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 journalArticlepeer-review

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. Following the unusual breathing behaviour of 17O-enriched mixed-metal (Al,Ga)-MIL-53 using NMR crystallography

    Rice, C. M., Davis, Z. H., McKay, D., Bignami, G. P. M., Chitac, R. G., Dawson, D. M., Morris, R. E. & Ashbrook, S. E., 14 Jul 2020, In: Physical Chemistry Chemical Physics. 22, 26, p. 14514-14526 13 p.

    Research output: Contribution to journalArticlepeer-review

  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 journalArticlepeer-review

  3. 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., Nov 2018, In: Nature Chemistry. 10, 11, p. 1096–1102 7 p.

    Research output: Contribution to journalArticlepeer-review

  4. In situ solid-state NMR and XRD studies of the ADOR process and the unusual structure of zeolite IPC-6

    Morris, S. A., Bignami, G. P. M., Tian, Y., Navarro-Rojas, M., Firth, D. S., Cejka, J., Wheatley, P. S., Dawson, D. M., Slawinski, W. A., Wragg, D. S., Morris, R. E. & Ashbrook, S. E., Oct 2017, In: Nature Chemistry. 9, 10, p. 1012-1018 7 p.

    Research output: Contribution to journalArticlepeer-review

  5. Synthesis, isotopic enrichment and solid-state NMR characterization of zeolites derived from the assembly, disassembly, organisation, reassembly process

    Bignami, G. P. M., Dawson, D. M., Seymour, V. R., Wheatley, P. S., Morris, R. E. & Ashbrook, S. E., 12 Apr 2017, In: Journal of the American Chemical Society. 139, 14, p. 5140-5148 9 p.

    Research output: Contribution to journalArticlepeer-review

Related by journal

  1. 17O NMR spectroscopy of crystalline microporous materials

    Ashbrook, S. E., Davis, Z., Morris, R. & Rice, C. M., 25 Feb 2021, In: Chemical Science. Advance Article, 21 p.

    Research output: Contribution to journalReview articlepeer-review

  2. Albumin-mediated alteration of plasma zinc speciation by fatty acids modulates blood clotting in type-2 diabetes

    Sobczak, A. I. S., Katundu, K. G. H., Phoenix, F. A., Khazaipoul, S., Yu, R., Lampiao, F., Stefanowicz, F., Blindauer, C. A., Pitt, S. J., Smith, T. K., Ajjan, R. A. & Stewart, A. J., 21 Mar 2021, In: Chemical Science. 12, 11, p. 4079-4093 15 p.

    Research output: Contribution to journalArticlepeer-review

  3. Single-step synthesis and interface tuning of core–shell metal–organic framework nanoparticles

    Orr, K. W. P., Collins, S. M., Reynolds, E. M., Nightingale, F., Boström, H. L. B., Cassidy, S. J., Dawson, D. M., Ashbrook, S. E., Magdysyuk, O. V., Midgley, P., Goodwin, A. L. & Yeung, H. H-M., 9 Feb 2021, In: Chemical Science. Advance Article, 9 p.

    Research output: Contribution to journalArticlepeer-review

  4. Mechanomechanically assisted hydrolysis in the ADOR process

    Rainer, D. N., Rice, C. M., Warrender, S. J., Ashbrook, S. E. & Morris, R. E., 15 Jun 2020, In: Chemical Science. Advance Article, 10 p.

    Research output: Contribution to journalArticlepeer-review

  5. Method for accurate experimental determination of singlet and triplet exciton diffusion between thermally activated delayed fluorescence molecules

    Jakoby, M., Heidrich, S., Graf von Reventlow, L., Degitz, C., Madayanad Suresh, S., Zysman-Colman, E., Wenzel, W., Richards, B. & Howard, I., 16 Nov 2020, In: Chemical Science. Advance article

    Research output: Contribution to journalArticlepeer-review

ID: 251607999

Top