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Triborate and pentaborate salts of non-metal cations derived from N-substituted piperazines: synthesis, structural (XRD) and thermal properties

Beckett, M.A. and Horton, P.N. and Hursthouse, M.B. and Timmis, J.L. (2013) Triborate and pentaborate salts of non-metal cations derived from N-substituted piperazines: synthesis, structural (XRD) and thermal properties. RSC Advances, 3. pp. 15185-15191. DOI: 10.1039/C3RA42387E

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Abstract

The synthesis and characterization of a triborate salt, [H2N(CH2CH2)2NH2][B3O3(OH)4]2 (1), and four pentaborate salts, [H2N(CH2CH2)2NH][B5O6(OH)4] (2a), [MeHN(CH2CH2)2NH][B5O6(OH)4] (2b), [MeHN(CH2CH2)2NMe][B5O6(OH)4] (2c) and [Me2N(CH2CH2)2NMe2][B5O6(OH)4]2 (2d) are described. TGA and DSC analysis (in air, 25�1000 °C) indicate that triborate 1 decomposes to B2O3via a multistage process, with the first stage (<250 °C) being dehydration to condensed polymeric hexaborate of approximate composition: [H2N(CH2CH2)2NH2][B6O10]. The pentaborates (2a�2d) are thermally decomposed to B2O3via a 2 stage process involving polymeric [NMC][B5O8]. The anhydrous polyborates were amorphous. BET analysis of materials derived from the thermolysis of 1 at 250, 400, 600, and 1000 °C, were all non-porous (surface area <1.8 m2 g�1). A single-crystal X-ray diffraction study of 1 showed that it contains isolated triborate(1�) anions in a structure comprised of alternating cationic and anionic layers held together via extensive H-bonds. Single-crystal XRD structural studies on pentaborate salts 2c and 2d are also reported.

Item Type: Article
Subjects: Research Publications
Departments: College of Physical and Applied Sciences > School of Chemistry
Date Deposited: 09 Dec 2014 16:42
Last Modified: 23 Sep 2015 03:05
ISSN: 2046-2069
URI: http://e.bangor.ac.uk/id/eprint/809
Identification Number: DOI: 10.1039/C3RA42387E
Publisher: Royal Society of Chemistry
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