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Issue 44, 2018
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Vanadyl sulfates: molecular structure, magnetism and electrochemical activity

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Reaction of differing amounts of vanadyl sulfate with p-tert-butylthiacalix[4]areneH4 and base allows access to the vanadyl-sulfate species [NEt4]4[(VO)43-OH)4(SO4)4]·½H2O (1), [HNEt3]5[(VO)53-O)4(SO4)4]·4MeCN (2·4MeCN) and [NEt4]2[(VO)6(O)2(SO4)4(OMe)(OH2)]·MeCN (3·MeCN). Similar use of p-tert-butylsulfonylcalix[4]areneH4, p-tert-butylcalix[8]areneH8 or p-tert-butylhexahomotrioxacalix[3]areneH3 led to the isolation of [HNEt3]2[H2NEt2]2{[VO(OMe)]2p-tert-butylcalix[8-SO2]areneH2} (4), [HNEt3]2[V(O)2p-tert-butylcalix[8]areneH5] (5) and [HNEt3]2[VIV2VV4O11(OMe)8] (6), respectively. Dc magnetic susceptibility measurements were performed on powdered microcrystalline samples of 1–3 in the T = 300–2 K temperature range. Preliminary screening for electrochemical water oxidation revealed some activity for 2 with turnover frequency (TOF) and number (TON) of 2.2 × 10−4 s−1 and 6.44 × 10−6 (mmol O2/mmol cat.), respectively. The compound 3 showed an improved electrochemical activity in the presence of water. This is related to the increased number and the rate of electrons exchanged during oxidation of V4+ species, facilitated by protons generated in the water discharge process.

Graphical abstract: Vanadyl sulfates: molecular structure, magnetism and electrochemical activity

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Publication details

The article was received on 07 Sep 2018, accepted on 21 Oct 2018 and first published on 22 Oct 2018

Article type: Paper
DOI: 10.1039/C8DT03626H
Citation: Dalton Trans., 2018,47, 15983-15993

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    Vanadyl sulfates: molecular structure, magnetism and electrochemical activity

    A. Ignaszak, N. Patterson, M. Radtke, M. R. J. Elsegood, J. W. A. Frese, J. L. Z. F. Lipman, T. Yamato, S. Sanz, E. K. Brechin, T. J. Prior and C. Redshaw, Dalton Trans., 2018, 47, 15983
    DOI: 10.1039/C8DT03626H

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