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Rapid acquisition of wideline MAS solid-state NMR spectra with fast MAS, proton detection, and dipolar HMQC pulse sequences

TitleRapid acquisition of wideline MAS solid-state NMR spectra with fast MAS, proton detection, and dipolar HMQC pulse sequences
Publication TypeJournal Article
Year of Publication2016
AuthorsRossini, AJ, Hanrahan, MP, Thuo, M
JournalPhysical Chemistry Chemical Physics
Volume18
Pagination25284-25295
Date Published09
Type of ArticleArticle
ISBN Number1463-9076
Accession NumberWOS:000384249300055
Keywordsadiabatic pulses, chemistry, cross-polarization, distance measurements, functionalized mesoporous silicas, integer quadrupolar nuclei, magnetic-resonance, paramagnetic systems, physics, polarization transfer, sensitivity enhancement, vanadium chloroperoxidase
Abstract

1/2). These NMR interactions often give rise to wideline solid-state NMR spectra which can span hundreds of kHz or several MHz. Here we demonstrate that by using fast MAS, proton detection and dipolar hetero-nuclear multiple-quantum (D-HMQC) pulse sequences, it is possible to rapidly acquire 2D spectra which correlate H-1 chemical shifts to the indirectly detected wideline MAS powder patterns of dipolar coupled heteronuclei. The D-HMQC pulse sequence enables broadband excitation of the wideline hetero-nuclear NMR spectrum and provides higher sensitivity by detecting the narrower and more sensitive H-1 NMR signal. This approach is demonstrated for the rapid acquisition of 2D H-1 detected Pt-195 solid-state NMR spectra of cisplatin and transplatin and the Ga-71 solid-state NMR spectrum of a self-assembled Ga coordination polymer of unconfirmed structure. This approach should be broadly applicable for the rapid acquisition of wideline MAS solid-state NMR spectra of moderately abundant NMR nuclei.

DOI10.1039/c6cp04279a
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Alternate JournalPhys. Chem. Chem. Phys.