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Pentaborate(1-) salts and a tetraborate(2-) salt derived from C2- or C3-linked bis(alkylammonium) dications: Synthesis, characterization, and structural (XRD) Studies

Pentaborate(1-) salts and a tetraborate(2-) salt derived from C2- or C3-linked bis(alkylammonium) dications: Synthesis, characterization, and structural (XRD) Studies
Pentaborate(1-) salts and a tetraborate(2-) salt derived from C2- or C3-linked bis(alkylammonium) dications: Synthesis, characterization, and structural (XRD) Studies

The synthesis of a number of pentaborate(1-) salts from cations arising from N-substituted α,α-, α,β-, and α,-diaminoalkanes has been attempted in aqueous solution from B(OH)3 and the appropriate diammine in a 10:1 ratio. Despite relatively mild work-up conditions the pentaborate(1-) salts prepared were not always as anticipated and the following compounds were isolated in good yield: [Me2NH(CH2)2NHMe2][B5O6(OH)4]2 (1), [Et2NH(CH2)2NHEt2][B5O6(OH)4]2 (2), [Et2NH2][B5O6(OH)4] (3), [Me2NH2][B5O6(OH)4] (4), [Me2NH(CH2)3NHMe2][B5O6(OH)4]2 (5), [Et2NH(CH2)3NHEt2][B5O6(OH)4]2 (6), [Me3NCH2CH=CH2][B5O6(OH)4] (7), and [Me3N(CH2)3NMe3] [B5O6(OH)4]2.0.5H2O (8). The tetraborate(2-) salt, [Me3N(CH2)2NMe3][B4O5(OH)4].2B(OH)3 .2H2O (9) was obtained in moderate yield (41%) from a 3:1 reaction of B(OH)3 with [Me3N(CH2)2NMe3](OH)2. All compounds were characterized by spectroscopy (1H, 11B, 13C NMR and IR) and thermal gravimetric analysis (TGA). BET analysis on materials derived thermally from selected samples (1, 2, 6, 7) all had porosities of < 1 m2/g, demonstrating that they were non-porous. Single-crystal XRD structures were obtained for 2, 3, 7, 8 and 9 and all contain extensive H-bonded polyborate lattices.

BET analysis, Borate, Diaminoalkane salts, Oxidipolyborate, Pentaborate(1-), Tetraborate(2-), TGA, XRD
1420-3049
Beckett, Michael A.
5b021ef6-fa5c-4f6d-9998-3313558f0dc1
Meena, Bashdar I.
03a7b5a1-7676-4e45-a607-5037747471f6
Rixon, Thomas A.
f5d9498d-b8cc-43b4-9b32-99253e1263db
Coles, Simon J.
3116f58b-c30c-48cf-bdd5-397d1c1fecf8
Horton, Peter N.
154c8930-bfc3-495b-ad4a-8a278d5da3a5
Beckett, Michael A.
5b021ef6-fa5c-4f6d-9998-3313558f0dc1
Meena, Bashdar I.
03a7b5a1-7676-4e45-a607-5037747471f6
Rixon, Thomas A.
f5d9498d-b8cc-43b4-9b32-99253e1263db
Coles, Simon J.
3116f58b-c30c-48cf-bdd5-397d1c1fecf8
Horton, Peter N.
154c8930-bfc3-495b-ad4a-8a278d5da3a5

Beckett, Michael A., Meena, Bashdar I., Rixon, Thomas A., Coles, Simon J. and Horton, Peter N. (2020) Pentaborate(1-) salts and a tetraborate(2-) salt derived from C2- or C3-linked bis(alkylammonium) dications: Synthesis, characterization, and structural (XRD) Studies. Molecules, 25 (1), [53]. (doi:10.3390/molecules25010053).

Record type: Article

Abstract

The synthesis of a number of pentaborate(1-) salts from cations arising from N-substituted α,α-, α,β-, and α,-diaminoalkanes has been attempted in aqueous solution from B(OH)3 and the appropriate diammine in a 10:1 ratio. Despite relatively mild work-up conditions the pentaborate(1-) salts prepared were not always as anticipated and the following compounds were isolated in good yield: [Me2NH(CH2)2NHMe2][B5O6(OH)4]2 (1), [Et2NH(CH2)2NHEt2][B5O6(OH)4]2 (2), [Et2NH2][B5O6(OH)4] (3), [Me2NH2][B5O6(OH)4] (4), [Me2NH(CH2)3NHMe2][B5O6(OH)4]2 (5), [Et2NH(CH2)3NHEt2][B5O6(OH)4]2 (6), [Me3NCH2CH=CH2][B5O6(OH)4] (7), and [Me3N(CH2)3NMe3] [B5O6(OH)4]2.0.5H2O (8). The tetraborate(2-) salt, [Me3N(CH2)2NMe3][B4O5(OH)4].2B(OH)3 .2H2O (9) was obtained in moderate yield (41%) from a 3:1 reaction of B(OH)3 with [Me3N(CH2)2NMe3](OH)2. All compounds were characterized by spectroscopy (1H, 11B, 13C NMR and IR) and thermal gravimetric analysis (TGA). BET analysis on materials derived thermally from selected samples (1, 2, 6, 7) all had porosities of < 1 m2/g, demonstrating that they were non-porous. Single-crystal XRD structures were obtained for 2, 3, 7, 8 and 9 and all contain extensive H-bonded polyborate lattices.

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Accepted/In Press date: 21 December 2019
e-pub ahead of print date: 23 December 2019
Published date: 1 January 2020
Keywords: BET analysis, Borate, Diaminoalkane salts, Oxidipolyborate, Pentaborate(1-), Tetraborate(2-), TGA, XRD

Identifiers

Local EPrints ID: 437320
URI: http://eprints.soton.ac.uk/id/eprint/437320
ISSN: 1420-3049
PURE UUID: 1db87fe8-4913-4436-8284-a187d9024824
ORCID for Simon J. Coles: ORCID iD orcid.org/0000-0001-8414-9272
ORCID for Peter N. Horton: ORCID iD orcid.org/0000-0001-8886-2016

Catalogue record

Date deposited: 24 Jan 2020 17:31
Last modified: 27 Jan 2020 13:38

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