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,γ-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: [Me
2NH(CH
2)
2NHMe
2][B
5O
6(OH)
4]
2 (
1), [Et
2NH(CH
2)
2NHEt
2][B
5O
6(OH)
4]
2 (
2), [Et
2NH
2][B
5O
6(OH)
4] (
3), [Me
2NH
2][B
5O
6(OH)
4] (
4), [Me
2NH(CH
2)
3NHMe
2][B
5O
6(OH)
4]
2 (
5), [Et
2NH(CH
2)
3NHEt
2][B
5O
6(OH)
4]
2 (
6), [Me
3NCH
2CH=CH
2][B
5O
6(OH)
4] (
7), and [Me
3N(CH
2)
3NMe
3] [B
5O
6(OH)
4]
2
.0.5H
2O (
8). The tetraborate(2-) salt, [Me
3N(CH
2)
2NMe
3][B
4O
5(OH)
4]
.2B(OH)
3
.2H
2O (
9) was obtained in moderate yield (41%) from a 3:1 reaction of B(OH)
3 with [Me
3N(CH
2)
2NMe
3](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 m
2/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
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
23 December 2019
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.
(2019)
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).
Abstract
The synthesis of a number of pentaborate(1-) salts from cations arising from
N-substituted α,α-, α,β-, and α,γ-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: [Me
2NH(CH
2)
2NHMe
2][B
5O
6(OH)
4]
2 (
1), [Et
2NH(CH
2)
2NHEt
2][B
5O
6(OH)
4]
2 (
2), [Et
2NH
2][B
5O
6(OH)
4] (
3), [Me
2NH
2][B
5O
6(OH)
4] (
4), [Me
2NH(CH
2)
3NHMe
2][B
5O
6(OH)
4]
2 (
5), [Et
2NH(CH
2)
3NHEt
2][B
5O
6(OH)
4]
2 (
6), [Me
3NCH
2CH=CH
2][B
5O
6(OH)
4] (
7), and [Me
3N(CH
2)
3NMe
3] [B
5O
6(OH)
4]
2
.0.5H
2O (
8). The tetraborate(2-) salt, [Me
3N(CH
2)
2NMe
3][B
4O
5(OH)
4]
.2B(OH)
3
.2H
2O (
9) was obtained in moderate yield (41%) from a 3:1 reaction of B(OH)
3 with [Me
3N(CH
2)
2NMe
3](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 m
2/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.
Text
molecules-25-00053
- Version of Record
More information
Accepted/In Press date: 21 December 2019
e-pub ahead of print date: 23 December 2019
Published date: 23 December 2019
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
Catalogue record
Date deposited: 24 Jan 2020 17:31
Last modified: 17 Mar 2024 02:50
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Contributors
Author:
Michael A. Beckett
Author:
Bashdar I. Meena
Author:
Thomas A. Rixon
Author:
Peter N. Horton
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