Search Menu
DOE PAGES title logo U.S. Department of Energy
Office of Scientific and Technical Information
Search Scholarly Publications

Title: Indirect detection of infinite-speed MAS solid-state NMR spectra

Abstract

Heavy spin-1/2 nuclides are known to possess very large chemical shift anisotropies that can challenge even the most advanced magic-angle-spinning (MAS) techniques. Wide manifolds of overlapping spinning sidebands and insufficient excitation bandwidths often obfuscate meaningful spectral information and force the use of static, low-resolution solid-state (SS)NMR methods for the characterization of materials. In order to address these issues, we have merged fast-magic-angle-turning (MAT) and dipolar heteronuclear multiple-quantum coherence (D-HMQC) experiments to obtain D-HMQC-MAT pulse sequences which enable the rapid acquisition of 2D SSNMR spectra that correlate isotropic 1H chemical shifts to the indirectly detected isotropic “infinite-MAS” spectra of heavy spin-1/2 nuclides. Furthermore, for these nuclides, the combination of fast MAS and 1H detection provides a high sensitivity, which rivals the DNP-enhanced ultra-wideline SSNMR. The new pulse sequences were used to determine the Pt coordination environments in a complex mixture of decomposition products of transplatin and in a metal-organic framework with Pt ions coordinated to the linker ligands.

Authors:
 [1];  [2];  [2];  [3];  [2];  [2];  [2]
+ Show Author Affiliations
  1. Ames Lab., Ames, IA (United States)
  2. Ames Lab., Ames, IA (United States); Iowa State Univ., Ames, IA (United States). Dept. of Chemistry
  3. Iowa State Univ., Ames, IA (United States). Dept. of Chemistry
Publication Date:
Research Org.:
Ames Laboratory (AMES), Ames, IA (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
OSTI Identifier:
1347897
Alternate Identifier(s):
OSTI ID: 1412960
Report Number(s):
IS-J-9222
Journal ID: ISSN 1090-7807; PII: S1090780717300101; TRN: US1800090
Grant/Contract Number:  
AC02-07CH11358
Resource Type:
Accepted Manuscript
Journal Name:
Journal of Magnetic Resonance
Additional Journal Information:
Journal Volume: 276; Journal Issue: C; Journal ID: ISSN 1090-7807
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; ultra-fast MAS; magic-angle-turning; D-HMQC; Platinum NMR; metal-organic-framework

Citation Formats

Perras, Frédéric A., Venkatesh, Amrit, Hanrahan, Michael P., Goh, Tian Wei, Huang, Wenyu, Rossini, Aaron J., and Pruski, Marek. Indirect detection of infinite-speed MAS solid-state NMR spectra. United States: N. p., 2017. Web. doi:10.1016/j.jmr.2017.01.010.
Copy to clipboard
Perras, Frédéric A., Venkatesh, Amrit, Hanrahan, Michael P., Goh, Tian Wei, Huang, Wenyu, Rossini, Aaron J., & Pruski, Marek. Indirect detection of infinite-speed MAS solid-state NMR spectra. United States. https://doi.org/10.1016/j.jmr.2017.01.010
Copy to clipboard
Perras, Frédéric A., Venkatesh, Amrit, Hanrahan, Michael P., Goh, Tian Wei, Huang, Wenyu, Rossini, Aaron J., and Pruski, Marek. Wed . "Indirect detection of infinite-speed MAS solid-state NMR spectra". United States. https://doi.org/10.1016/j.jmr.2017.01.010. https://www.osti.gov/servlets/purl/1347897.
Copy to clipboard
@article{osti_1347897,
title = {Indirect detection of infinite-speed MAS solid-state NMR spectra},
author = {Perras, Frédéric A. and Venkatesh, Amrit and Hanrahan, Michael P. and Goh, Tian Wei and Huang, Wenyu and Rossini, Aaron J. and Pruski, Marek},
abstractNote = {Heavy spin-1/2 nuclides are known to possess very large chemical shift anisotropies that can challenge even the most advanced magic-angle-spinning (MAS) techniques. Wide manifolds of overlapping spinning sidebands and insufficient excitation bandwidths often obfuscate meaningful spectral information and force the use of static, low-resolution solid-state (SS)NMR methods for the characterization of materials. In order to address these issues, we have merged fast-magic-angle-turning (MAT) and dipolar heteronuclear multiple-quantum coherence (D-HMQC) experiments to obtain D-HMQC-MAT pulse sequences which enable the rapid acquisition of 2D SSNMR spectra that correlate isotropic 1H chemical shifts to the indirectly detected isotropic “infinite-MAS” spectra of heavy spin-1/2 nuclides. Furthermore, for these nuclides, the combination of fast MAS and 1H detection provides a high sensitivity, which rivals the DNP-enhanced ultra-wideline SSNMR. The new pulse sequences were used to determine the Pt coordination environments in a complex mixture of decomposition products of transplatin and in a metal-organic framework with Pt ions coordinated to the linker ligands.},
doi = {10.1016/j.jmr.2017.01.010},
journal = {Journal of Magnetic Resonance},
number = C,
volume = 276,
place = {United States},
year = {Wed Jan 18 00:00:00 EST 2017},
month = {Wed Jan 18 00:00:00 EST 2017}
}
Copy to clipboard
Journal Article:
Free Publicly Available Full Text
Publisher's Version of Record
https://doi.org/10.1016/j.jmr.2017.01.010
Copyright Statement
Other availability
Search WorldCat Search WorldCat to find libraries that may hold this journal
Citation Metrics:
Cited by: 32 works
Citation information provided by
Web of Science
Save / Share:
Export Metadata
Save to My Library
You must Sign In or Create an Account in order to save documents to your library.

Works referenced in this record:

Ultra-Wideline Solid-State NMR Spectroscopy
journal, June 2013

  • Schurko, Robert W.
  • Accounts of Chemical Research, Vol. 46, Issue 9
  • DOI: 10.1021/ar400045t

71Ga and 69Ga nuclear magnetic resonance study of β-Ga2O3: resolution of four- and six-fold coordinated Ga sites in static conditions
journal, May 1995

  • Massiot, Dominique; Farnan, Ian; Gautier, Nathalie
  • Solid State Nuclear Magnetic Resonance, Vol. 4, Issue 4
  • DOI: 10.1016/0926-2040(95)00002-8

Adsorption of rubidium(1+) to .gamma.-alumina as followed by solid-state rubidium-87 NMR spectroscopy
journal, March 1989

  • Cheng, John T.; Ellis, Paul D.
  • The Journal of Physical Chemistry, Vol. 93, Issue 6
  • DOI: 10.1021/j100343a061

Nuclear magnetic resonance study of the bonding and diffusion of CO chemisorbed on Pd
journal, March 1987

  • Shore, Susan E.; Ansermet, Jean-Philippe; Slichter, Charles P.
  • Physical Review Letters, Vol. 58, Issue 9
  • DOI: 10.1103/PhysRevLett.58.953

Sensitivity-Enhanced Quadrupolar-Echo NMR of Half-Integer Quadrupolar Nuclei. Magnitudes and Relative Orientation of Chemical Shielding and Quadrupolar Coupling Tensors
journal, November 1997

  • Larsen, Flemming H.; Jakobsen, Hans J.; Ellis, Paul D.
  • The Journal of Physical Chemistry A, Vol. 101, Issue 46
  • DOI: 10.1021/jp971547b

Solid-State QCPMG NMR of Low-γ Quadrupolar Metal Nuclei in Natural Abundance
journal, July 2000

  • Larsen, Flemming H.; Skibsted, Jørgen; Jakobsen, Hans J.
  • Journal of the American Chemical Society, Vol. 122, Issue 29
  • DOI: 10.1021/ja0003526

Central Transition Nuclear Magnetic Resonance in the Presence of Large Quadrupole Couplings:  Cobalt-59 Nuclear Magnetic Resonance of Cobaltophthalocyanines †
journal, June 1999

  • Medek, Ales; Frydman, Veronica; Frydman, Lucio
  • The Journal of Physical Chemistry A, Vol. 103, Issue 25
  • DOI: 10.1021/jp990410d

Slow turning reveals enormous quadrupolar interactions (STREAQI)
journal, June 2007

Quadrupolar nuclear magnetic resonance spectroscopy in solids using frequency-swept echoing pulses
journal, November 2007

  • Bhattacharyya, Rangeet; Frydman, Lucio
  • The Journal of Chemical Physics, Vol. 127, Issue 19
  • DOI: 10.1063/1.2793783

Adiabatic Pulses for Wideband Inversion and Broadband Decoupling
journal, August 1995

  • Kupce, E.; Freeman, R.
  • Journal of Magnetic Resonance, Series A, Vol. 115, Issue 2
  • DOI: 10.1006/jmra.1995.1179

QCPMG using adiabatic pulses for faster acquisition of ultra-wideline NMR spectra
journal, October 2008

Broadband adiabatic inversion pulses for cross polarization in wideline solid-state NMR spectroscopy
journal, November 2012

  • Harris, Kristopher J.; Lupulescu, Adonis; Lucier, Bryan E. G.
  • Journal of Magnetic Resonance, Vol. 224
  • DOI: 10.1016/j.jmr.2012.08.015

DNP-Enhanced Ultrawideline Solid-State NMR Spectroscopy: Studies of Platinum in Metal–Organic Frameworks
journal, June 2016

  • Kobayashi, Takeshi; Perras, Frédéric A.; Goh, Tian Wei
  • The Journal of Physical Chemistry Letters, Vol. 7, Issue 13
  • DOI: 10.1021/acs.jpclett.6b00860

35 Cl dynamic nuclear polarization solid-state NMR of active pharmaceutical ingredients
journal, January 2016

  • Hirsh, David A.; Rossini, Aaron J.; Emsley, Lyndon
  • Physical Chemistry Chemical Physics, Vol. 18, Issue 37
  • DOI: 10.1039/C6CP04353D

Fast magic-angle sample spinning solid-state NMR at 60–100 kHz for natural abundance samples
journal, September 2016

Ultrafast Magic-Angle Spinning: Benefits for the Acquisition of Ultrawide-Line NMR Spectra of Heavy Spin-1/2 Nuclei
journal, January 2016

  • Pöppler, Ann-Christin; Demers, Jean-Philippe; Malon, Michal
  • ChemPhysChem, Vol. 17, Issue 6
  • DOI: 10.1002/cphc.201501136

Implementing solenoid microcoils for wide-line solid-state NMR
journal, March 2004

  • Yamauchi, K.; Janssen, J. W. G.; Kentgens, A. P. M.
  • Journal of Magnetic Resonance, Vol. 167, Issue 1
  • DOI: 10.1016/j.jmr.2003.12.003

High-resolution liquid- and solid-state nuclear magnetic resonance of nanoliter sample volumes using microcoil detectors
journal, February 2008

  • Kentgens, A. P. M.; Bart, J.; van Bentum, P. J. M.
  • The Journal of Chemical Physics, Vol. 128, Issue 5
  • DOI: 10.1063/1.2833560

Application of static microcoils and WURST pulses for solid-state ultra-wideline NMR spectroscopy of quadrupolar nuclei
journal, December 2008

Broadband “Infinite-Speed” Magic-Angle Spinning NMR Spectroscopy
journal, June 2009

  • Hu, Yan-Yan; Levin, E. M.; Schmidt-Rohr, Klaus
  • Journal of the American Chemical Society, Vol. 131, Issue 24
  • DOI: 10.1021/ja903334p

Technical aspects of fast magic-angle turning NMR for dilute spin-1/2 nuclei with broad spectra
journal, September 2011

High-resolution chemical shift and chemical shift anisotropy correlation in solids using slow magic angle spinning
journal, October 1992

  • Gan, Zhehong
  • Journal of the American Chemical Society, Vol. 114, Issue 21
  • DOI: 10.1021/ja00047a062

Isotropic High Field NMR Spectra of Li-Ion Battery Materials with Anisotropy >1 MHz
journal, January 2012

  • Hung, Ivan; Zhou, Lina; Pourpoint, Frédérique
  • Journal of the American Chemical Society, Vol. 134, Issue 4
  • DOI: 10.1021/ja209600m

Rapid acquisition of wideline MAS solid-state NMR spectra with fast MAS, proton detection, and dipolar HMQC pulse sequences
journal, January 2016

  • Rossini, Aaron J.; Hanrahan, Michael P.; Thuo, Martin
  • Physical Chemistry Chemical Physics, Vol. 18, Issue 36
  • DOI: 10.1039/C6CP04279A

Sensitivity Enhancement in Solid State 15N NMR by Indirect Detection with High-Speed Magic Angle Spinning
journal, January 2000

  • Ishii, Yoshitaka; Tycko, Robert
  • Journal of Magnetic Resonance, Vol. 142, Issue 1
  • DOI: 10.1006/jmre.1999.1976

Sensitivity Enhancement in Solid-State 13 C NMR of Synthetic Polymers and Biopolymers by 1 H NMR Detection with High-Speed Magic Angle Spinning
journal, March 2001

  • Ishii, Yoshitaka; Yesinowski, James P.; Tycko, Robert
  • Journal of the American Chemical Society, Vol. 123, Issue 12
  • DOI: 10.1021/ja015505j

Chemical Shift Correlation NMR Spectroscopy with Indirect Detection in Fast Rotating Solids:  Studies of Organically Functionalized Mesoporous Silicas
journal, September 2007

  • Wiench, Jerzy W.; Bronnimann, Charles E.; Lin, Victor S. -Y
  • Journal of the American Chemical Society, Vol. 129, Issue 40, p. 12076-12077
  • DOI: 10.1021/ja074746+

Proton-Detected Solid-State NMR Spectroscopy of Fully Protonated Proteins at 40 kHz Magic-Angle Spinning
journal, September 2007

  • Zhou, Donghua H.; Shah, Gautam; Cormos, Mircea
  • Journal of the American Chemical Society, Vol. 129, Issue 38
  • DOI: 10.1021/ja073462m

13C/14N heteronuclear multiple-quantum correlation with rotary resonance and REDOR dipolar recoupling
journal, January 2007

Sideband manipulation in magic-angle-spinning nuclear magnetic resonance
journal, October 1999

Spinning‐sideband‐free and spinning‐sideband‐only NMR spectra in spinning samples
journal, August 1982

  • Dixon, W. Thomas
  • The Journal of Chemical Physics, Vol. 77, Issue 4
  • DOI: 10.1063/1.444076

Magic-Angle Spinning Sideband Elimination by Temporary Interruption of the Chemical Shift
journal, November 1993

  • Hong, J.; Harbison, G. S.
  • Journal of Magnetic Resonance, Series A, Vol. 105, Issue 2
  • DOI: 10.1006/jmra.1993.1264

Fast adiabatic pulses for solid-state NMR of paramagnetic systems
journal, February 2007

Spin-Transfer Pathways in Paramagnetic Lithium Transition-Metal Phosphates from Combined Broadband Isotropic Solid-State MAS NMR Spectroscopy and DFT Calculations
journal, October 2012

  • Clément, Raphaële J.; Pell, Andrew J.; Middlemiss, Derek S.
  • Journal of the American Chemical Society, Vol. 134, Issue 41
  • DOI: 10.1021/ja306876u

Proton-Selective 17 O− 1 H Distance Measurements in Fast Magic-Angle-Spinning Solid-State NMR Spectroscopy for the Determination of Hydrogen Bond Lengths
journal, November 2006

  • Brinkmann, Andreas; Kentgens, Arno P. M.
  • Journal of the American Chemical Society, Vol. 128, Issue 46
  • DOI: 10.1021/ja065415k

Comparison of several hetero-nuclear dipolar recoupling NMR methods to be used in MAS HMQC/HSQC
journal, May 2008

Cogwheel Phase Cycling
journal, April 2002

  • Levitt, Malcolm H.; Madhu, P. K.; Hughes, Colan E.
  • Journal of Magnetic Resonance, Vol. 155, Issue 2
  • DOI: 10.1006/jmre.2002.2520

Calculation of coherence pathway selection and cogwheel cycles
journal, January 2003

Magic-Angle-Turning Experiments for Measuring Chemical-Shift-Tensor Principal Values in Powdered Solids
journal, April 1995

  • Hu, J. Z.; Wang, W.; Liu, F.
  • Journal of Magnetic Resonance, Series A, Vol. 113, Issue 2
  • DOI: 10.1006/jmra.1995.1082

A reduced power selective adiabatic spin-echo pulse sequence
journal, March 1991

  • Conolly, Steven; Glover, Gary; Nishimura, Dwight
  • Magnetic Resonance in Medicine, Vol. 18, Issue 1
  • DOI: 10.1002/mrm.1910180105

ZFiltering in MQMAS NMR
journal, November 1996

  • Amoureux, Jean-Paul; Fernandez, Christian; Steuernagel, Stefan
  • Journal of Magnetic Resonance, Series A, Vol. 123, Issue 1
  • DOI: 10.1006/jmra.1996.0221

Application of cogwheel phase cycling to sideband manipulation experiments in solid-state NMR
journal, October 2003

SIMPSON: A General Simulation Program for Solid-State NMR Spectroscopy
journal, December 2000

  • Bak, Mads; Rasmussen, Jimmy T.; Nielsen, Niels Chr
  • Journal of Magnetic Resonance, Vol. 147, Issue 2
  • DOI: 10.1006/jmre.2000.2179

Optimal control in NMR spectroscopy: Numerical implementation in SIMPSON
journal, April 2009

  • Tošner, Zdeněk; Vosegaard, Thomas; Kehlet, Cindie
  • Journal of Magnetic Resonance, Vol. 197, Issue 2
  • DOI: 10.1016/j.jmr.2008.11.020

Insights into the mechanism of action of platinum anticancer drugs from multinuclear NMR spectroscopy
journal, August 2006

  • Berners-Price, Susan J.; Ronconi, Luca; Sadler, Peter J.
  • Progress in Nuclear Magnetic Resonance Spectroscopy, Vol. 49, Issue 1
  • DOI: 10.1016/j.pnmrs.2006.05.002

Platinum NMR Spectroscopy
book, January 1986

Selective Host-Guest Interaction between Metal Ions and Metal-Organic Frameworks Using Dynamic Nuclear Polarization Enhanced Solid-State NMR Spectroscopy
journal, October 2014

  • Guo, Zhiyong; Kobayashi, Takeshi; Wang, Lin-Lin
  • Chemistry - A European Journal, Vol. 20, Issue 49
  • DOI: 10.1002/chem.201403884
    Sort by:
    [ × clear filter / sort ]

    Works referencing / citing this record:

    Resolving the Core and the Surface of CdSe Quantum Dots and Nanoplatelets Using Dynamic Nuclear Polarization Enhanced PASS–PIETA NMR Spectroscopy
    journal, June 2018

      Sort by:
      [ × clear filter / sort ]

      Similar Records in DOE PAGES and OSTI.GOV collections: