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Tri-, tetra-, and hexanuclear mixed-valence molybdenum clusters: structural diversity and catalysis of acetylene hydrogenation.

A series of novel cluster compounds comprising molybdenum in a low valence state was synthesized by means of a disproportionation of the dimeric compound [Mo+4 2 Cl4 (OCH3 )4 (CH3 OH)2 ] (1). The reaction of 1 with CH3 OH leads to the disproportionation of Mo+4 yielding an unusual mixed-valence cluster [Mo+3.5 4 Cl4 O2 (OCH3 )6 (CH3 OH)4 ] (2). By exploring this synthetic approach further, tri-{[Mo3 Cl3 (OCH3 )7 (CH3 OH)3 ] (3)}, tetra-{[Mo4 Cl4 (OCH3 )10 (CH3 OH)2 ] (4), [Mo4 Cl3 O(OCH3 )9 (CH3 OH)3 ] (5), [Mo4 Cl2 (OCH3 )12 (CH3 OH)2 ] (6)}, and hexanuclear {[Mo6 Cl4 O6 (OCH3 )10 (CH3 OH)2 ] (7)} molybdenum alkoxides were synthesized by the reaction of 1 with methanol and stoichiometric amounts of magnesium methoxide, thus providing a general facile access to the polynuclear methoxide complexes of a low-valence molybdenum. Due to the feasibility to adopt multiple oxidation states in a reversible manner and the documented competence of molybdenum alkoxide compounds to catalyze the reduction of inert molecules, including N2 , the synthesized compounds were expected to function as catalysts of small molecule substrates reduction/hydrogenation. Accordingly, the reduction of acetylene (C2 H2 ) to an ethylene (C2 H4 ) and ethane (C2 H6 ) mixture, in methanol (with water additives) serving as a reaction medium and a proton donor, and using sodium or europium amalgams as reducing agents, was performed in the presence of 2. Preliminary kinetic studies evidently point to a catalytic function of molybdenum species derived from 2, thus establishing the observed reactivity as a rare example of non-precious metal-catalyzed acetylene hydrogenation, providing, in addition, a convenient model for further mechanistic studies.

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