Related ArticlesA Magic-Angle Spinning NMR Method for the Site-Specific Measurement of Proton Chemical-Shift Anisotropy in Biological and Organic Solids.
Isr J Chem. 2014 Feb 1;54(1-2):171-183
Authors: Hou G, Gupta R, Polenova T, Vega AJ
Abstract
Proton chemical shifts are a rich probe of structure and hydrogen bonding environments in organic and biological molecules. Until recently, measurements of (1)H chemical shift tensors have been restricted to either solid systems with sparse proton sites or were based on the indirect determination of anisotropic tensor components from cross-relaxation and liquid-crystal experiments. We have introduced an MAS approach that permits site-resolved determination of CSA tensors of protons forming chemical bonds with labeled spin-1/2 nuclei in fully protonated solids with multiple sites, including organic molecules and proteins. This approach, originally introduced for the measurements of chemical shift tensors of amide protons, is based on three RN-symmetry based experiments, from which the principal components of the (1)H CS tensor can be reliably extracted by simultaneous triple fit of the data. In this article, we expand our approach to a much more challenging system involving aliphatic and aromatic protons. We start with a review of the prior work on experimental-NMR and computational-quantum-chemical approaches for the measurements of (1)H chemical shift tensors and for relating these to the electronic structures. We then present our experimental results on U-(13)C,(15)N-labeled histdine demonstrating that (1)H chemical shift tensors can be reliably determined for the (1)H(15)N and (1)H(13)C spin pairs in cationic and neutral forms of histidine. Finally, we demonstrate that the experimental (1)H(C) and (1)H(N) chemical shift tensors are in agreement with Density Functional Theory calculations, therefore establishing the usefulness of our method for characterization of structure and hydrogen bonding environment in organic and biological solids.
PMID: 25484446 [PubMed - as supplied by publisher]
[NMR paper] Multiple acquisition/multiple observation separated local field/chemical shift correlation solid-state magic angle spinning NMR spectroscopy.
Multiple acquisition/multiple observation separated local field/chemical shift correlation solid-state magic angle spinning NMR spectroscopy.
Multiple acquisition/multiple observation separated local field/chemical shift correlation solid-state magic angle spinning NMR spectroscopy.
J Magn Reson. 2014 Jun 28;245C:98-104
Authors: Das BB, Opella SJ
Abstract
Multiple acquisition spectroscopy (MACSY) experiments that enable multiple free induction decays to be recorded during individual experiments are demonstrated. In...
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07-16-2014 10:46 AM
[NMR paper] Broadband homonuclear correlation spectroscopy driven by combined R2n(v) sequences under fast magic angle spinning for NMR structural analysis of organic and biological solids.
Broadband homonuclear correlation spectroscopy driven by combined R2n(v) sequences under fast magic angle spinning for NMR structural analysis of organic and biological solids.
Related Articles Broadband homonuclear correlation spectroscopy driven by combined R2n(v) sequences under fast magic angle spinning for NMR structural analysis of organic and biological solids.
J Magn Reson. 2013 Apr 28;232C:18-30
Authors: Hou G, Yan S, Trébosc J, Amoureux JP, Polenova T
Abstract
We recently described a family of experiments for R2n(v) Driven Spin...
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05-21-2013 02:34 PM
[NMR paper] Broadband Homonuclear Correlation Spectroscopy Driven by Combined R2nv Sequences under Fast Magic Angle Spinning for NMR Structural Analysis of Organic and Biological Solids
Broadband Homonuclear Correlation Spectroscopy Driven by Combined R2nv Sequences under Fast Magic Angle Spinning for NMR Structural Analysis of Organic and Biological Solids
Publication date: Available online 28 April 2013
Source:Journal of Magnetic Resonance</br>
Author(s): Guangjin Hou , Si Yan , Julien Trebosc , Jean-Paul Amoureux , Tatyana Polenova</br>
We recently described a family of experiments for R2 n v Driven Spin Diffusion (RDSD) spectroscopy suitable for homonuclear correlation experiments under fast MAS conditions (J. Am. Chem. Soc., 133, 2011,...
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04-29-2013 06:00 AM
[NMR paper] Magic-Angle-Spinning NMR Techniques for Measuring Long-Range Distances in Biological Macromolecules.
Magic-Angle-Spinning NMR Techniques for Measuring Long-Range Distances in Biological Macromolecules.
http://www.ncbi.nlm.nih.gov/corehtml/query/egifs/http:--pubs.acs.org-images-pubmed-acspubs.jpg Related Articles Magic-Angle-Spinning NMR Techniques for Measuring Long-Range Distances in Biological Macromolecules.
Acc Chem Res. 2013 Feb 7;
Authors: Hong M, Schmidt-Rohr K
Abstract
The determination of molecular structures using solid-state NMR spectroscopy requires distance measurement through nuclear-spin dipole-dipole couplings....
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02-09-2013 12:18 AM
Multidimensional Magic Angle Spinning NMR Spectroscopy for Site-Resolved Measurement of Proton Chemical Shift Anisotropy in Biological Solids
Multidimensional Magic Angle Spinning NMR Spectroscopy for Site-Resolved Measurement of Proton Chemical Shift Anisotropy in Biological Solids
Guangjin Hou, Sivakumar Paramasivam, Si Yan, Tatyana Polenova and Alexander J. Vega
http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jacsat/0/jacsat.ahead-of-print/ja3084972/aop/images/medium/ja-2012-084972_0008.gif
Journal of the American Chemical Society
DOI: 10.1021/ja3084972
http://feeds.feedburner.com/~ff/acs/jacsat?d=yIl2AUoC8zA
http://feeds.feedburner.com/~r/acs/jacsat/~4/y3Jt7S8MwHM
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[NMR paper] Magic-angle spinning solid-state NMR spectroscopy of the beta1 immunoglobulin binding domain of protein G (GB1): 15N and 13C chemical shift assignments and conformational analysis.
Magic-angle spinning solid-state NMR spectroscopy of the beta1 immunoglobulin binding domain of protein G (GB1): 15N and 13C chemical shift assignments and conformational analysis.
Related Articles Magic-angle spinning solid-state NMR spectroscopy of the beta1 immunoglobulin binding domain of protein G (GB1): 15N and 13C chemical shift assignments and conformational analysis.
J Am Chem Soc. 2005 Sep 7;127(35):12291-305
Authors: Franks WT, Zhou DH, Wylie BJ, Money BG, Graesser DT, Frericks HL, Sahota G, Rienstra CM
Magic-angle spinning...
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12-01-2010 06:56 PM
[NMR paper] Site-specific 13C chemical shift anisotropy measurements in a uniformly 15N,13C-labeled microcrystalline protein by 3D magic-angle spinning NMR spectroscopy.
Site-specific 13C chemical shift anisotropy measurements in a uniformly 15N,13C-labeled microcrystalline protein by 3D magic-angle spinning NMR spectroscopy.
Related Articles Site-specific 13C chemical shift anisotropy measurements in a uniformly 15N,13C-labeled microcrystalline protein by 3D magic-angle spinning NMR spectroscopy.
J Am Chem Soc. 2005 Aug 31;127(34):11946-7
Authors: Wylie BJ, Franks WT, Graesser DT, Rienstra CM
In this Communication, we introduce a 3D magic-angle spinning recoupling experiment that correlates chemical shift...
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12-01-2010 06:56 PM
A device for the measurement of residual chemical shift anisotropy and residual dipol
Abstract Residual dipolar coupling (RDC) and residual chemical shift anisotropy (RCSA) report on orientational properties of a dipolar bond vector and a chemical shift anisotropy principal axis system, respectively. They can be highly complementary in the analysis of backbone structure and dynamics in proteins as RCSAs generally include a report on vectors out of a peptide plane while RDCs usually report on in-plane vectors. Both RDC and RCSA average to zero in isotropic solutions and require partial orientation in a magnetic field to become observable. While the alignment and measurement of...