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Issue 15, 2012
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Templated heptaborate and pentaborate salts of cyclo-alkylammonium cations: structural and thermal properties

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Abstract

The synthesis and characterization of a series of cyclo-alkylammonium pentaborate salts {[cyclo-CnH2n−1NR3][B5O6(OH)4] (R = H, n = 3, 5–7 (1–4); R = Me, n = 6 (5))} are reported. Compounds 1, 2 and 5 have been further characterized by single-crystal XRD studies. Attempted recrystallization of 3 and 4 yielded small crops of the unexpected heptaborate salts, [cyclo-C6H11NH3]2[B7O9(OH)5]·3H2O·B(OH)3 (6) and [cyclo-C7H13NH3]2[B7O9(OH)5]·2H2O·2B(OH)3 (7) which were also characterized crystallographically. All compounds show extensive supramolecular H-bonded anionic lattices templated by the cations. H-bond interactions are described in detail. TGA–DSC analysis of the pentaborates 1–5 showed that they thermally decomposed in air at 800 °C to 2.5B2O3, in a 2 step process involving dehydration (<250 °C) and oxidative decomposition (250–600 °C). BET analysis of materials derived from the pentaborates had internal porosities of <1 m2 g−1.

Graphical abstract: Templated heptaborate and pentaborate salts of cyclo-alkylammonium cations: structural and thermal properties

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Publication details

The article was received on 01 Dec 2011, accepted on 16 Jan 2012 and first published on 17 Feb 2012


Article type: Paper
DOI: 10.1039/C2DT12310J
Citation: Dalton Trans., 2012,41, 4396-4403
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    Templated heptaborate and pentaborate salts of cyclo-alkylammonium cations: structural and thermal properties

    M. A. Beckett, P. N. Horton, M. B. Hursthouse, J. L. Timmis and K. S. Varma, Dalton Trans., 2012, 41, 4396
    DOI: 10.1039/C2DT12310J

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