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

Eva Pump; Jasmine Viger-Gravel; Edy Abou-Hamad; Manoja K. Samantaray; Bilel Hamzaoui; Andrei Gurinov; Dalaver H. Anjum; David Gajan; Anne Lesage; Anissa Bendjeriou-Sedjerari; Lyndon Emsley; Jean Marie Basset

doi:10.1039/c6sc02379g

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

Eva Pump
, Jasmine Viger-Gravel
, Edy Abou-Hamad
, Manoja K. Samantaray
, Bilel Hamzaoui
, Andrei Gurinov
, Dalaver H. Anjum
, David Gajan
, Anne Lesage
, Anissa Bendjeriou-Sedjerari
, Lyndon Emsley
, Jean Marie Basset

Physics

Research output: Contribution to journal › Article › peer-review

59 Scopus citations

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 [(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.

Original language	British English
Pages (from-to)	284-290
Number of pages	7
Journal	Chemical Science
Volume	8
Issue number	1
DOIs	https://doi.org/10.1039/c6sc02379g
State	Published - 2016

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Pump, E., Viger-Gravel, J., Abou-Hamad, E., Samantaray, M. K., Hamzaoui, B., Gurinov, A., Anjum, D. H., Gajan, D., Lesage, A., Bendjeriou-Sedjerari, A., Emsley, L., & Basset, J. M. (2016). Reactive surface organometallic complexes observed using dynamic nuclear polarization surface enhanced NMR spectroscopy. Chemical Science, 8(1), 284-290. https://doi.org/10.1039/c6sc02379g

@article{662433807a3e4145a023588a3fdc6c0d,

title = "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 [(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.",

author = "Eva Pump and Jasmine Viger-Gravel and Edy Abou-Hamad and Samantaray, \{Manoja K.\} and Bilel Hamzaoui and Andrei Gurinov and Anjum, \{Dalaver H.\} and David Gajan and Anne Lesage and Anissa Bendjeriou-Sedjerari and Lyndon Emsley and Basset, \{Jean Marie\}",

note = "Funding Information: 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 Copyright: {\textcopyright} The Royal Society of Chemistry",

year = "2016",

doi = "10.1039/c6sc02379g",

language = "British English",

volume = "8",

pages = "284--290",

journal = "Chemical Science",

issn = "2041-6520",

publisher = "Royal Society of Chemistry",

number = "1",

}

Pump, E, Viger-Gravel, J, Abou-Hamad, E, Samantaray, MK, Hamzaoui, B, Gurinov, A, Anjum, DH, Gajan, D, Lesage, A, Bendjeriou-Sedjerari, A, Emsley, L & Basset, JM 2016, 'Reactive surface organometallic complexes observed using dynamic nuclear polarization surface enhanced NMR spectroscopy', Chemical Science, vol. 8, no. 1, pp. 284-290. https://doi.org/10.1039/c6sc02379g

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T1 - Reactive surface organometallic complexes observed using dynamic nuclear polarization surface enhanced NMR spectroscopy

AU - Pump, Eva

AU - Viger-Gravel, Jasmine

AU - Abou-Hamad, Edy

AU - Samantaray, Manoja K.

AU - Hamzaoui, Bilel

AU - Gurinov, Andrei

AU - Anjum, Dalaver H.

AU - Gajan, David

AU - Lesage, Anne

AU - Bendjeriou-Sedjerari, Anissa

AU - Emsley, Lyndon

AU - Basset, Jean Marie

N1 - Funding Information: 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 Copyright: © The Royal Society of Chemistry

PY - 2016

Y1 - 2016

N2 - 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 [(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.

AB - 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 [(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.

UR - https://www.scopus.com/pages/publications/85007193563

U2 - 10.1039/c6sc02379g

DO - 10.1039/c6sc02379g

M3 - Article

AN - SCOPUS:85007193563

SN - 2041-6520

VL - 8

SP - 284

EP - 290

JO - Chemical Science

JF - Chemical Science

IS - 1

ER -

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

Abstract

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