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Issue 1, 2017
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Reactive surface organometallic complexes observed using dynamic nuclear polarization surface enhanced NMR spectroscopy

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Abstract

Dynamic Nuclear Polarization Surface Enhanced NMR Spectroscopy (DNP SENS) is an emerging technique that allows access to high-sensitivity NMR spectra from surfaces. However, DNP SENS usually requires the use of radicals as an exogenous source of polarization, which has so far limited applications for organometallic surface species to those that do not react with the radicals. Here we show that reactive surface species can be studied if they are immobilized inside porous materials with suitably small windows, and if bulky nitroxide bi-radicals (here TEKPol) are used as the polarization source and which cannot enter the pores. The method is demonstrated by obtaining significant DNP enhancements from highly reactive complelxes [([triple bond, length as m-dash]Si–O–)W(Me)5] supported on MCM-41, and effects of pore size (6.0, 3.0 and 2.5 nm) on the performance are discussed.

Graphical abstract: Reactive surface organometallic complexes observed using dynamic nuclear polarization surface enhanced NMR spectroscopy

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Publication details

The article was received on 30 May 2016, accepted on 12 Aug 2016 and first published on 15 Aug 2016


Article type: Edge Article
DOI: 10.1039/C6SC02379G
Citation: Chem. Sci., 2017,8, 284-290
  • Open access: Creative Commons BY license
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    Reactive surface organometallic complexes observed using dynamic nuclear polarization surface enhanced NMR spectroscopy

    E. Pump, J. Viger-Gravel, E. Abou-Hamad, M. K. Samantaray, B. Hamzaoui, A. Gurinov, D. H. Anjum, D. Gajan, A. Lesage, A. Bendjeriou-Sedjerari, L. Emsley and J. Basset, Chem. Sci., 2017, 8, 284
    DOI: 10.1039/C6SC02379G

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