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

Nick J. Brownbill | Zendy; Reiner Sebastian Sprick | Zendy; Baltasar Bonillo | Zendy; Shane Pawsey | Zendy; Fabien Aussenac | Zendy; Alistair J. Fielding | Zendy; Andrew I. Cooper | Zendy; Frédéric Blanc | Zendy

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

Author(s) -

Nick J. Brownbill,

Reiner Sebastian Sprick,

Baltasar Bonillo,

Shane Pawsey,

Fabien Aussenac,

Alistair J. Fielding,

Andrew I. Cooper,

Frédéric Blanc

Publication year - 2018

Publication title -

macromolecules

Language(s) - English

Resource type - Journals

SCImago Journal Rank - 1.994

H-Index - 313

eISSN - 1520-5835

pISSN - 0024-9297

DOI - 10.1021/acs.macromol.7b02544

Subject(s) - magic angle spinning , monomer , amorphous solid , pyrene , chemistry , solid state nuclear magnetic resonance , carbon 13 nmr , polymer , nuclear magnetic resonance spectroscopy , polarization (electrochemistry) , benzene , analytical chemistry (journal) , nuclear magnetic resonance , materials science , crystallography , organic chemistry , physics

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, enabl...

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