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Synthesis, thermal properties and structural characterisation, of the tetraphenylphosphonium pentaborate salt, [PPh4][B5O6(OH)4]·1.5H2O

Synthesis, thermal properties and structural characterisation, of the tetraphenylphosphonium pentaborate salt, [PPh4][B5O6(OH)4]·1.5H2O
Synthesis, thermal properties and structural characterisation, of the tetraphenylphosphonium pentaborate salt, [PPh4][B5O6(OH)4]·1.5H2O
[Ph4P][B5O6(OH)4] · 1.5H2O (1) was obtained as colourless crystals in high yield from a MeOH/H2O solution of B(OH)3 and [PPh4][OH] (5:1). A single-crystal X-ray study confirmed that the solid-state structure was comprised of supramolecular networks of interconnected anions (H-bonds) and cations (phenyl embraces). Crystals are triclinic, P (1) over bar with a = 13.3174(3) angstrom, b = 13.3180(3) angstrom, c = 16.2055(4) angstrom, alpha = 91.1950(10)degrees, beta = 91.180(2)degrees, gamma = 105.456(2)degrees, T = 120(2) K, V = 2768.66(11) angstrom(3) and Z = 4. TGA/DSC analysis showed that 1 thermally decomposed in air at 800 degrees C to 2.5B2O3, via a low temperature dehydration step to a condensed pentaborate, [PPh4][B5O8].
0020-1693
199-203
Beckett, Michael A.
5b021ef6-fa5c-4f6d-9998-3313558f0dc1
Horton, Peter N.
154c8930-bfc3-495b-ad4a-8a278d5da3a5
Hursthouse, Michael B.
57a2ddf9-b1b3-4f38-bfe9-ef2f526388da
Timmis, James L.
3bc450de-1482-49d1-8e75-3d957a989300
Sukumar Varma, K.
ee829f4b-6265-4a2b-9413-dac4bbbe84a3
Beckett, Michael A.
5b021ef6-fa5c-4f6d-9998-3313558f0dc1
Horton, Peter N.
154c8930-bfc3-495b-ad4a-8a278d5da3a5
Hursthouse, Michael B.
57a2ddf9-b1b3-4f38-bfe9-ef2f526388da
Timmis, James L.
3bc450de-1482-49d1-8e75-3d957a989300
Sukumar Varma, K.
ee829f4b-6265-4a2b-9413-dac4bbbe84a3

Beckett, Michael A., Horton, Peter N., Hursthouse, Michael B., Timmis, James L. and Sukumar Varma, K. (2012) Synthesis, thermal properties and structural characterisation, of the tetraphenylphosphonium pentaborate salt, [PPh4][B5O6(OH)4]·1.5H2O. Inorganica Chimica Acta, 383, 199-203. (doi:10.1016/j.ica.2011.11.001).

Record type: Article

Abstract

[Ph4P][B5O6(OH)4] · 1.5H2O (1) was obtained as colourless crystals in high yield from a MeOH/H2O solution of B(OH)3 and [PPh4][OH] (5:1). A single-crystal X-ray study confirmed that the solid-state structure was comprised of supramolecular networks of interconnected anions (H-bonds) and cations (phenyl embraces). Crystals are triclinic, P (1) over bar with a = 13.3174(3) angstrom, b = 13.3180(3) angstrom, c = 16.2055(4) angstrom, alpha = 91.1950(10)degrees, beta = 91.180(2)degrees, gamma = 105.456(2)degrees, T = 120(2) K, V = 2768.66(11) angstrom(3) and Z = 4. TGA/DSC analysis showed that 1 thermally decomposed in air at 800 degrees C to 2.5B2O3, via a low temperature dehydration step to a condensed pentaborate, [PPh4][B5O8].

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Published date: 30 March 2012
Related URLs:
Organisations: Organic Chemistry: Synthesis, Catalysis and Flow, Chemistry, Faculty of Natural and Environmental Sciences
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Identifiers

Local EPrints ID: 347409
URI: http://eprints.soton.ac.uk/id/eprint/347409
DOI: doi:10.1016/j.ica.2011.11.001
ISSN: 0020-1693
PURE UUID: a7512256-e6dd-4a70-b5cb-85ced8c64919
ORCID for Peter N. Horton: ORCID iD orcid.org/0000-0001-8886-2016

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Date deposited: 23 Jan 2013 10:08
Last modified: 15 Mar 2024 03:04

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Contributors

Author: Michael A. Beckett
Author: Peter N. Horton ORCID iD
Author: Michael B. Hursthouse
Author: James L. Timmis
Author: K. Sukumar Varma

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