Further studies of fluoride ion entrapment in octasilsesquioxane cages; X-ray crystal structure studies and factors that affect their formation

Taylor, Peter G.; Bassindale, Alan R.; El Aziz, Youssef; Pourny, Manuel; Hursthouse, Michael B. and Coles, Simon J. (2012). Further studies of fluoride ion entrapment in octasilsesquioxane cages; X-ray crystal structure studies and factors that affect their formation. Dalton Transactions, 41(7) pp. 2048–2059.

DOI: https://doi.org/10.1039/C1DT11340B

Abstract

A range of fluoride-encapsulated octasilsesquioxane cage compounds have been prepared using the TBAF route. Our studies suggest that whilst it is relatively straightforward to prepare fluoride-encapsulated octasilsesquioxane cage compounds with adjacent sp² carbons, leading to a range of aryl and vinyl substituted compounds, the corresponding sp³ carbon derivatives are more capricious, requiring an electron withdrawing group that can stabilize the cage whilst not acting as a leaving group. Analysis by X-ray crystallography and solution ¹⁹F/²⁹Si NMR spectroscopy of R8T8@F⁻ reveal very similar environments for the encapsulated fluoride octasilsesquioxane cages. Migration of a fluoride ion from inside the cage to outside the cage without breaking the T8 framework and the possibility of encapsulating other anions within silsesquioxane cages have been also investigated.

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