Lanthanide silasesquioxanes: monomeric and functionalised complexes

摘要

Lanthanide tris(silylamides) LnL(3) reacted with 2/3 equivalents of the trisilanol (C6H11)(7)Si7O9(OH)(3) 1 in THF to give the lanthanide silasesquioxanes [(C6H11)(7)Si(7)O(12)Ln(THF)(2)] which are dimeric in solution at 233 K. Reaction of LnL(3) with 1 equivalent of 1 in THF resulted in complete conversion of 1 into the trisilylated compound (C6H11)(7)Si7O9(OSiMe3)(3) as does reaction of LnL(3) with 2/3 equivalents of 1 in toluene. Reaction of [(C6H11)(7)Si(7)O(12)Ln(THF)(2)] with 1 equivalent of (Me2NCH2CH2)(2)NMe (PMDTA) gave the monomeric complex [(C6H11)(7)Si(7)O(12)Ln(PMDTA)]. The chloro-functionalised lanthanide silasesquioxane [(C6H11)(7)Si7O11(OSiMe3)LnCl(THF)] was formed by reaction of [(C6H11)(7)SiO(7)O(12)Ln(THF)(2)]with 1 equivalent of Me3SiCl. New compounds have been characterised by NMR spectroscopy and by elemental analysis. [References: 18]