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Reaction of Mo(CO)6 with Bu4NI and I2 in diglyme yielded a new butterfly MoIII cluster [Mo4OI12]2–. The structure of tetraphenylphosphonium salt was determined by X‐ray single crystal diffraction. Ph4P+ and Bu4N+ salts were further characterized by elemental analysis, mass spectrometry, energy‐dispersive X‐ray (EDX), IR, Raman, and UV/Vis spectroscopy and CVA studies. The cluster anion has a butterfly...
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