Natural abundance 14N and 15N solid-state NMR of pharmaceuticals and their polymorphs
Abstract
14N ultra-wideline (UW), 1H{15N} indirectly-detected HETCOR (idHETCOR) and 15N dynamic nuclear polarization (DNP) solid-state NMR (SSNMR) experiments, in combination with plane-wave density functional theory (DFT) calculations of 14N EFG tensors, were utilized to characterize a series of nitrogen-containing active pharmaceutical ingredients (APIs), including HCl salts of scopolamine, alprenolol, isoprenaline, acebutolol, dibucaine, nicardipine, and ranitidine. Here, a case study applying these methods for the differentiation of polymorphs of bupivacaine HCl is also presented. All experiments were conducted upon samples with naturally-abundant nitrogen isotopes. For most of the APIs, it was possible to acquire frequency-stepped UW 14N SSNMR spectra of stationary samples, which display powder patterns corresponding to pseudo-tetrahedral (i.e., RR'R"NH+ and RR'NH2+) or other (i.e., RNH2 and RNO2) nitrogen environments.
- Authors:
-
- Univ. of Windsor, Windsor (Canada)
- Durham Univ., Durham (United Kingdom)
- Ames Lab. and Iowa State Univ., Ames, IA (United States)
- Publication Date:
- Research Org.:
- Ames Laboratory (AMES), Ames, IA (United States)
- Sponsoring Org.:
- USDOE
- OSTI Identifier:
- 1278752
- Report Number(s):
- IS-J-9006
Journal ID: ISSN 1463-9076; PPCPFQ
- Grant/Contract Number:
- AC02-07CH11358
- Resource Type:
- Journal Article: Accepted Manuscript
- Journal Name:
- Physical Chemistry Chemical Physics. PCCP
- Additional Journal Information:
- Journal Volume: 18; Journal Issue: 26; 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
Veinberg, Stanislav L., Johnston, Karen E., Jaroszewicz, Michael J., Kispal, Brianna M., Mireault, Christopher R., Kobayashi, Takeshi, Pruski, Marek, and Schurko, Robert W. Natural abundance 14N and 15N solid-state NMR of pharmaceuticals and their polymorphs. United States: N. p., 2016.
Web. doi:10.1039/C6CP02855A.
Veinberg, Stanislav L., Johnston, Karen E., Jaroszewicz, Michael J., Kispal, Brianna M., Mireault, Christopher R., Kobayashi, Takeshi, Pruski, Marek, & Schurko, Robert W. Natural abundance 14N and 15N solid-state NMR of pharmaceuticals and their polymorphs. United States. https://doi.org/10.1039/C6CP02855A
Veinberg, Stanislav L., Johnston, Karen E., Jaroszewicz, Michael J., Kispal, Brianna M., Mireault, Christopher R., Kobayashi, Takeshi, Pruski, Marek, and Schurko, Robert W. 2016.
"Natural abundance 14N and 15N solid-state NMR of pharmaceuticals and their polymorphs". United States. https://doi.org/10.1039/C6CP02855A. https://www.osti.gov/servlets/purl/1278752.
@article{osti_1278752,
title = {Natural abundance 14N and 15N solid-state NMR of pharmaceuticals and their polymorphs},
author = {Veinberg, Stanislav L. and Johnston, Karen E. and Jaroszewicz, Michael J. and Kispal, Brianna M. and Mireault, Christopher R. and Kobayashi, Takeshi and Pruski, Marek and Schurko, Robert W.},
abstractNote = {14N ultra-wideline (UW), 1H{15N} indirectly-detected HETCOR (idHETCOR) and 15N dynamic nuclear polarization (DNP) solid-state NMR (SSNMR) experiments, in combination with plane-wave density functional theory (DFT) calculations of 14N EFG tensors, were utilized to characterize a series of nitrogen-containing active pharmaceutical ingredients (APIs), including HCl salts of scopolamine, alprenolol, isoprenaline, acebutolol, dibucaine, nicardipine, and ranitidine. Here, a case study applying these methods for the differentiation of polymorphs of bupivacaine HCl is also presented. All experiments were conducted upon samples with naturally-abundant nitrogen isotopes. For most of the APIs, it was possible to acquire frequency-stepped UW 14N SSNMR spectra of stationary samples, which display powder patterns corresponding to pseudo-tetrahedral (i.e., RR'R"NH+ and RR'NH2+) or other (i.e., RNH2 and RNO2) nitrogen environments.},
doi = {10.1039/C6CP02855A},
url = {https://www.osti.gov/biblio/1278752},
journal = {Physical Chemistry Chemical Physics. PCCP},
issn = {1463-9076},
number = 26,
volume = 18,
place = {United States},
year = {Wed Jun 08 00:00:00 EDT 2016},
month = {Wed Jun 08 00:00:00 EDT 2016}
}
Web of Science
Works referenced in this record:
Solid‐State NMR Studies of Pharmaceutical Systems
journal, March 2008
- Geppi, Marco; Mollica, Giulia; Borsacchi, Silvia
- Applied Spectroscopy Reviews, Vol. 43, Issue 3
Characterisation of salts of drug substances
journal, January 2003
- Giron, D.
- Journal of Thermal Analysis and Calorimetry, Vol. 73, Issue 2, p. 441-457
Solid-State Pharmaceutical Chemistry
journal, August 1994
- Byrn, S. R.; Pfeiffer, R. R.; Stephenson, G.
- Chemistry of Materials, Vol. 6, Issue 8
Investigations of Polymorphism and Pseudo-polymorphism in Pharmaceuticals by Combined Thermoanalytical Techniques
journal, January 2001
- Giron, D.
- Journal of Thermal Analysis and Calorimetry, Vol. 64, Issue 1, p. 37-60
Pharmaceutical Applications of Polymorphism
journal, August 1969
- Haleblian, John; McCrone, Walter
- Journal of Pharmaceutical Sciences, Vol. 58, Issue 8
Polymorphism of Active Pharmaceutical Ingredients
journal, February 2006
- Karpinski, P. H.
- Chemical Engineering & Technology, Vol. 29, Issue 2
A new method for the reproducible generation of polymorphs: two forms of sulindac with very different solubilities
journal, March 2007
- Llinàs, Antonio; Box, Karl J.; Burley, Jonathan C.
- Journal of Applied Crystallography, Vol. 40, Issue 2
NMR studies of organic polymorphs & solvates
journal, January 2006
- Harris, Robin K.
- The Analyst, Vol. 131, Issue 3
Applications of solid-state NMR to pharmaceutical polymorphism and related matters*
journal, February 2007
- Harris, Robin K.
- Journal of Pharmacy and Pharmacology, Vol. 59, Issue 2
Molecular Architecture of Nanocapsules, Bilayer-Enclosed Solid Particles of Cisplatin
journal, October 2004
- Chupin, Vladimir; de Kroon, Anton I. P. M.; de Kruijff, Ben
- Journal of the American Chemical Society, Vol. 126, Issue 42
Distinguishing Anhydrous and Hydrous Forms of an Active Pharmaceutical Ingredient in a Tablet Formulation Using Solid-State NMR Spectroscopy
journal, October 2007
- Griffin, John M.; Martin, Dave R.; Brown, Steven P.
- Angewandte Chemie International Edition, Vol. 46, Issue 42
Solid-State Acid−Base Interactions in Complexes of Heterocyclic Bases with Dicarboxylic Acids: Crystallography, Hydrogen Bond Analysis, and 15 N NMR Spectroscopy
journal, June 2006
- Li, Z. Jane; Abramov, Yuriy; Bordner, Jon
- Journal of the American Chemical Society, Vol. 128, Issue 25
The Determination of the Crystal Structure of Anhydrous Theophylline by X-ray Powder Diffraction with a Systematic Search Algorithm, Lattice Energy Calculations, and 13 C and 15 N Solid-State NMR: A Question of Polymorphism in a Given Unit Cell
journal, June 2001
- Smith, Elaine D. L.; Hammond, Robert B.; Jones, Matthew J.
- The Journal of Physical Chemistry B, Vol. 105, Issue 24
Physical, Crystallographic, and Spectroscopic Characterization of a Crystalline Pharmaceutical Hydrate: Understanding the Role of Water
journal, October 2006
- Vogt, Frederick G.; Brum, Jeffrey; Katrincic, Lee M.
- Crystal Growth & Design, Vol. 6, Issue 10
1H, 13C, 15N NMR analysis of sildenafil base and citrate (Viagra) in solution, solid state and pharmaceutical dosage forms
journal, August 2005
- Wawer, Iwona; Pisklak, Maciej; Chilmonczyk, Zdzisław
- Journal of Pharmaceutical and Biomedical Analysis, Vol. 38, Issue 5
19 F Solid-State NMR Spectroscopic Investigation of Crystalline and Amorphous Forms of a Selective Muscarinic M 3 Receptor Antagonist, in Both Bulk and Pharmaceutical Dosage Form Samples
journal, January 2002
- Wenslow, Robert M.
- Drug Development and Industrial Pharmacy, Vol. 28, Issue 5
17 O Solid-State NMR as a Sensitive Probe of Hydrogen Bonding in Crystalline and Amorphous Solid Forms of Diflunisal
journal, July 2013
- Vogt, Frederick G.; Yin, Hao; Forcino, Rachel G.
- Molecular Pharmaceutics, Vol. 10, Issue 9
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
Solid-State NMR Analysis of a Complex Crystalline Phase of Ronacaleret Hydrochloride
journal, August 2014
- Vogt, Frederick G.; Williams, Glenn R.; Strohmeier, Mark
- The Journal of Physical Chemistry B, Vol. 118, Issue 34
23 Na magic-angle spinning and double-rotation NMR study of solid forms of sodium valproate
journal, January 2014
- Dicaire, Nuiok M.; Perras, Frédéric A.; Bryce, David L.
- Canadian Journal of Chemistry, Vol. 92, Issue 1
Solid-State 17 O NMR of Pharmaceutical Compounds: Salicylic Acid and Aspirin
journal, August 2013
- Kong, Xianqi; Shan, Melissa; Terskikh, Victor
- The Journal of Physical Chemistry B, Vol. 117, Issue 33
13 C and 15 N CP/MAS, 1 H- 15 N SCT CP/MAS and FTIR spectroscopy as tools for qualitative detection of the presence of zwitterionic and non-ionic forms of ansa -macrolide 3-formylrifamycin SV and its derivatives in solid state
journal, November 2013
- Przybylski, Piotr; Pyta, Krystian; Klich, Katarzyna
- Magnetic Resonance in Chemistry, Vol. 52, Issue 1-2
Solid-state NMR in the analysis of drugs and naturally occurring materials
journal, May 2014
- Paradowska, Katarzyna; Wawer, Iwona
- Journal of Pharmaceutical and Biomedical Analysis, Vol. 93
A study of variable hydration states in topotecan hydrochloride
journal, March 2006
- Vogt, Frederick G.; Dell’Orco, Philip C.; Diederich, Ann. M.
- Journal of Pharmaceutical and Biomedical Analysis, Vol. 40, Issue 5
Solid-state NMR and IR for the analysis of pharmaceutical solids: Polymorphs of fosinopril sodium
journal, January 1993
- Brittain, Harry G.; Morris, Kenneth R.; Bugay, David E.
- Journal of Pharmaceutical and Biomedical Analysis, Vol. 11, Issue 11-12
Sodium-23 Ssolid-Sstate Snuclear Smagnetic Sresonance of Scommercial Ssodium Snaproxen and its Ssolvates
journal, August 2012
- Burgess, Kevin M. N.; Perras, Frédéric A.; Lebrun, Aurore
- Journal of Pharmaceutical Sciences, Vol. 101, Issue 8
Solid-State NMR Analysis of a Boron-Containing Pharmaceutical Hydrochloride Salt
journal, October 2013
- Vogt, Frederick G.; Williams, Glenn R.; Copley, Royston C. B.
- Journal of Pharmaceutical Sciences, Vol. 102, Issue 10
Conformational Isomerism in Solid State of AMG 853—Structure Studies Using Solid-State Nuclear Magnetic Resonance and X-ray Diffraction
journal, July 2015
- Kiang, Y. -H.; Nagapudi, Karthik; Wu, Tian
- Journal of Pharmaceutical Sciences, Vol. 104, Issue 7
Quantification of compaction-induced crystallinity reduction of a pharmaceutical solid using 19 F solid-state NMR and powder X-ray diffraction
journal, May 2009
- Liu, Jodi; Nagapudi, Karthik; Kiang, Y. -H.
- Drug Development and Industrial Pharmacy, Vol. 35, Issue 8
Characterization of Two Distinct Amorphous Forms of Valsartan by Solid-State NMR
journal, December 2015
- Skotnicki, Marcin; Apperley, David C.; Aguilar, Juan A.
- Molecular Pharmaceutics, Vol. 13, Issue 1
A Solid-State NMR Study of Amorphous Ezetimibe Dispersions in Mesoporous Silica
journal, June 2013
- Vogt, Frederick G.; Roberts-Skilton, Karen; Kennedy-Gabb, Sonya A.
- Pharmaceutical Research, Vol. 30, Issue 9
Application of Solid-State 35 Cl NMR to the Structural Characterization of Hydrochloride Pharmaceuticals and their Polymorphs
journal, August 2008
- Hamaed, Hiyam; Pawlowski, Jenna M.; Cooper, Benjamin F. T.
- Journal of the American Chemical Society, Vol. 130, Issue 33
35 Cl solid-state NMR of HCl salts of active pharmaceutical ingredients: structural prediction, spectral fingerprinting and polymorph recognition
journal, January 2014
- Hildebrand, Marcel; Hamaed, Hiyam; Namespetra, Andrew M.
- CrystEngComm, Vol. 16, Issue 31
Two-dimensional proton-detected 35 Cl/ 1 H correlation solid-state NMR experiment under fast magic angle sample spinning: application to pharmaceutical compounds
journal, January 2016
- Pandey, Manoj Kumar; Kato, Hiroshi; Ishii, Yuji
- Physical Chemistry Chemical Physics, Vol. 18, Issue 8
Characterization of Pharmaceutical Compounds by Solid-state NMR
book, January 2015
- Vogt, Frederick G.
- eMagRes
Nitrogen nuclear magnetic resonance spectroscopy as a probe of bonding, bending and fluxionality of the imido ligand
journal, January 1992
- Bradley, Donald C.; Hodge, Stephen R.; Runnacles, John D.
- Journal of the Chemical Society, Dalton Transactions, Issue 10
14 N Quadrupolar, 14 N and 15 N Chemical Shift, and 14 N− 1 H Dipolar Tensors of Sulfamic Acid
journal, October 2002
- Harbison, Gerard S.; Kye, Young-Sik; Penner, Glenn H.
- The Journal of Physical Chemistry B, Vol. 106, Issue 40
Some dynamical properties of nitrogen-14 quadrupolar spin-system with non-symmetric electric field gradient tensor
journal, April 2004
- Rudakov, T. N.; Mikhaltsevitch, V. T.; Hayes, P. A.
- Chemical Physics Letters, Vol. 387, Issue 4-6
Solid-state14N MAS NMR of ammonium ions as a spy to structural insights for ammonium salts
journal, January 2006
- Jakobsen, Hans J.; Hove, Anders R.; Hazell, Rita G.
- Magnetic Resonance in Chemistry, Vol. 44, Issue 3
Nitrogen-15 chemical shift anisotropy and 1H–15N dipolar coupling tensors associated with the phenylalanine residue in the solid state
journal, August 1999
- Lee, D. K.; Santos, J. S.; Ramamoorthy, A.
- Chemical Physics Letters, Vol. 309, Issue 3-4
Effects of polymorphic differences for sulfanilamide, as seen through13C and15N solid-state NMR, together with shielding calculations
journal, February 2004
- Portieri, Alessia; Harris, Robin K.; Fletton, Richard A.
- Magnetic Resonance in Chemistry, Vol. 42, Issue 3
Signal assignments and chemical-shift structural analysis of uniformly 13 C, 15 N-labeled peptide, mastoparan-X, by multidimensional solid-state NMR under magic-angle spinning
journal, April 2004
- Fujiwara, Toshimichi; Todokoro, Yasuto; Yanagishita, Hajime
- Journal of Biomolecular NMR, Vol. 28, Issue 4
High-resolution 14N-edited 1H–13C correlation NMR experiment to study biological solids
journal, October 2008
- Amoureux, Jean-Paul; Trébosc, Julien; Hu, Bingwen
- Journal of Magnetic Resonance, Vol. 194, Issue 2
Probing amide bond nitrogens in solids using 14N NMR spectroscopy
journal, May 2008
- Antonijevic, Sasa; Halpern-Manners, Nicholas
- Solid State Nuclear Magnetic Resonance, Vol. 33, Issue 4
Indirectly detected heteronuclear correlation solid-state NMR spectroscopy of naturally abundant 15N nuclei
journal, February 2014
- Althaus, Stacey M.; Mao, Kanmi; Stringer, John A.
- Solid State Nuclear Magnetic Resonance, Vol. 57-58
Nitrogen-15 Chemical Shift Tensors and Conformation of Poly(β-benzyl l -aspartate) in the Solid State by NMR
journal, April 1999
- Ashikawa, Mikiya; Shoji, Akira; Ozaki, Takuo
- Macromolecules, Vol. 32, Issue 7
A solid-state 14N magic-angle spinning NMR study of some amino acids
journal, February 2004
- Giavani, Tania; Bildsøe, Henrik; Skibsted, Jørgen
- Journal of Magnetic Resonance, Vol. 166, Issue 2
A Study on the Intermolecular Hydrogen Bonds of α-Glycylglycine in Its Actual Crystalline Phase Using ab Initio Calculated 14 N and 2 H Nuclear Quadrupole Coupling Constants
journal, March 2005
- Elmi, Fatemeh; Hadipour, Nasser L.
- The Journal of Physical Chemistry A, Vol. 109, Issue 8
Static solid-state 14N NMR and computational studies of nitrogen EFG tensors in some crystalline amino acids
journal, January 2009
- O’Dell, Luke A.; Schurko, Robert W.
- Physical Chemistry Chemical Physics, Vol. 11, Issue 32
Interaction Tensors and Local Dynamics in Common Structural Motifs of Nitrogen: A Solid-State 14 N NMR and DFT Study
journal, January 2011
- O’Dell, Luke A.; Schurko, Robert W.; Harris, Kristopher J.
- Journal of the American Chemical Society, Vol. 133, Issue 3
Multinuclear Solid-State Nuclear Magnetic Resonance and Density Functional Theory Characterization of Interaction Tensors in Taurine
journal, January 2012
- O’Dell, Luke A.; Ratcliffe, Christopher I.; Kong, Xianqi
- The Journal of Physical Chemistry A, Vol. 116, Issue 3
Density functional theory study of nitrogen-14 nuclear quadrupole coupling parameters of L-histidine: hydrogen-bonded system: Nitrogen-14 NQR parameters of L-his
journal, March 2012
- Elmi, Maryam Mitra; Kaykhaei, Abbas Ali; Elmi, Fatemeh
- Magnetic Resonance in Chemistry, Vol. 50, Issue 4
Probing intermolecular interactions and nitrogen protonation in pharmaceuticals by novel 15N-edited and 2D 14N-1H solid-state NMR
journal, January 2012
- Tatton, Andrew S.; Pham, Tran N.; Vogt, Frederick G.
- CrystEngComm, Vol. 14, Issue 8
Probing Hydrogen Bonding in Cocrystals and Amorphous Dispersions Using 14 N– 1 H HMQC Solid-State NMR
journal, February 2013
- Tatton, Andrew S.; Pham, Tran N.; Vogt, Frederick G.
- Molecular Pharmaceutics, Vol. 10, Issue 3
Dynamic nuclear polarisation enhanced 14 N overtone MAS NMR spectroscopy
journal, January 2014
- Rossini, Aaron J.; Emsley, Lyndon; O'Dell, Luke A.
- Phys. Chem. Chem. Phys., Vol. 16, Issue 25
Rapid Acquisition of 14 N Solid-State NMR Spectra with Broadband Cross Polarization
journal, October 2013
- Harris, Kristopher J.; Veinberg, Stanislav L.; Mireault, Christopher R.
- Chemistry - A European Journal, Vol. 19, Issue 48
Investigating Albendazole Desmotropes by Solid-State NMR Spectroscopy
journal, January 2015
- Chattah, Ana K.; Zhang, Rongchun; Mroue, Kamal H.
- Molecular Pharmaceutics, Vol. 12, Issue 3
Analysis of Conformational Polymorphism in Pharmaceutical Solids Using Solid-State NMR and Electronic Structure Calculations
journal, April 2006
- Smith, Jay R.; Xu, Weizong; Raftery, Daniel
- The Journal of Physical Chemistry B, Vol. 110, Issue 15
Investigation of Drug–Excipient Interactions in Lapatinib Amorphous Solid Dispersions Using Solid-State NMR Spectroscopy
journal, January 2015
- Song, Yang; Yang, Xinghao; Chen, Xin
- Molecular Pharmaceutics, Vol. 12, Issue 3
Potential of Nuclear Quadrupole Resonance in Pharmaceutical Analysis
journal, July 2005
- Balchin, Elizabeth; Malcolme-Lawes, David J.; Poplett, Iain J. F.
- Analytical Chemistry, Vol. 77, Issue 13
Nitrogen-14 Nuclear Quadrupole Resonance Spectroscopy: A Promising Analytical Methodology for Medicines Authentication and Counterfeit Antimalarial Analysis
journal, February 2013
- Barras, Jamie; Murnane, Darragh; Althoefer, Kaspar
- Analytical Chemistry, Vol. 85, Issue 5
Application of 14N NQR to the Study of Piroxicam Polymorphism
journal, December 2010
- Lavric, Zoran; Pirnat, Janez; Luznik, Janko
- Journal of Pharmaceutical Sciences, Vol. 99, Issue 12
Nuclear quadrupole resonance of norephedrine
journal, October 2011
- Shinohara, Junichiro; Kobayashi, Kazuhiko; Sato-Akaba, Hideo
- Solid State Nuclear Magnetic Resonance, Vol. 40, Issue 3
WURST–QCPMG sequence and “spin-lock” in 14N nuclear quadrupole resonance
journal, August 2013
- Gregorovič, Alan; Apih, Tomaž
- Journal of Magnetic Resonance, Vol. 233
An Insight into Prototropism and Supramolecular Motifs in Solid-State Structures of Allopurinol, Hypoxanthine, Xanthine, and Uric Acid. A 1 H– 14 N NQDR Spectroscopy, Hybrid DFT/QTAIM, and Hirshfeld Surface-Based Study
journal, August 2014
- Latosińska, Jolanta Natalia; Latosińska, Magdalena; Seliger, Janez
- The Journal of Physical Chemistry B, Vol. 118, Issue 37
Direct detection of nitrogen-14 in solid-state NMR spectroscopy
journal, November 2011
- O’Dell, Luke A.
- Progress in Nuclear Magnetic Resonance Spectroscopy, Vol. 59, Issue 4
Probing Crystal Structures and Transformation Reactions of Ammonium Molybdates by 14 N MAS NMR Spectroscopy
journal, December 2006
- Hove, Anders R.; Bildsøe, Henrik; Skibsted, Jørgen
- Inorganic Chemistry, Vol. 45, Issue 26
Long-term stability of rotor-controlled MAS frequencies to 0.1Hz proved by 14N MAS NMR experiments and simulations
journal, March 2007
- Jakobsen, Hans J.; Hove, Anders R.; Bildsøe, Henrik
- Journal of Magnetic Resonance, Vol. 185, Issue 1
Overtone NMR spectroscopy
journal, February 1987
- Tycko, R.; Opella, S. J.
- The Journal of Chemical Physics, Vol. 86, Issue 4
14N magic angle spinning overtone NMR spectra
journal, September 2011
- O’Dell, Luke A.; Ratcliffe, Christopher I.
- Chemical Physics Letters, Vol. 514, Issue 1-3
14 N overtone NMR spectra under magic angle spinning: Experiments and numerically exact simulations
journal, February 2013
- O’Dell, Luke A.; Brinkmann, Andreas
- The Journal of Chemical Physics, Vol. 138, Issue 6
Proton–nitrogen-14 overtone two-dimensional correlation NMR spectroscopy of solid-sample at very fast magic angle sample spinning
journal, May 2013
- Nishiyama, Yusuke; Malon, Michal; Gan, Zhehong
- Journal of Magnetic Resonance, Vol. 230
Solid-state nitrogen-14 nuclear magnetic resonance enhanced by dynamic nuclear polarization using a gyrotron
journal, July 2010
- Vitzthum, Veronika; Caporini, Marc A.; Bodenhausen, Geoffrey
- Journal of Magnetic Resonance, Vol. 205, Issue 1
Indirect detection of nitrogen-14 in solids via protons by nuclear magnetic resonance spectroscopy
journal, September 2006
- Cavadini, Simone; Antonijevic, Sasa; Lupulescu, Adonis
- Journal of Magnetic Resonance, Vol. 182, Issue 1
Indirect Detection of Nitrogen-14 in Solid-State NMR Spectroscopy
journal, June 2007
- Cavadini, Simone; Antonijevic, Sasa; Lupulescu, Adonis
- ChemPhysChem, Vol. 8, Issue 9
Line-narrowing in proton-detected nitrogen-14 NMR
journal, January 2010
- Cavadini, Simone; Vitzthum, Veronika; Ulzega, Simone
- Journal of Magnetic Resonance, Vol. 202, Issue 1
New Tools in Bio-NMR: Indirect Detection of Nitrogen-14 in Solids
journal, March 2010
- Ulzega, Simone
- CHIMIA International Journal for Chemistry, Vol. 64, Issue 3
Proton-detected 14N MAS NMR using homonuclear decoupled rotary resonance
journal, February 2007
- Gan, Zhehong; Amoureux, Jean Paul; Trébosc, Julien
- Chemical Physics Letters, Vol. 435, Issue 1-3
Indirect detection of nitrogen-14 in solid-state NMR spectroscopy
journal, January 2010
- Cavadini, Simone
- Progress in Nuclear Magnetic Resonance Spectroscopy, Vol. 56, Issue 1
QCPMG using adiabatic pulses for faster acquisition of ultra-wideline NMR spectra
journal, October 2008
- O’Dell, Luke A.; Schurko, Robert W.
- Chemical Physics Letters, Vol. 464, Issue 1-3
Acquisition of ultra-wideline NMR spectra from quadrupolar nuclei by frequency stepped WURST–QCPMG
journal, January 2009
- O’Dell, Luke A.; Rossini, Aaron J.; Schurko, Robert W.
- Chemical Physics Letters, Vol. 468, Issue 4-6
Fast and Simple Acquisition of Solid-State 14 N NMR Spectra with Signal Enhancement via Population Transfer
journal, May 2009
- O’Dell, Luke A.; Schurko, Robert W.
- Journal of the American Chemical Society, Vol. 131, Issue 19
Ultra-wideline 14N NMR spectroscopy as a probe of molecular dynamics
journal, January 2010
- O'Dell, Luke A.; Ratcliffe, Christopher I.
- Chemical Communications, Vol. 46, Issue 36
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
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
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
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
New methods for the acquisition of ultra-wideline solid-state NMR spectra of spin-1/2 nuclides
journal, January 2011
- MacGregor, Alan W.; O’Dell, Luke A.; Schurko, Robert W.
- Journal of Magnetic Resonance, Vol. 208, Issue 1
Multinuclear solid-state NMR of square-planar platinum complexes — Cisplatin and related systems
journal, July 2011
- Lucier, Bryan E. G.; Reidel, Alex R.; Schurko, Robert W.
- Canadian Journal of Chemistry, Vol. 89, Issue 7
Unravelling the Structure of Magnus’ Pink Salt
journal, January 2014
- Lucier, Bryan E. G.; Johnston, Karen E.; Xu, Wenqian
- Journal of the American Chemical Society, Vol. 136, Issue 4
New Insights into the Short-Range Structures of Microporous Titanosilicates As Revealed by 47/49 Ti, 23 Na, 39 K, and 29 Si Solid-State NMR Spectroscopy
journal, November 2014
- Xu, Jun; Lucier, Bryan E. G.; Lin, Zhi
- The Journal of Physical Chemistry C, Vol. 118, Issue 47
A Study of Transition-Metal Organometallic Complexes Combining 35 Cl Solid-State NMR Spectroscopy and 35 Cl NQR Spectroscopy and First-Principles DFT Calculations
journal, August 2013
- Johnston, Karen E.; O'Keefe, Christopher A.; Gauvin, Régis M.
- Chemistry - A European Journal, Vol. 19, Issue 37
An Investigation of Chlorine Ligands in Transition-Metal Complexes via 35 Cl Solid-State NMR and Density Functional Theory Calculations
journal, August 2014
- O’Keefe, Christopher A.; Johnston, Karen E.; Sutter, Kiplangat
- Inorganic Chemistry, Vol. 53, Issue 18
Multinuclear Solid-State Magnetic Resonance and X-ray Diffraction Study of Some Thiocyanate and Selenocyanate Complexes Exhibiting Halogen Bonding
journal, November 2011
- Viger-Gravel, Jasmine; Korobkov, Ilia; Bryce, David L.
- Crystal Growth & Design, Vol. 11, Issue 11
Feasibility of arsenic and antimony NMR spectroscopy in solids: An investigation of some group 15 compounds
journal, July 2014
- Faucher, Alexandra; Terskikh, Victor V.; Wasylishen, Roderick E.
- Solid State Nuclear Magnetic Resonance, Vol. 61-62
Solid-State 63 Cu, 65 Cu, and 31 P NMR Spectroscopy of Photoluminescent Copper(I) Triazole Phosphine Complexes
journal, July 2015
- Yu, Huaguang; Tan, Xiuzhen; Bernard, Guy M.
- The Journal of Physical Chemistry A, Vol. 119, Issue 30
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
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
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
Indirectly detected through-bond chemical shift correlation NMR spectroscopy in solids under fast MAS: Studies of organic–inorganic hybrid materials
journal, January 2009
- Mao, Kanmi; Wiench, Jerzy W.; Lin, Victor S. -Y.
- Journal of Magnetic Resonance, Vol. 196, Issue 1
Sensitive High Resolution Inverse Detection NMR Spectroscopy of Proteins in the Solid State
journal, November 2003
- Paulson, Eric K.; Morcombe, Corey R.; Gaponenko, Vadim
- Journal of the American Chemical Society, Vol. 125, Issue 51
Study of the thermal processes in molecular crystals of peptides by means of NMR crystallography
journal, January 2013
- Pawlak, Tomasz; Paluch, Piotr; Trzeciak-Karlikowska, Katarzyna
- CrystEngComm, Vol. 15, Issue 43
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
Molecular ordering of mixed surfactants in mesoporous silicas: A solid-state NMR study
journal, May 2011
- Kobayashi, Takeshi; Mao, Kanmi; Wang, Shy-Guey
- Solid State Nuclear Magnetic Resonance, Vol. 39, Issue 3-4
Adiabatic passage Hartmann-Hahn cross polarization in NMR under magic angle sample spinning
journal, July 1995
- Hediger, S.; Meier, B. H.; Ernst, R. R.
- Chemical Physics Letters, Vol. 240, Issue 5-6
Directly and indirectly detected through-bond heteronuclear correlation solid-state NMR spectroscopy under fast MAS
journal, December 2009
- Mao, Kanmi; Pruski, Marek
- Journal of Magnetic Resonance, Vol. 201, Issue 2
Polarization of Nuclei in Metals
journal, October 1953
- Overhauser, Albert W.
- Physical Review, Vol. 92, Issue 2
Polarization of Nuclear Spins in Metals
journal, October 1953
- Carver, T. R.; Slichter, C. P.
- Physical Review, Vol. 92, Issue 1
Operational characteristics of a 14-W 140-GHz gyrotron for dynamic nuclear polarization
journal, June 2006
- Joye, C. D.; Griffin, R. G.; Hornstein, M. K.
- IEEE Transactions on Plasma Science, Vol. 34, Issue 3
Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization
journal, June 2009
- Barnes, Alexander B.; Mak-Jurkauskas, Melody L.; Matsuki, Yoh
- Journal of Magnetic Resonance, Vol. 198, Issue 2
TOTAPOL: A Biradical Polarizing Agent for Dynamic Nuclear Polarization Experiments in Aqueous Media
journal, September 2006
- Song, Changsik; Hu, Kan-Nian; Joo, Chan-Gyu
- Journal of the American Chemical Society, Vol. 128, Issue 35
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
Dynamic nuclear polarization at high magnetic fields
journal, February 2008
- Maly, Thorsten; Debelouchina, Galia T.; Bajaj, Vikram S.
- The Journal of Chemical Physics, Vol. 128, Issue 5
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
Rapid Natural-Abundance 2D 13 C- 13 C Correlation Spectroscopy Using Dynamic Nuclear Polarization Enhanced Solid-State NMR and Matrix-Free Sample Preparation
journal, October 2012
- Takahashi, Hiroki; Lee, Daniel; Dubois, Lionel
- Angewandte Chemie International Edition, Vol. 51, Issue 47
Natural Abundance 17 O DNP Two-Dimensional and Surface-Enhanced NMR Spectroscopy
journal, June 2015
- Perras, Frédéric A.; Kobayashi, Takeshi; Pruski, Marek
- Journal of the American Chemical Society, Vol. 137, Issue 26
A Slowly Relaxing Rigid Biradical for Efficient Dynamic Nuclear Polarization Surface-Enhanced NMR Spectroscopy: Expeditious Characterization of Functional Group Manipulation in Hybrid Materials
journal, January 2012
- Zagdoun, Alexandre; Casano, Gilles; Ouari, Olivier
- Journal of the American Chemical Society, Vol. 134, Issue 4
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
Mechanism of Solid-State Thermolysis of Ammonia Borane: A 15 N NMR Study Using Fast Magic-Angle Spinning and Dynamic Nuclear Polarization
journal, August 2014
- Kobayashi, Takeshi; Gupta, Shalabh; Caporini, Marc A.
- The Journal of Physical Chemistry C, Vol. 118, Issue 34
Structures and absolute configurations of enantiomers of two local anaesthetics: (2S)-1-methyl- and (2R)-1-butyl-2',6'-pipecoloxylidide hydrochlorides
journal, October 1992
- Csöregh, I.
- Acta Crystallographica Section C Crystal Structure Communications, Vol. 48, Issue 10
The solid-state structures of (-)-scopolamine free base, (-)-scopolamine methobromide, (-)-scopolamine hydrobromide trihydrate, and of the pseudopolymorphic forms of (-)-scopolamine hydrochloride anhydrate and 1.66hydrate
journal, February 2000
- Glaser, Robert; Shiftan, Dror; Drouin, Marc
- Canadian Journal of Chemistry, Vol. 78, Issue 2
Conformations cristallines d'adrénolytiques β-bloquants: propranolol et alprénolol
journal, June 1973
- Barrans, Y.; Cotrait, M.; Dangoumau, J.
- Acta Crystallographica Section B Structural Crystallography and Crystal Chemistry, Vol. 29, Issue 6
Crystal Structures and Molecular Conformations of Isoprenaline Hydrochloride and ( S )-Isoprenaline Hydrogen (2 R ,3 R )-Tartrate
journal, October 1993
- Kingsford-Adaboh, Robert; Hayashi, Eiichi; Haisa, Masao
- Bulletin of the Chemical Society of Japan, Vol. 66, Issue 10
Chlorhydrate d'acébutolol [(hydroxy-2 isopropylamino-3 propoxy)-2 butyrylamino-5 acétophénone chlorhydraté]
journal, January 1979
- Carpy, A.; Gadret, M.; Hickel, D.
- Acta Crystallographica Section B Structural Crystallography and Crystal Chemistry, Vol. 35, Issue 1
Crystal structures of two local anesthetics: Dibucaine�HCl�H2O and Dimethisoquin�HCl�H2O
journal, December 1977
- Hayward, Barbara Sindel; Donohue, Jerry
- Journal of Crystal and Molecular Structure, Vol. 7, Issue 6
Polymorphs and Solvates of Nicardipine Hydrochloride. Selective Stabilization of Different Diastereomeric Racemates
journal, January 2011
- Moreno-Calvo, Evelyn; Muntó, María; Wurst, Klaus
- Molecular Pharmaceutics, Vol. 8, Issue 2
Structure of ranitidine hydrochloride
journal, October 1990
- Ishida, T.; In, Y.; Inoue, M.
- Acta Crystallographica Section C Crystal Structure Communications, Vol. 46, Issue 10
Ultra-wideline27Al NMR Investigation of Three- and Five-Coordinate Aluminum Environments
journal, January 2006
- Tang, Joel A.; Masuda, Jason D.; Boyle, Timothy J.
- ChemPhysChem, Vol. 7, Issue 1
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
Rotary resonance recoupling of dipolar interactions in solid‐state nuclear magnetic resonance spectroscopy
journal, July 1988
- Oas, T. G.; Griffin, R. G.; Levitt, M. H.
- The Journal of Chemical Physics, Vol. 89, Issue 2
Further conventions for NMR shielding and chemical shifts (IUPAC Recommendations 2008)
journal, January 2008
- Harris, Robin K.; Becker, Edwin D.; Cabral de Menezes, Sonia M.
- Pure and Applied Chemistry, Vol. 80, Issue 1
All-electron magnetic response with pseudopotentials: NMR chemical shifts
journal, May 2001
- Pickard, Chris J.; Mauri, Francesco
- Physical Review B, Vol. 63, Issue 24
Quadrupolar effects transferred to spin-12 magic-angle spinning spectra of solids
journal, January 1992
- Harris, Robin K.; Olivieri, Alejandro C.
- Progress in Nuclear Magnetic Resonance Spectroscopy, Vol. 24, Issue 5
Magnetic resonance tensors in Uracil: Calculation of 13C, 15N, 17O NMR chemical shifts, 17O and 14N electric field gradients and measurement of 13C and 15N chemical shifts
journal, February 2010
- Amini, Saeed K.; Shaghaghi, Hoora; Bain, Alex D.
- Solid State Nuclear Magnetic Resonance, Vol. 37, Issue 1-2
Photo-oxidation of Atmospheric SO2
journal, February 1971
- Cox, R. A.; Penkett, S. A.
- Nature, Vol. 229, Issue 5285
Microwave spectrum and structure of nitromethane
journal, January 1972
- Cox, A. Peter; Waring, Stephen
- Journal of the Chemical Society, Faraday Transactions 2, Vol. 68
Nitrogen-14 nuclear quadrupole resonance study of substituted nitrobenzenes
journal, January 1999
- Subbarao, S. N.
- The Journal of Chemical Physics, Vol. 67, Issue 9
Residual (13C,14N) dipolar coupling in13C NMR of solid nitrogen-containing aromatic compounds
journal, July 1985
- Harris, R. K.; Jonsen, P.; Packer, K. J.
- Magnetic Resonance in Chemistry, Vol. 23, Issue 7
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
Rapid measurement of multidimensional 1H solid-state NMR spectra at ultra-fast MAS frequencies
journal, February 2014
- Ye, Yue Qi; Malon, Michal; Martineau, Charlotte
- Journal of Magnetic Resonance, Vol. 239
Studies of minute quantities of natural abundance molecules using 2D heteronuclear correlation spectroscopy under 100 kHz MAS
journal, April 2015
- Nishiyama, Y.; Kobayashi, T.; Malon, M.
- Solid State Nuclear Magnetic Resonance, Vol. 66-67
Powder crystallography of pharmaceutical materials by combined crystal structure prediction and solid-state 1H NMR spectroscopy
journal, January 2013
- Baias, Maria; Widdifield, Cory M.; Dumez, Jean-Nicolas
- Physical Chemistry Chemical Physics, Vol. 15, Issue 21
Energetics of hydrogen/lithium complexes in silicon analyzed using the Maxwell construction
journal, December 2011
- Morris, Andrew J.; Grey, C. P.; Needs, R. J.
- Physical Review B, Vol. 84, Issue 22
A molecular dynamics study of the effects of fast molecular motions on solid-state NMR parameters
journal, January 2013
- Dračínský, Martin; Hodgkinson, Paul
- CrystEngComm, Vol. 15, Issue 43
Predicting solid compounds via global exploration of the energy landscape of solids on the ab initio level without recourse to experimental information
journal, January 2010
- Schön, J. Christian; Doll, Klaus; Jansen, Martin
- physica status solidi (b), Vol. 247, Issue 1
Distinguishing Anhydrous and Hydrous Forms of an Active Pharmaceutical Ingredient in a Tablet Formulation Using Solid-State NMR Spectroscopy
journal, October 2007
- Griffin, John M.; Martin, Dave R.; Brown, Steven P.
- Angewandte Chemie, Vol. 119, Issue 42
Applications of Solid-State NMR to Pharmaceutical Polymorphism and Related Matters
journal, July 2007
- Harris, Robin K.
- ChemInform, Vol. 38, Issue 27
The solid-state structures of (-)-scopolamine free base, (-)-scopolamine methobromide, (-)-scopolamine hydrobromide trihydrate, and of the pseudopolymorphic forms of (-)-scopolamine hydrochloride anhydrate and 1.66hydrate
journal, January 2000
- Glaser, Robert; Shiftan, Dror; Drouin, Marc
- Canadian Journal of Chemistry, Vol. 78, Issue 2
Further Conventions for NMR Shielding and Chemical Shifts (IUPAC Recommendations 2008)
journal, January 2008
- Harris, Robin K.; Becker, Edwin D.; Cabral de Menezes, Sonia M.
- Chemistry International -- Newsmagazine for IUPAC, Vol. 30, Issue 3
Rapid Natural-Abundance 2D 13 C- 13 C Correlation Spectroscopy Using Dynamic Nuclear Polarization Enhanced Solid-State NMR and Matrix-Free Sample Preparation
journal, October 2012
- Takahashi, Hiroki; Lee, Daniel; Dubois, Lionel
- Angewandte Chemie, Vol. 124, Issue 47
All-electron magnetic response with pseudopotentials: NMR chemical shifts
text, January 2001
- Pickard, Chris J.; Mauri, Francesco
- arXiv
Indirect detection of nitrogen-14 in solid-state NMR spectroscopy
text, January 2008
- Cavadini, Simone
- Lausanne, EPFL
Works referencing / citing this record:
Understanding Surface and Interfacial Chemistry in Functional Nanomaterials via Solid-State NMR
journal, March 2017
- Marchetti, Alessandro; Chen, Juner; Pang, Zhenfeng
- Advanced Materials, Vol. 29, Issue 14
Deracemization in a Complex Quaternary System with a Second‐Order Asymmetric Transformation by Using Phase Diagram Studies
journal, October 2012
- Oketani, Ryusei; Marin, Francesco; Tinnemans, Paul
- Chemistry – A European Journal, Vol. 25, Issue 61
Deracemization in a Complex Quaternary System with a Second‐Order Asymmetric Transformation by Using Phase Diagram Studies
journal, October 2012
- Oketani, Ryusei; Marin, Francesco; Tinnemans, Paul
- Chemistry – A European Journal, Vol. 25, Issue 61
14 N Solid-State NMR Spectroscopy of Amino Acids
journal, October 2016
- Veinberg, Stanislav L.; Friedl, Zachary W.; Lindquist, Austin W.
- ChemPhysChem, Vol. 17, Issue 23
Tuning nuclear depolarization under MAS by electron T 1e
journal, January 2018
- Lund, Alicia; Equbal, Asif; Han, Songi
- Physical Chemistry Chemical Physics, Vol. 20, Issue 37
14 N overtone nuclear magnetic resonance of rotating solids
journal, August 2018
- Gan, Zhehong; Hung, Ivan; Nishiyama, Yusuke
- The Journal of Chemical Physics, Vol. 149, Issue 6