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Tetrahydroxidohexaoxidopentaborate(1-) Salts of C6-linked substituted diimidazolium and dipyrrolidinium cations: synthesis, characterization and XRD studies

Tetrahydroxidohexaoxidopentaborate(1-) Salts of C6-linked substituted diimidazolium and dipyrrolidinium cations: synthesis, characterization and XRD studies
Tetrahydroxidohexaoxidopentaborate(1-) Salts of C6-linked substituted diimidazolium and dipyrrolidinium cations: synthesis, characterization and XRD studies

Several tetrahydroxidohexaoxidopentaborate(1-) salts of N-substituted diimidazolium cations or N-substituted dipyrrolidinium cations linked through N-C6-N chains have been synthesized and characterized spectroscopically (NMR, IR) and by single-crystal XRD studies: [R(NC3H3N)(CH2)6(NC3H3N)R][B5O6(OH)4]2·xH2O (R = Me, x = 0 (1); R = Et, x = 3 (2); [Me(NC3H3N)(CH2(C6H4)CH2)(NC3H3N)Me][B5O6(OH)4]2 (3), [(C4H8N)(R)(CH2)6(R)(NC4H8)][B5O6(OH)4]2·xB(OH)3 (R = Me, x = 0 (4, two polymorphs); R = Et, x = 0 (5); R = Bu, x = 4 (6); R = allyl, x = 0 (7)). Representative samples (1 and 7) were also characterized by thermal (TGA/DSC) studies; compounds are thermally decomposed to B2O3 in air. Numerous anion-anion H-bonding interactions are present in the solid-state structures of 1–5 and 7 as giant anionic networks. Unusually, in 6 there are no R22(8) anion-anion interactions as the co-crystallized B(OH)3 bridges between all pentaborate anions. H-bonding interactions in 1–7 have been examined using Etter graph set analysis; C(8), C33(18), R22(8), R22(12) and R44(12) motifs have been identified.

H-bonding, imidazolium, pentaborate, pyrrolidium, tetrahydroxidohexaoxidopeentaborate(1-), XRD
2304-6740
Al-Dulayymi, Ahmad R.
413e92b4-dc52-4747-b06e-58e71d3ddfca
Beckett, Michael A.
5b021ef6-fa5c-4f6d-9998-3313558f0dc1
Braganca, Radek
f1d38acc-ea4f-46f3-9e7a-21ceb55fcb44
Coles, Simon J.
3116f58b-c30c-48cf-bdd5-397d1c1fecf8
Horton, Peter N.
154c8930-bfc3-495b-ad4a-8a278d5da3a5
Rixon, Thomas A.
f5d9498d-b8cc-43b4-9b32-99253e1263db
Al-Dulayymi, Ahmad R.
413e92b4-dc52-4747-b06e-58e71d3ddfca
Beckett, Michael A.
5b021ef6-fa5c-4f6d-9998-3313558f0dc1
Braganca, Radek
f1d38acc-ea4f-46f3-9e7a-21ceb55fcb44
Coles, Simon J.
3116f58b-c30c-48cf-bdd5-397d1c1fecf8
Horton, Peter N.
154c8930-bfc3-495b-ad4a-8a278d5da3a5
Rixon, Thomas A.
f5d9498d-b8cc-43b4-9b32-99253e1263db

Al-Dulayymi, Ahmad R., Beckett, Michael A., Braganca, Radek, Coles, Simon J., Horton, Peter N. and Rixon, Thomas A. (2024) Tetrahydroxidohexaoxidopentaborate(1-) Salts of C6-linked substituted diimidazolium and dipyrrolidinium cations: synthesis, characterization and XRD studies. Inorganics, 12 (8), [220]. (doi:10.3390/inorganics12080220).

Record type: Article

Abstract

Several tetrahydroxidohexaoxidopentaborate(1-) salts of N-substituted diimidazolium cations or N-substituted dipyrrolidinium cations linked through N-C6-N chains have been synthesized and characterized spectroscopically (NMR, IR) and by single-crystal XRD studies: [R(NC3H3N)(CH2)6(NC3H3N)R][B5O6(OH)4]2·xH2O (R = Me, x = 0 (1); R = Et, x = 3 (2); [Me(NC3H3N)(CH2(C6H4)CH2)(NC3H3N)Me][B5O6(OH)4]2 (3), [(C4H8N)(R)(CH2)6(R)(NC4H8)][B5O6(OH)4]2·xB(OH)3 (R = Me, x = 0 (4, two polymorphs); R = Et, x = 0 (5); R = Bu, x = 4 (6); R = allyl, x = 0 (7)). Representative samples (1 and 7) were also characterized by thermal (TGA/DSC) studies; compounds are thermally decomposed to B2O3 in air. Numerous anion-anion H-bonding interactions are present in the solid-state structures of 1–5 and 7 as giant anionic networks. Unusually, in 6 there are no R22(8) anion-anion interactions as the co-crystallized B(OH)3 bridges between all pentaborate anions. H-bonding interactions in 1–7 have been examined using Etter graph set analysis; C(8), C33(18), R22(8), R22(12) and R44(12) motifs have been identified.

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Accepted/In Press date: 13 August 2024
Published date: 15 August 2024
Keywords: H-bonding, imidazolium, pentaborate, pyrrolidium, tetrahydroxidohexaoxidopeentaborate(1-), XRD

Identifiers

Local EPrints ID: 494408
URI: http://eprints.soton.ac.uk/id/eprint/494408
ISSN: 2304-6740
PURE UUID: 3aa4048c-a88b-4b52-9a09-6418cf557732
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

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Date deposited: 07 Oct 2024 17:17
Last modified: 08 Oct 2024 01:36

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Contributors

Author: Ahmad R. Al-Dulayymi
Author: Michael A. Beckett
Author: Radek Braganca
Author: Simon J. Coles ORCID iD
Author: Peter N. Horton ORCID iD
Author: Thomas A. Rixon

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