Structural Elucidation of Amorphous Photocatalytic Polymers from Dynamic Nuclear Polarization Enhanced Solid State NMR

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Brownbill, NJ, Sprick, RS, Bonillo, B, Pawsey, S, Aussenac, F, Fielding, AJ, Cooper, AI and Blanc, F (2018) Structural Elucidation of Amorphous Photocatalytic Polymers from Dynamic Nuclear Polarization Enhanced Solid State NMR. Macromolecules, 51 (8). pp. 3088-3096. ISSN 0024-9297

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Publisher URL: http://dx.doi.org/10.1021/acs.macromol.7b02544

Abstract

Dynamic nuclear polarization (DNP) solid-state nuclear magnetic resonance (NMR) offers a recent approach to dramatically enhance NMR signals and has enabled detailed structural information to be obtained in a series of amorphous photocatalytic copolymers of alternating pyrene and benzene monomer units, the structures of which cannot be reliably established by other spectroscopic or analytical techniques. Large 13C cross-polarization (CP) magic angle spinning (MAS) signal enhancements were obtained at high magnetic fields (9.4–14.1 T) and low temperature (110–120 K), permitting the acquisition of a 13C INADEQUATE spectrum at natural abundance and facilitating complete spectral assignments, including when small amounts of specific monomers are present. The high 13C signal-to-noise ratios obtained are harnessed to record quantitative multiple contact CP NMR data, used to determine the polymers’ composition. This correlates well with the putative pyrene:benzene stoichiometry from the monomer feed ratio, enabling their structures to be understood.

Item Type:	Article
Uncontrolled Keywords:	03 Chemical Sciences, 09 Engineering
Subjects:	Q Science > QD Chemistry
Divisions:	Pharmacy and Biomolecular Sciences
Publisher:	American Chemical Society
Related URLs:	http://gateway.webofknowledge.com/gateway/Gateway.cgi?GWVersion=2&SrcApp=PARTNER_APP&SrcAuth=LinksAMR&KeyUT=WOS:000431088700033&DestLinkType=FullRecord&DestApp=ALL_WOS&UsrCustomerID=7f77ca1697db64ccb27a8011c7ced90d
Date of acceptance:	23 March 2018
Date of first compliant Open Access:	27 June 2018
Date Deposited:	27 Jun 2018 10:15
Last Modified:	04 Sep 2021 10:22
DOI or ID number:	10.1021/acs.macromol.7b02544
URI:	https://ljmu-9.eprints-hosting.org/id/eprint/8900

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