Journal
POLYHEDRON
Volume 26, Issue 18, Pages 5193-5202Publisher
PERGAMON-ELSEVIER SCIENCE LTD
DOI: 10.1016/j.poly.2007.07.037
Keywords
hexafluoroniobate and hexafluorotantalate anions; oxonium ions; crown ethers; hydrogen bond; crystal structure
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Two synthetic pathways, the interaction of Nb2O5 or Ta2O5 with an aqueous solution of hydrofluoric acid, HF, in the presence of 18crown-6 (18C6), 15-crown-5 (15C5), benzo-15-crown-5 (B15C5) or benzo-12-crown-4 (B12C4), and the direct interaction of the corresponding pentafluorides, MF5 (M = Ta, Nb), in the presence of HF with the same crown ethers result in crystalline complexes of the same composition, [18C6 center dot H3O][NbF6] (1), [18C6 center dot H3O][TaF6] (2), [15C5 center dot H5O2][TaF6] (3), [(B15C5)(2)center dot H5O2][(B15C5)(2)center dot H3O][TaF6](2) (4) and [(B12C4)(2)center dot H3O][TaF6] (5). Complexes 1-5 were identified by elemental and X-ray structural analysis. Compounds 1 and 2 are isostructural, with the [H3O](+) oxonium ion embedded in one crown molecule via OH center dot center dot center dot O hydrogen bonds. Complexes 3-5 represent sandwich-like adducts with the [H3O](+) or [H5O2](+) cations encapsulated. A plethora of weak C-H center dot center dot center dot F interactions with NbF6- and TaF6- anions is responsible for the extended supramolecular architectures. (C) 2007 Elsevier Ltd. All rights reserved.
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