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Issue 1, 2017

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

Author affiliations

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

Supplementary files

Article information


Submitted
30 May 2016
Accepted
12 Aug 2016
First published
15 Aug 2016

This article is Open Access
All publication charges for this article have been paid for by the Royal Society of Chemistry

Chem. Sci., 2017,8, 284-290
Article type
Edge Article

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

This article is licensed under a Creative Commons Attribution 3.0 Unported Licence. You can use material from this article in other publications without requesting further permissions from the RSC, provided that the correct acknowledgement is given.

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