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Structural and thermal studies of non-metal cation pentaborate salts with cations derived from 1,5-diazobicyclo[4.3.0]non-5-ene, 1,8-diazobicyclo[5.4.0]undec-7-ene and 1,8-bis(dimethylamino)naphthalene

Structural and thermal studies of non-metal cation pentaborate salts with cations derived from 1,5-diazobicyclo[4.3.0]non-5-ene, 1,8-diazobicyclo[5.4.0]undec-7-ene and 1,8-bis(dimethylamino)naphthalene
Structural and thermal studies of non-metal cation pentaborate salts with cations derived from 1,5-diazobicyclo[4.3.0]non-5-ene, 1,8-diazobicyclo[5.4.0]undec-7-ene and 1,8-bis(dimethylamino)naphthalene
The reaction of the cyclic amines 1,5-diazobicyclo[4.3.0,non-5-ene (DBN), 1,8-diazobicyclo[5.4.0]undec7-ene (DBU) and 1,8-bis(dimethylamino)naphthalene (PS) with B(OH)(3) in a 1:5 ratio affords in high yields the non-metal cation pentaborate salts [HDBN][B5O6(OH)(4)] (1), [HDBU][B5O6(OH)(4)] (2) and [HPS][B5O6(OH)(4)].B(OH)(3) (3). Compounds 1-3 were characterized by spectroscopic studies (NMR, IR) and compounds 1 and 3 were further characterized by single-crystal XRD studies. The pentaborate salts compounds show extensively H-bonded supramolecular anionic lattices which are templated by the cations. Thermal analysis (TGA) of 1-3 showed that thermally decomposed in air at 10000 degrees to B2O3 in a two step process involving dehydration (<250 degrees C) and oxidation (250-600 degrees C). BET analysis of materials derived from thermolysis of 1-3 had internal porosities of <1 m(2)/g. (C) 2012 Elsevier Ltd. All rights reserved.
0277-5387
157-161
Beckett, Michael A.
5b021ef6-fa5c-4f6d-9998-3313558f0dc1
Horton, Peter N.
48f162d1-d6ce-43c1-aeef-d58b3ec702b8
Coles, Simon J.
3116f58b-c30c-48cf-bdd5-397d1c1fecf8
Kose, Dursun A.
237fb201-6633-4505-9e2f-0f63411f359c
Kreuziger, Anna-Marlena
8157a7a3-48e1-4cc1-88cb-6fb81d456dad
Beckett, Michael A.
5b021ef6-fa5c-4f6d-9998-3313558f0dc1
Horton, Peter N.
48f162d1-d6ce-43c1-aeef-d58b3ec702b8
Coles, Simon J.
3116f58b-c30c-48cf-bdd5-397d1c1fecf8
Kose, Dursun A.
237fb201-6633-4505-9e2f-0f63411f359c
Kreuziger, Anna-Marlena
8157a7a3-48e1-4cc1-88cb-6fb81d456dad

Beckett, Michael A., Horton, Peter N., Coles, Simon J., Kose, Dursun A. and Kreuziger, Anna-Marlena (2012) Structural and thermal studies of non-metal cation pentaborate salts with cations derived from 1,5-diazobicyclo[4.3.0]non-5-ene, 1,8-diazobicyclo[5.4.0]undec-7-ene and 1,8-bis(dimethylamino)naphthalene. Polyhedron, 38 (1), 157-161. (doi:10.1016/j.poly.2012.02.031).

Record type: Article

Abstract

The reaction of the cyclic amines 1,5-diazobicyclo[4.3.0,non-5-ene (DBN), 1,8-diazobicyclo[5.4.0]undec7-ene (DBU) and 1,8-bis(dimethylamino)naphthalene (PS) with B(OH)(3) in a 1:5 ratio affords in high yields the non-metal cation pentaborate salts [HDBN][B5O6(OH)(4)] (1), [HDBU][B5O6(OH)(4)] (2) and [HPS][B5O6(OH)(4)].B(OH)(3) (3). Compounds 1-3 were characterized by spectroscopic studies (NMR, IR) and compounds 1 and 3 were further characterized by single-crystal XRD studies. The pentaborate salts compounds show extensively H-bonded supramolecular anionic lattices which are templated by the cations. Thermal analysis (TGA) of 1-3 showed that thermally decomposed in air at 10000 degrees to B2O3 in a two step process involving dehydration (<250 degrees C) and oxidation (250-600 degrees C). BET analysis of materials derived from thermolysis of 1-3 had internal porosities of <1 m(2)/g. (C) 2012 Elsevier Ltd. All rights reserved.

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Published date: 11 May 2012
Organisations: Organic Chemistry: Synthesis, Catalysis and Flow

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Local EPrints ID: 346089
URI: https://eprints.soton.ac.uk/id/eprint/346089
ISSN: 0277-5387
PURE UUID: d2b7babc-44f2-4a39-8003-49b87e620770
ORCID for Simon J. Coles: ORCID iD orcid.org/0000-0001-8414-9272

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Date deposited: 14 Dec 2012 15:12
Last modified: 31 Jul 2019 00:47

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