Abstract
Different solid aluminum isopropoxide fluorides AlFx(OiPr)3−x with varying Al/F molar ratios (from 4:1 to 1:3) were synthesized following the fluorolytic sol−gel synthesis route. The subsequent characterization by multinuclear (27A1, 19F, 1H, and 13C) and multidimensional solid-state MAS NMR techniques enables the characterization of local structural features in these solids. The mechanism of the fluorolytic sol−gel process deduced earlier was strongly supported by following changes of the local structures in these compounds in dependence on their composition. For the first time, the existence of four-fold fluorine-coordinated Al species (AlF4) was proven as intermediates in the case of low fluorine supply. Additionally, a plausible pathway for the formation of monofluorinated Al3(OiPr)8F·D (DMSO, pyridine) is given, which was isolated as single crystals recently. The appropriate spectra point out that similar species exist also in powders of pyridine- and DMSO-free reaction mixtures.
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