Skip to content

Research at St Andrews

Cost-effective 17O enrichment and NMR spectroscopy of mixed-metal terephthalate metal-organic frameworks

Research output: Contribution to journalArticle

DOI

Open Access permissions

Open

Author(s)

Giulia P. M. Bignami, Zachary H. Davis, Daniel M. Dawson, Samuel A. Morris, Samantha E. Russell, David McKay, Richard E. Parke, Dinu Iuga, Russell E. Morris, Sharon E. Ashbrook

School/Research organisations

Abstract

17O solid-state NMR spectroscopy is employed to investigate the cation disorder in metal–organic frameworks containing two different types of metal cations. Although NMR offers exquisite sensitivity to the local, atomic-scale structure, making it an ideal tool for the characterisation of disordered materials, the low natural abundance of 17O (0.037%) necessitates expensive isotopic enrichment to acquire spectra on a reasonable timescale. Using dry gel conversion and a novel steaming method we show that cost-effective and atom-efficient enrichment of MOFs is possible, and that high-resolution 17O NMR spectra are sensitive both to the structural forms of the MOF and the presence of guest molecules. For mixed-metal forms of MIL-53, NMR can also provide information on the final composition of the materials (notably different to that of the initial starting material) and the preference for cation clustering/ordering within the MOFs. For Al, Ga MIL-53, the distribution of cations results in a mixed-pore form upon exposure to water, unlike the different structures seen for the corresponding end members. This work shows that as good levels of enrichment can be achieved at reasonable cost, 17O NMR spectroscopy should be an invaluable tool for the study of these important functional materials.
Close

Details

Original languageEnglish
Pages (from-to)850-859
JournalChemical Science
Volume9
Issue number4
Early online date23 Nov 2017
DOIs
Publication statusPublished - 28 Jan 2018

Discover related content
Find related publications, people, projects and more using interactive charts.

View graph of relations

Related by author

  1. Hydrolytic stability in hemilabile metal–organic frameworks

    McHugh, L. N., McPherson, M. J., McCormick, L. J., Morris, S. A., Wheatley, P. S., Teat, S. J., McKay, D., Dawson, D. M., Sansome, C. E. F., Ashbrook, S. E., Stone, C. A., Smith, M. W. & Morris, R. E., 13 Aug 2018, In : Nature Chemistry. In press

    Research output: Contribution to journalArticle

  2. 13C pNMR of “crumple zone” Cu(II) isophthalate metal-organic frameworks

    Dawson, D. M., Sansome, C. E. F., McHugh, L. N., McPherson, M. J., McCormick McPherson, L. J., Morris, R. E. & Ashbrook, S. E., 14 May 2019, In : Solid State Nuclear Magnetic Resonance. In press

    Research output: Contribution to journalArticle

  3. A picture of disorder in hydrous wadsleyite – under the combined microscope of solid-state NMR spectroscopy and ab initio random structure searching

    McKay, D., Moran, R. F., Dawson, D. M., Griffin, J. M., Sturniolo, S., Pickard, C. J., Berry, A. J. & Ashbrook, S. E., 20 Feb 2019, In : Journal of the American Chemical Society. 141, 7, p. 3024–3036

    Research output: Contribution to journalArticle

  4. Polymorphism, weak interactions and phase transitions in chalcogen-phosphorus heterocycles

    Sanz Camacho, P., Stanford, M., McKay, D., Dawson, D. M., Athukorala Arachchige, K. S., Cordes, D. B., Slawin, A. M. Z., Woollins, J. D. & Ashbrook, S. E. M., 28 Jun 2018, In : Chemistry - A European Journal. Early View

    Research output: Contribution to journalArticle

  5. 17O solid-state NMR spectroscopy of A2B2O7 oxides: quantitative isotopic enrichment and spectral acquisition?

    Fernandes, A., Moran, R., Sneddon, S., Dawson, D. M., McKay, D., Bignami, G. P. M., Blanc, F., Whittle, K. & Ashbrook, S. E., 14 Feb 2018, In : RSC Advances. 8, 13, p. 7089-7101

    Research output: Contribution to journalArticle

Related by journal

  1. A natural solution to photoprotection and isolation of the potent polyene antibiotic, marinomycin A

    Bailey, C. S., Zarins-Tutt, J. S., Agbo, M., Gao, H., Diego-Taboada, A., Gan, M., Hamed Farghal, R. B., Abraham, E., Mackenzie, G., Evans, P. A. & Goss, R. J. M., 21 May 2019, In : Chemical Science. Advance Article, 5 p.

    Research output: Contribution to journalReview article

  2. Catalytic enantioselective synthesis of perfluoroalkyl-substituted β-lactones via a concerted asynchronous [2+2] cycloaddition: a synthetic and computational study

    Barrios Antunez, D-J., Greenhalgh, M. D., Brueckner, A. C., Walden, D. M., Elías-Rodríguez, P., Roberts, P., Young, B. G., West, T. H., Slawin, A. M. Z., Cheong, P. H-Y. & Smith, A. D., 28 Jun 2019, In : Chemical Science. 10, 24, p. 6162-6173 12 p.

    Research output: Contribution to journalArticle

  3. Turn on of sky-blue thermally activated delayed fluorescence and circularly polarized luminescence (CPL) via increased torsion by a bulky carbazolophane donor

    Sharma, N., Spuling, E., Mattern, C., Li, W., Fuhr, O., Tsuchiya, Y., Adachi, C., Bräse, S., Samuel, I. D. W. & Zysman-Colman, E., 29 May 2019, In : Chemical Science. Advance Article, 8 p.

    Research output: Contribution to journalReview article

  4. Visualization of the effect of additives on the nanostructures of individual bio-inspired calcite crystals

    Ihli, J., Clark, J. N., Kanwal, N., Kim, Y. Y., Holden, M. A., Harder, R. J., Tang, C. C., Ashbrook, S. E., Robinson, I. K. & Meldrum, F. C., 28 Jan 2019, In : Chemical Science. 10, 4, p. 1176-1185 10 p.

    Research output: Contribution to journalArticle

  5. Continuum tuning of nanoparticle interfacial properties by dynamic covalent exchange

    Edwards, W., Marro, N., Turner, G. & Kay, E. R., 7 Jan 2018, In : Chemical Science. 9, 1, p. 125-133

    Research output: Contribution to journalArticle

ID: 251607999