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Treatment of [MoCl 4 (THF) 2 ] with MO t Bu (M = Na, Li) does not result in simple metathetic ligand exchange but entails disproportionation with formation of the well-known dinuclear complex [( t BuO) 3 Mo≡Mo(O t Bu) 3 ] and a new paramagnetic compound, [Mo(O t Bu) 5 ]. This particular five-coordinate species is the first monomeric, homoleptic, all-oxygen-ligated but non-oxo 4d 1 Mo(V) complex known to date; as such, it proves that the dominance of the Mo═O group over (high-valent) molybdenum chemistry can be challenged. [Mo(O t Bu) 5 ] was characterized in detail by a combined experimental/computational approach using X-ray diffraction; UV/vis, MCD, IR, EPR, and NMR spectroscopy; and quantum chemistry. The recorded data confirm a Jahn-Teller distortion of the structure, as befitting a d 1 species, and show that the complex undergoes Berry pseudorotation. The alkoxide ligands render the disproportionation reaction, leading the formation of [Mo(O t Bu) 5 ] to be particularly facile, even though the parent complex [MoCl 4 (THF) 2 ] itself was also found to be intrinsically unstable; remarkably, this substrate converts into a crystalline material, in which the newly formed Mo(III) and Mo(V) products cohabitate the same unit cell.

Isolation of a Homoleptic Non-oxo Mo(V) Alkoxide Complex: Synthesis, Structure, and Electronic Properties of Penta-tert-Butoxymolybdenum