Campus Units

Materials Science and Engineering, Chemistry, Ames Laboratory

Document Type

Article

Publication Version

Published Version

Publication Date

2016

Journal or Book Title

Physical Chemistry Chemical Physics

Volume

18

Issue

36

First Page

25284

Last Page

25295

DOI

10.1039/C6CP04279A

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.

Comments

This article is published as Rossini, Aaron J., Michael P. Hanrahan, and Martin Thuo. "Rapid acquisition of wideline MAS solid-state NMR spectra with fast MAS, proton detection, and dipolar HMQC pulse sequences." Physical Chemistry Chemical Physics 18, no. 36 (2016): 25284-25295, doi:10.1039/C6CP04279A . Posted with permission.

Creative Commons License

Creative Commons Attribution-Noncommercial 3.0 License
This work is licensed under a Creative Commons Attribution-Noncommercial 3.0 License

Copyright Owner

The Owner Societies

Language

en

File Format

application/pdf

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