skip to main content
DOE PAGES title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Enhancing the resolution of 1 H and 13 C solid-state NMR spectra by reduction of anisotropic bulk magnetic susceptibility broadening

Abstract

2D HETCOR experiments enhance the resolution of 1H and 13C solid-state NMR spectra by reducing anisotropic bulk magnetic susceptibility (ABMS) signal broadening.

Authors:
 [1];  [1];  [1];  [2]; ORCiD logo [3];  [2]; ORCiD logo [1]
  1. Iowa State Univ., Ames, IA (United States). Dept. of Chemistry; Ames Lab., Ames, IA (United States)
  2. Univ. of Kentucky, Lexington, KY (United States). College of Pharmacy
  3. Genentech Inc., South San Francisco, CA (United States). Dept. of Small Molecule Pharmaceutical Sciences
Publication Date:
Research Org.:
Ames Laboratory (AMES), Ames, IA (United States)
Sponsoring Org.:
USDOE; National Science Foundation (NSF)
OSTI Identifier:
1408913
Report Number(s):
IS-J 9484
Journal ID: ISSN 1463-9076; PPCPFQ; TRN: US1703313
Grant/Contract Number:  
AC02-07CH11358; 1709972; 1710453
Resource Type:
Accepted Manuscript
Journal Name:
Physical Chemistry Chemical Physics. PCCP (Print)
Additional Journal Information:
Journal Name: Physical Chemistry Chemical Physics. PCCP (Print); Journal Volume: 19; Journal Issue: 41; Journal ID: ISSN 1463-9076
Publisher:
Royal Society of Chemistry
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats

Hanrahan, Michael P., Venkatesh, Amrit, Carnahan, Scott L., Calahan, Julie L., Lubach, Joseph W., Munson, Eric J., and Rossini, Aaron J. Enhancing the resolution of 1 H and 13 C solid-state NMR spectra by reduction of anisotropic bulk magnetic susceptibility broadening. United States: N. p., 2017. Web. doi:10.1039/C7CP04223J.
Hanrahan, Michael P., Venkatesh, Amrit, Carnahan, Scott L., Calahan, Julie L., Lubach, Joseph W., Munson, Eric J., & Rossini, Aaron J. Enhancing the resolution of 1 H and 13 C solid-state NMR spectra by reduction of anisotropic bulk magnetic susceptibility broadening. United States. doi:10.1039/C7CP04223J.
Hanrahan, Michael P., Venkatesh, Amrit, Carnahan, Scott L., Calahan, Julie L., Lubach, Joseph W., Munson, Eric J., and Rossini, Aaron J. Mon . "Enhancing the resolution of 1 H and 13 C solid-state NMR spectra by reduction of anisotropic bulk magnetic susceptibility broadening". United States. doi:10.1039/C7CP04223J. https://www.osti.gov/servlets/purl/1408913.
@article{osti_1408913,
title = {Enhancing the resolution of 1 H and 13 C solid-state NMR spectra by reduction of anisotropic bulk magnetic susceptibility broadening},
author = {Hanrahan, Michael P. and Venkatesh, Amrit and Carnahan, Scott L. and Calahan, Julie L. and Lubach, Joseph W. and Munson, Eric J. and Rossini, Aaron J.},
abstractNote = {2D HETCOR experiments enhance the resolution of1H and13C solid-state NMR spectra by reducing anisotropic bulk magnetic susceptibility (ABMS) signal broadening.},
doi = {10.1039/C7CP04223J},
journal = {Physical Chemistry Chemical Physics. PCCP (Print)},
number = 41,
volume = 19,
place = {United States},
year = {2017},
month = {9}
}

Journal Article:
Free Publicly Available Full Text
Publisher's Version of Record

Citation Metrics:
Cited by: 5 works
Citation information provided by
Web of Science

Save / Share:

Works referenced in this record:

Solid-State NMR of a Paramagnetic DIAD-Fe II Catalyst:  Sensitivity, Resolution Enhancement, and Structure-Based Assignments
journal, October 2006

  • Kervern, Gwendal; Pintacuda, Guido; Zhang, Yong
  • Journal of the American Chemical Society, Vol. 128, Issue 41
  • DOI: 10.1021/ja063510n

Study of Intermolecular Interactions in the Corrole Matrix by Solid-State NMR under 100 kHz MAS and Theoretical Calculations
journal, November 2013

  • Kobayashi, Takeshi; Mao, Kanmi; Paluch, Piotr
  • Angewandte Chemie International Edition, Vol. 52, Issue 52
  • DOI: 10.1002/anie.201305475

The Third Ambient Aspirin Polymorph
journal, May 2017

  • Shtukenberg, Alexander G.; Hu, Chunhua T.; Zhu, Qiang
  • Crystal Growth & Design, Vol. 17, Issue 6
  • DOI: 10.1021/acs.cgd.7b00673

An Improved Broadband Decoupling Sequence for Liquid Crystals and Solids
journal, January 2000

  • Fung, B. M.; Khitrin, A. K.; Ermolaev, Konstantin
  • Journal of Magnetic Resonance, Vol. 142, Issue 1
  • DOI: 10.1006/jmre.1999.1896

Generalized Gradient Approximation Made Simple
journal, October 1996

  • Perdew, John P.; Burke, Kieron; Ernzerhof, Matthias
  • Physical Review Letters, Vol. 77, Issue 18, p. 3865-3868
  • DOI: 10.1103/PhysRevLett.77.3865

Chemical Shift Correlations in Disordered Solids
journal, March 2005

  • Cadars, Sylvian; Lesage, Anne; Emsley, Lyndon
  • Journal of the American Chemical Society, Vol. 127, Issue 12
  • DOI: 10.1021/ja043698f

Combining insights from solid-state NMR and first principles calculation: applications to the 19F NMR of octafluoronaphthalene
journal, January 2007

  • Robbins, Andrew J.; Ng, William T. K.; Jochym, Dominik
  • Physical Chemistry Chemical Physics, Vol. 9, Issue 19
  • DOI: 10.1039/b701291h

Origins of linewidth in H1 magic-angle spinning NMR
journal, October 2006

  • Zorin, Vadim E.; Brown, Steven P.; Hodgkinson, Paul
  • The Journal of Chemical Physics, Vol. 125, Issue 14
  • DOI: 10.1063/1.2357602

Five decades of homonuclear dipolar decoupling in solid-state NMR: Status and outlook
journal, November 2016

  • Mote, Kaustubh R.; Agarwal, Vipin; Madhu, P. K.
  • Progress in Nuclear Magnetic Resonance Spectroscopy, Vol. 97
  • DOI: 10.1016/j.pnmrs.2016.08.001

Rationalising Heteronuclear Decoupling in Refocussing Applications of Solid-State NMR Spectroscopy
journal, January 2017

  • Frantsuzov, Ilya; Vasa, Suresh K.; Ernst, Matthias
  • ChemPhysChem, Vol. 18, Issue 4
  • DOI: 10.1002/cphc.201601003

The dissolution of aspirin and aspirin tablets*
journal, November 1967


1163. The crystal and molecular structure of aspirin
journal, January 1964


Dynamic Nuclear Polarization NMR Spectroscopy of Microcrystalline Solids
journal, September 2012

  • Rossini, Aaron J.; Zagdoun, Alexandre; Hegner, Franziska
  • Journal of the American Chemical Society, Vol. 134, Issue 40
  • DOI: 10.1021/ja308135r

Dynamic Nuclear Polarization of Amyloidogenic Peptide Nanocrystals:  GNNQQNY, a Core Segment of the Yeast Prion Protein Sup35p
journal, August 2006

  • van der Wel, Patrick C. A.; Hu, Kan-Nian; Lewandowski, Józef
  • Journal of the American Chemical Society, Vol. 128, Issue 33
  • DOI: 10.1021/ja0626685

Local Magnetic Field Distribution in a Polycrystalline Sample Exposed to a Strong Magnetic Field
journal, April 1996

  • Schwerk, U.; Michel, D.; Pruski, M.
  • Journal of Magnetic Resonance, Series A, Vol. 119, Issue 2
  • DOI: 10.1006/jmra.1996.0068

Homonuclear dipolar decoupling at magic-angle spinning frequencies up to 65kHz in solid-state nuclear magnetic resonance
journal, November 2008


Direct spectral optimisation of proton–proton homonuclear dipolar decoupling in solid-state NMR
journal, November 2004


A 13 C solid-state NMR investigation of four cocrystals of caffeine and theophylline
journal, February 2017

  • Vigilante, Nicolas J.; Mehta, Manish A.
  • Acta Crystallographica Section C Structural Chemistry, Vol. 73, Issue 3
  • DOI: 10.1107/S2053229617000869

Increasing 13 C CP-MAS NMR Resolution Using Single Crystals: Application to Model Octaethyl Porphyrins
journal, July 2012

  • Dugar, Sneha; Fu, Riqiang; Dalal, Naresh S.
  • The Journal of Physical Chemistry B, Vol. 116, Issue 30
  • DOI: 10.1021/jp302189r

Heteronuclear decoupling in the NMR of solids
journal, September 2005


High-resolution NMR spectra in inhomogeneous magnetic fields: application of total spin coherence transfer echoes
journal, June 1981

  • Weitekamp, D. P.; Garbow, J. R.; Murdoch, J. B.
  • Journal of the American Chemical Society, Vol. 103, Issue 12
  • DOI: 10.1021/ja00402a057

Highly Efficient, Water-Soluble Polarizing Agents for Dynamic Nuclear Polarization at High Frequency
journal, August 2013

  • Sauvée, Claire; Rosay, Melanie; Casano, Gilles
  • Angewandte Chemie International Edition, Vol. 52, Issue 41
  • DOI: 10.1002/anie.201304657

Coherence transfer echoes
journal, April 1978


Homogeneous NMR Spectra in Inhomogeneous Fields
journal, April 1996


Proton‐enhanced NMR of dilute spins in solids
journal, July 1973

  • Pines, A.; Gibby, M. G.; Waugh, J. S.
  • The Journal of Chemical Physics, Vol. 59, Issue 2
  • DOI: 10.1063/1.1680061

Mesoporous Silica Nanoparticles Loaded with Surfactant: Low Temperature Magic Angle Spinning 13 C and 29 Si NMR Enhanced by Dynamic Nuclear Polarization
journal, January 2013

  • Lafon, Olivier; Thankamony, Aany S. Lilly; Kobayashi, Takeshi
  • The Journal of Physical Chemistry C, Vol. 117, Issue 3
  • DOI: 10.1021/jp310109s

All-electron magnetic response with pseudopotentials: NMR chemical shifts
journal, May 2001


Dynamic Nuclear Polarization Enhanced NMR Spectroscopy for Pharmaceutical Formulations
journal, January 2014

  • Rossini, Aaron J.; Widdifield, Cory M.; Zagdoun, Alexandre
  • Journal of the American Chemical Society, Vol. 136, Issue 6
  • DOI: 10.1021/ja4092038

Toward Crystal Structure Prediction for Conformationally Flexible Molecules:  The Headaches Illustrated by Aspirin
journal, November 2004

  • Ouvrard, Carole; Price, Sarah L.
  • Crystal Growth & Design, Vol. 4, Issue 6
  • DOI: 10.1021/cg049922u

NMR studies of organic polymorphs & solvates
journal, January 2006


Improved Phase-Modulated Homonuclear Dipolar Decoupling for Solid-State NMR Spectroscopy from Symmetry Considerations
journal, June 2013

  • Halse, Meghan E.; Emsley, Lyndon
  • The Journal of Physical Chemistry A, Vol. 117, Issue 25
  • DOI: 10.1021/jp4038733

High-resolution solid-state 13 C μMAS NMR with long coherence life times
journal, January 2011

  • Vasa, Suresh K.; Janssen, Hans; Van Eck, Ernst R. H.
  • Phys. Chem. Chem. Phys., Vol. 13, Issue 1
  • DOI: 10.1039/C0CP01929A

High-Resolution NMR Correlation Spectra of Disordered Solids
journal, April 2003

  • Sakellariou, Dimitris; Brown, Steven P.; Lesage, Anne
  • Journal of the American Chemical Society, Vol. 125, Issue 14
  • DOI: 10.1021/ja0292389

Solid State NMR of Drugs: Soluble Aspirin
journal, October 1987

  • Díaz, Luis E.; Frydman, Lucio; Olivieri, Alejandro C.
  • Analytical Letters, Vol. 20, Issue 10
  • DOI: 10.1080/00032718708078032

Large Molecular Weight Nitroxide Biradicals Providing Efficient Dynamic Nuclear Polarization at Temperatures up to 200 K
journal, August 2013

  • Zagdoun, Alexandre; Casano, Gilles; Ouari, Olivier
  • Journal of the American Chemical Society, Vol. 135, Issue 34
  • DOI: 10.1021/ja405813t

In-Phase Ultra High-Resolution In Vivo NMR
journal, April 2017

  • Fugariu, Ioana; Bermel, Wolfgang; Lane, Daniel
  • Angewandte Chemie International Edition, Vol. 56, Issue 22
  • DOI: 10.1002/anie.201701097

Functional magnetic resonance imaging with intermolecular multiple-quantum coherences
journal, June 2000


Powder Crystallography by Combined Crystal Structure Prediction and High-Resolution 1 H Solid-State NMR Spectroscopy
journal, March 2010

  • Salager, Elodie; Day, Graeme M.; Stein, Robin S.
  • Journal of the American Chemical Society, Vol. 132, Issue 8
  • DOI: 10.1021/ja909449k

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


Non-aqueous solvents for DNP surface enhanced NMR spectroscopy
journal, January 2012

  • Zagdoun, Alexandre; Rossini, Aaron J.; Gajan, David
  • Chem. Commun., Vol. 48, Issue 5
  • DOI: 10.1039/C1CC15242D

Surface Enhanced NMR Spectroscopy by Dynamic Nuclear Polarization
journal, November 2010

  • Lesage, Anne; Lelli, Moreno; Gajan, David
  • Journal of the American Chemical Society, Vol. 132, Issue 44
  • DOI: 10.1021/ja104771z

Resolution limits in magic-angle rotation NMR spectra of polycrystalline solids
journal, March 1982


High-Field High-Speed MAS Resolution Enhancement in 1H NMR Spectroscopy of Solids
journal, November 2001

  • Samoson, A.; Tuherm, T.; Gan, Z.
  • Solid State Nuclear Magnetic Resonance, Vol. 20, Issue 3-4
  • DOI: 10.1006/snmr.2001.0037

High-resolution NMR in inhomogeneous fields
journal, October 1997


Elimination of signals tilting caused by B0 field inhomogeneity using 2D-lineshape reference deconvolution
journal, August 2017

  • Sheberstov, Kirill F.; Sinitsyn, Dmitry O.; Cheshkov, Dmitry A.
  • Journal of Magnetic Resonance, Vol. 281
  • DOI: 10.1016/j.jmr.2017.06.005

Solid-state NMR spectroscopy in pharmaceutical research and analysis
journal, November 2006

  • Berendt, Robert T.; Sperger, Diana M.; Munson, Eric J.
  • TrAC Trends in Analytical Chemistry, Vol. 25, Issue 10
  • DOI: 10.1016/j.trac.2006.07.006

Variable-Amplitude Cross-Polarization MAS NMR
journal, October 1993

  • Peersen, O. B.; Wu, X. L.; Kustanovich, I.
  • Journal of Magnetic Resonance, Series A, Vol. 104, Issue 3
  • DOI: 10.1006/jmra.1993.1231

Reference deconvolution methods
journal, September 1997

  • Morris, Gareth A.; Barjat, Hervé; Home, Timothy J.
  • Progress in Nuclear Magnetic Resonance Spectroscopy, Vol. 31, Issue 2-3
  • DOI: 10.1016/S0079-6565(97)00011-3

Solid-state13C NMR study of drugs: Aspirin
journal, September 1986

  • Chang, Ching-Jer; Díaz, Luis E.; Morin, Frederick
  • Magnetic Resonance in Chemistry, Vol. 24, Issue 9
  • DOI: 10.1002/mrc.1260240907

Two-dimensional heteronuclear chemical shift correlation spectroscopy in rotating solids
journal, May 1984

  • Roberts, James E.; Vega, Shimon; Griffin, Robert G.
  • Journal of the American Chemical Society, Vol. 106, Issue 9
  • DOI: 10.1021/ja00321a003

Diffuse scattering study of aspirin forms (I) and (II)
journal, November 2010

  • Chan, E. J.; Welberry, T. R.; Heerdegen, A. P.
  • Acta Crystallographica Section B Structural Science, Vol. 66, Issue 6
  • DOI: 10.1107/S0108768110037055

Measurement of high-resolution NMR spectra in an inhomogeneous magnetic field
journal, November 1987

  • Hall, Laurance D.; Norwood, Timothy J.
  • Journal of the American Chemical Society, Vol. 109, Issue 24
  • DOI: 10.1021/ja00258a080

An experimental study of resolution of proton chemical shifts in solids: Combined multiple pulse NMR and magic‐angle spinning
journal, January 1980

  • Ryan, L. M.; Taylor, R. E.; Paff, A. J.
  • The Journal of Chemical Physics, Vol. 72, Issue 1
  • DOI: 10.1063/1.438935

High resolution n.m.r. measurements in inhomogeneous magnetic fields: use of the SECSY pulse sequence
journal, January 1986

  • Hall, Laurance D.; Norwood, Timothy J.
  • Journal of the Chemical Society, Chemical Communications, Issue 20
  • DOI: 10.1039/c39860001508

High-Resolution, > 1 GHz NMR in Unstable Magnetic Fields
journal, October 2000


Influence of Structure on the Spectroscopic Properties of the Polymorphs of Piroxicam
journal, December 2010

  • Liu, Wei; Wang, Wei David; Wang, Wei
  • The Journal of Physical Chemistry B, Vol. 114, Issue 49
  • DOI: 10.1021/jp1084444

On the Polymorphism of Aspirin: Crystalline Aspirin as Intergrowths of Two “Polymorphic” Domains
journal, January 2007

  • Bond, Andrew D.; Boese, Roland; Desiraju, Gautam R.
  • Angewandte Chemie International Edition, Vol. 46, Issue 4
  • DOI: 10.1002/anie.200603373

Total spin coherence transfer echo spectroscopy
journal, December 1983

  • Garbow, J. R.; Weitekamp, D. P.; Pines, A.
  • The Journal of Chemical Physics, Vol. 79, Issue 11
  • DOI: 10.1063/1.445692

Soft self-consistent pseudopotentials in a generalized eigenvalue formalism
journal, April 1990


Enforcing Ostwald's rule of stages: Isolation of paracetamol forms III and II
journal, August 2007

  • Burley, Jonathan C.; Duer, Melinda J.; Stein, Robin S.
  • European Journal of Pharmaceutical Sciences, Vol. 31, Issue 5
  • DOI: 10.1016/j.ejps.2007.04.002

Single crystals of aspirin form II: crystallisation and stability
journal, January 2011

  • Bond, Andrew D.; Solanko, Katarzyna A.; Parsons, Simon
  • CrystEngComm, Vol. 13, Issue 2
  • DOI: 10.1039/C0CE00588F

Aspirin: Dissolution Rates of Two Polymorphic Forms
journal, April 1968


The Predictably Elusive Form II of Aspirin
journal, December 2005

  • Vishweshwar, Peddy; McMahon, Jennifer A.; Oliveira, Mark
  • Journal of the American Chemical Society, Vol. 127, Issue 48
  • DOI: 10.1021/ja056455b

Structural Study of Mg-Based Metal–Organic Frameworks by X-ray Diffraction, 1 H, 13 C, and 25 Mg Solid-State NMR Spectroscopy, and First-Principles Calculations
journal, March 2015

  • Mali, Gregor; Trebosc, Julien; Martineau, Charlotte
  • The Journal of Physical Chemistry C, Vol. 119, Issue 14
  • DOI: 10.1021/acs.jpcc.5b01381

Investigation of Solid-State NMR Line Widths of Ibuprofen in Drug Formulations
journal, July 2006

  • Barich, Dewey H.; Davis, Jacob M.; Schieber, Loren J.
  • Journal of Pharmaceutical Sciences, Vol. 95, Issue 7
  • DOI: 10.1002/jps.20564

Heteronuclear solid-state correlation spectroscopy
journal, July 1982


Evolution of solid-state NMR in pharmaceutical analysis
journal, June 2010


MR Imaging Contrast Enhancement Based on Intermolecular Zero Quantum Coherences
journal, July 1998


Solid-state dynamic nuclear polarization at 263 GHz: spectrometer design and experimental results
journal, January 2010

  • Rosay, Melanie; Tometich, Leo; Pawsey, Shane
  • Physical Chemistry Chemical Physics, Vol. 12, Issue 22
  • DOI: 10.1039/c003685b

Detailed analysis of the TIMES and TIMES0 high-resolution MAS methods for high-resolution proton NMR
journal, October 2012