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Issue 5, 1998
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Synthesis and structural characterisation of rare-earth bis(dimethylsilyl)amides and their surface organometallic chemistry on mesoporous MCM-41

Abstract

Rare-earth silylamides of type [Ln{N(SiHMe2)2}3(thf )x] (Ln = Sc, Y, La, Nd, Er or Lu) have been prepared in high yield by reaction of 2.9 equivalents of Li[N(SiHMe2)2] with [LnCl3(thf )x] in n-hexane or thf, depending on the solubility of the rare-earth halide precursor. The complexes [Ln{N(SiHMe2)2}3(thf )2] (Ln = Y, La to Lu) are isostructural in the solid state, adopting the preferred (3 + 2, distorted) trigonal bipyramidal geometry, whilst [Sc{N(SiHMe2)2}3(thf )] has a distorted tetrahedral co-ordination geometry and short Sc  · · ·  Si contacts in the solid state. The reaction of [Y{N(SiHMe2)2}3(thf )2] with varying amounts of AlMe3 resulted in desolvation and alkylation with formation of AlMe3(thf ), {AlMe2[µ-N(SiHMe2]2}2 and heterobimetallic (Y/Al) species. The generation of surface-bonded ‘([triple bond, length half m-dash]SiO)xY[N(SiHMe2)2]y’ and ‘[triple bond, length half m-dash]SiOSiHMe2’ moieties via the grafting of [Y{N(SiHMe2)2}3(thf )2] onto the mesoporous silicate MCM-41 is described in detail. Consideration is given to the factors governing the siloxide formation and silylation reactions, and the thermal stability of the surface species.

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Article type: Paper
DOI: 10.1039/A705608G
Citation: J. Chem. Soc., Dalton Trans., 1998,0, 847-858
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    Synthesis and structural characterisation of rare-earth bis(dimethylsilyl)amides and their surface organometallic chemistry on mesoporous MCM-41

    R. Anwander, O. Runte, J. Eppinger, G. Gerstberger, E. Herdtweck and M. Spiegler, J. Chem. Soc., Dalton Trans., 1998, 0, 847
    DOI: 10.1039/A705608G

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