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

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).

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.

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Contributors

Author: Simon J. Coles

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