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Issue 9, 2009
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One-pot synthesis of lithium alkylzinc alkoxo heterocubanes with a LiZn3O4 core as suitable organometallic precursors for Li-containing ZnO nanocrystals

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Abstract

A convenient and efficient synthesis of the stable monolithium alkylzinc alkoxo cubanes {Li(thf)(RZn)3(OR′)4} [R = Me, R′ = iPr (1), tBu (2); R = Et, R′ = iPr (3), tBu (4)] is reported. They are well soluble in organic solvents and suitable molecular precursors for the formation of Li-containing ZnO nanoparticles. The compounds are accessible by a convenient one-pot reaction of the respective dialkylzinc with lithium alkoxides in the presence of water and can be isolated as white solids in 35–50% yield. Higher yields (80–85%) for 1 and 3 can be achieved by applying excess iPrOH instead of H2O as protolysis source. The compounds 1–4 were characterized by elemental analyses, multinuclear NMR and FT-IR spectroscopy, and single-crystal X-ray diffraction analysis (1 and 2). Interestingly, thermal treatment of solutions of 1 and 2, respectively, in anhydrous benzyl alkohol at 190 °C yields pure and highly crystalline Li-containing ZnO nanoparticles as evidenced by powder X-ray diffraction analysis (PXRD), Transition Electron Microscopy (TEM), FT-IR and 7Li MAS NMR spectroscopy.

Graphical abstract: One-pot synthesis of lithium alkylzinc alkoxo heterocubanes with a LiZn3O4 core as suitable organometallic precursors for Li-containing ZnO nanocrystals

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Publication details

The article was received on 23 Sep 2008, accepted on 14 Nov 2008 and first published on 08 Jan 2009


Article type: Paper
DOI: 10.1039/B816623D
Citation: Dalton Trans., 2009,0, 1516-1521
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    One-pot synthesis of lithium alkylzinc alkoxo heterocubanes with a LiZn3O4 core as suitable organometallic precursors for Li-containing ZnO nanocrystals

    S. Jana, Y. Aksu and M. Driess, Dalton Trans., 2009, 0, 1516
    DOI: 10.1039/B816623D

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