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Reactive surface organometallic complexes observed using dynamic nuclear polarization surface enhanced NMR spectroscopy
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 fo...
Autores principales: | , , , , , , , , , , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
Royal Society of Chemistry
2017
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5365068/ https://www.ncbi.nlm.nih.gov/pubmed/28451174 http://dx.doi.org/10.1039/c6sc02379g |
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author | Pump, Eva Viger-Gravel, Jasmine Abou-Hamad, Edy Samantaray, Manoja K. Hamzaoui, Bilel Gurinov, Andrei Anjum, Dalaver H. Gajan, David Lesage, Anne Bendjeriou-Sedjerari, Anissa Emsley, Lyndon Basset, Jean-Marie |
author_facet | Pump, Eva Viger-Gravel, Jasmine Abou-Hamad, Edy Samantaray, Manoja K. Hamzaoui, Bilel Gurinov, Andrei Anjum, Dalaver H. Gajan, David Lesage, Anne Bendjeriou-Sedjerari, Anissa Emsley, Lyndon Basset, Jean-Marie |
author_sort | Pump, Eva |
collection | PubMed |
description | 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. |
format | Online Article Text |
id | pubmed-5365068 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2017 |
publisher | Royal Society of Chemistry |
record_format | MEDLINE/PubMed |
spelling | pubmed-53650682017-04-27 Reactive surface organometallic complexes observed using dynamic nuclear polarization surface enhanced NMR spectroscopy Pump, Eva Viger-Gravel, Jasmine Abou-Hamad, Edy Samantaray, Manoja K. Hamzaoui, Bilel Gurinov, Andrei Anjum, Dalaver H. Gajan, David Lesage, Anne Bendjeriou-Sedjerari, Anissa Emsley, Lyndon Basset, Jean-Marie Chem Sci Chemistry 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. Royal Society of Chemistry 2017-01-01 2016-08-15 /pmc/articles/PMC5365068/ /pubmed/28451174 http://dx.doi.org/10.1039/c6sc02379g Text en This journal is © The Royal Society of Chemistry 2016 https://creativecommons.org/licenses/by/3.0/This is an Open Access article distributed under the terms of the Creative Commons Attribution 3.0 Unported License (http://creativecommons.org/licenses/by/3.0/ (https://creativecommons.org/licenses/by/3.0/) ) which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. |
spellingShingle | Chemistry Pump, Eva Viger-Gravel, Jasmine Abou-Hamad, Edy Samantaray, Manoja K. Hamzaoui, Bilel Gurinov, Andrei Anjum, Dalaver H. Gajan, David Lesage, Anne Bendjeriou-Sedjerari, Anissa Emsley, Lyndon Basset, Jean-Marie Reactive surface organometallic complexes observed using dynamic nuclear polarization surface enhanced NMR spectroscopy |
title | Reactive surface organometallic complexes observed using dynamic nuclear polarization surface enhanced NMR spectroscopy
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title_full | Reactive surface organometallic complexes observed using dynamic nuclear polarization surface enhanced NMR spectroscopy
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title_fullStr | Reactive surface organometallic complexes observed using dynamic nuclear polarization surface enhanced NMR spectroscopy
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title_full_unstemmed | Reactive surface organometallic complexes observed using dynamic nuclear polarization surface enhanced NMR spectroscopy
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title_short | Reactive surface organometallic complexes observed using dynamic nuclear polarization surface enhanced NMR spectroscopy
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title_sort | reactive surface organometallic complexes observed using dynamic nuclear polarization surface enhanced nmr spectroscopy |
topic | Chemistry |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5365068/ https://www.ncbi.nlm.nih.gov/pubmed/28451174 http://dx.doi.org/10.1039/c6sc02379g |
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