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

作者: Aaron J. Rossini , Michael P. Hanrahan , Martin Thuo

DOI: 10.1039/C6CP04279A

关键词:

摘要: The solid-state NMR spectra of many active elements are often extremely broad due to the presence chemical shift anisotropy (CSA) and/or quadrupolar interaction (for nuclei with spin I > 1/2). These interactions give rise wideline which can span hundreds 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 rapidly acquire 2D correlate 1H shifts indirectly detected MAS powder patterns coupled hetero-nuclei. D-HMQC sequence enables broadband excitation spectrum provides higher sensitivity detecting narrower more sensitive signal. This approach demonstrated for rapid acquisition 195Pt cisplatin transplatin 71Ga a self-assembled Ga coordination polymer unconfirmed structure. should be broadly applicable moderately abundant nuclei.

参考文章(91)
FLEMMING H. LARSEN, HANS J. JAKOBSEN, PAUL D. ELLIS, NIELS CHR. NIELSEN, High-field QCPMG-MAS NMR of half-integer quadrupolar nuclei with large quadrupole couplings Molecular Physics. ,vol. 95, pp. 1185- 1195 ,(1998) , 10.1080/00268979809483250
Flemming H. Larsen, Hans J. Jakobsen, Paul D. Ellis, Niels Chr. Nielsen, QCPMG-MAS NMR of Half-Integer Quadrupolar Nuclei Journal of Magnetic Resonance. ,vol. 131, pp. 144- 147 ,(1998) , 10.1006/JMRE.1997.1341
Kristopher J. Harris, Adonis Lupulescu, Bryan E.G. Lucier, Lucio Frydman, Robert W. Schurko, Broadband adiabatic inversion pulses for cross polarization in wideline solid-state NMR spectroscopy. Journal of Magnetic Resonance. ,vol. 224, pp. 38- 47 ,(2012) , 10.1016/J.JMR.2012.08.015
Paulus J. Knijn, P. Jan M. van Bentum, Ernst R. H. van Eck, Changming Fang, Dennis L. A. G. Grimminck, Robert A. de Groot, Remco W. A. Havenith, Martijn Marsman, W. Leo Meerts, Gilles A. de Wijs, Arno P. M. Kentgens, A solid-state NMR and DFT study of compositional modulations in AlxGa1−xAs Physical Chemistry Chemical Physics. ,vol. 12, pp. 11517- 11535 ,(2010) , 10.1039/C003624B
Luke A. O'Dell, Rongliang He, Jessica Pandohee, Identifying H–N proximities in solid-state NMR using 14N overtone irradiation under fast MAS CrystEngComm. ,vol. 15, pp. 8657- 8667 ,(2013) , 10.1039/C3CE40967H
Sheetal K Jain, Anders B Nielsen, Matthias Hiller, Liselotte Handel, Matthias Ernst, Hartmut Oschkinat, Ümit Akbey, Niels Chr Nielsen, None, Low-power polarization transfer between deuterons and spin-1/2 nuclei using adiabatic RESPIRATIONCP in solid-state NMR Physical Chemistry Chemical Physics. ,vol. 16, pp. 2827- 2830 ,(2014) , 10.1039/C3CP54419B
Andreas Brinkmann, Arno P. M. Kentgens, Proton-Selective17O−1H Distance Measurements in Fast Magic-Angle-Spinning Solid-State NMR Spectroscopy for the Determination of Hydrogen Bond Lengths Journal of the American Chemical Society. ,vol. 128, pp. 14758- 14759 ,(2006) , 10.1021/JA065415K
Sharon E. Ashbrook, Melinda J. Duer, Structural information from quadrupolar nuclei in solid state NMR Concepts in Magnetic Resonance Part A. ,vol. 28A, pp. 183- 248 ,(2006) , 10.1002/CMR.A.20053
Zdeněk Tošner, Thomas Vosegaard, Cindie Kehlet, Navin Khaneja, Steffen J. Glaser, Niels Chr. Nielsen, Optimal control in NMR spectroscopy: Numerical implementation in SIMPSON Journal of Magnetic Resonance. ,vol. 197, pp. 120- 134 ,(2009) , 10.1016/J.JMR.2008.11.020