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

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 [(equivalent to 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.

Citation
Pump E, Viger-Gravel J, Abou-Hamad E, Samantaray MK, Hamzaoui B, et al. (2017) Reactive surface organometallic complexes observed using dynamic nuclear polarization surface enhanced NMR spectroscopy. Chem Sci 8: 284–290. Available: http://dx.doi.org/10.1039/c6sc02379g.

Acknowledgements
This work received support from the King Abdullah University of Science and Technology (KAUST) and ERC Advanced Grant No. 320860. We thank Dr Olivier Ouari and Paul Tordo from the University of Aix-Marseille, for providing the TEKPol radical.

Publisher
Royal Society of Chemistry (RSC)

Journal
Chemical Science

DOI
10.1039/c6sc02379g

Additional Links
http://pubs.rsc.org/en/Content/ArticleLanding/2017/SC/C6SC02379G#!divAbstract

Permanent link to this record