Preparation of aluminum(III) (bis(amido)pyridine)(thiolate) complexes: unexpected transmetalation mediated by LiAlH(4).

Inorganica Chimica Acta
Yosra M BadieiDavid P Goldberg

Abstract

Treatment of an unsymmetrical bis(imino)pyridyl-thiolate zinc(II) complex [Zn(II)(LN(3)S)(OTf)] (1) with LiAlH(4) results in the double reduction of the two imino groups in the ligand backbone, and at the same time causes a rare transmetalation reaction to occur. The products formed in this reaction are two novel aluminium(III) bis(amido)pyridyl-thiolate complexes [(R,S/S,R-[Al(III)(LH(2)N(3)S)(THF)] (2a) and [(R,R/S,S-[Al(III)(LH(2)N(3)S)(THF)] (2b), which are diastereomers of each other. These complexes have been characterized by single-crystal X-ray diffraction and (1)H NMR spectroscopy. Single crystal X-ray structure analysis shows that the Al(III) ion is bound in an almost idealized square pyramidal geometry in 2a, while being held in a more distorted square pyramidal geometry in 2b. The major difference between 2a and 2b arises in the orientation of the terminal methyl groups of the ligand backbone in relation to the Al(III)N(3)S plane. These two complexes are crystallized at different temperatures (room temperature vs -35 °C), allowing for their separate isolation. Structural analysis shows that these complexes are reduced by the formal addition of one hydride ion to each imino group, resulting in a deprotonated bis(amid...Continue Reading

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Jan 7, 2011·Journal of the American Chemical Society·Yosra M BadieiDavid P Goldberg

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