction of Mo(CO) 6 with Bu 4 NI and I 2 in diglyme yielded a new butterfly Mo III cluster [Mo 4 OI 12 ] 2-. The structure of tetraphenylphosphonium salt was determined by X-ray single crystal diffraction. Ph 4 P + and Bu 4 N + salts were further characterized by elemental analy-* Dr. M. Mikhaylov 438 sis, mass spectrometry, energy-dispersive X-ray (EDX), IR, Raman, and UV/Vis spectroscopy and CVA studies. The cluster anion has a butterfly array of molybdenum atoms and can be represented as [Mo 4 (μ 4 -O)(μ 3 -I) 2 (μ 2 -I 4 )I 6 ] 2-.