Issue 36, 2016

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

Abstract

The solid-state NMR spectra of many NMR active elements are often extremely broad due to the presence of chemical shift anisotropy (CSA) and/or the quadrupolar interaction (for nuclei with spin I > 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 1H chemical shifts to the indirectly detected wideline MAS powder patterns of dipolar coupled hetero-nuclei. 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 1H NMR signal. This approach is demonstrated for the rapid acquisition of 2D 1H detected 195Pt solid-state NMR spectra of cisplatin and transplatin and the 71Ga 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.

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

Supplementary files

Article information

Article type
Paper
Submitted
21 Jun 2016
Accepted
22 Aug 2016
First published
22 Aug 2016
This article is Open Access
Creative Commons BY-NC license

Phys. Chem. Chem. Phys., 2016,18, 25284-25295

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

A. J. Rossini, M. P. Hanrahan and M. Thuo, Phys. Chem. Chem. Phys., 2016, 18, 25284 DOI: 10.1039/C6CP04279A

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