Abstract Chemical shift assignment is the first step toward the structure elucidation of natural products and other chemical compounds. We propose here the use of 2D concurrent HMQC-COSY as an experiment for rapid chemical shift assignment of small molecules. This experiment provides well-dispersed 1Hâ??13C peak patterns that are distinctive for different functional groups plus 1Hâ??1H COSY connectivities that serve to identify adjacent groups. The COSY diagonal peaks, which are phased to be absorptive, resemble 1Hâ??13C HMQC cross peaks. We demonstrate the applicability of this experiment for rapidly and unambiguously establishing correlations between different functional groups through the analysis of the spectrum of a metabolite (jasmonic acid) dissolved in CDCl3. In addition, we show that the experiment can be used to assign spectra of compounds in a mixture of metabolites in D2O.
Content Type Journal Article
Pages 1-6
DOI 10.1007/s10858-011-9494-4
Authors
Kaifeng Hu, National Magnetic Resonance Facility at Madison, University of Wisconsin-Madison, Madison, WI 53706, USA
William M. Westler, National Magnetic Resonance Facility at Madison, University of Wisconsin-Madison, Madison, WI 53706, USA
John L. Markley, National Magnetic Resonance Facility at Madison, University of Wisconsin-Madison, Madison, WI 53706, USA
[CNS Yahoo group] How to add bond between protein residue and a small molecule in CNS
How to add bond between protein residue and a small molecule in CNS
Dear All, I'm stuck in a step where in i need to connect a bond an amino acid residue and a small molecule in CNS Thank you. Joseph
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nmrlearner
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08-07-2011 01:35 AM
[NMR paper] Selective chemical shift assignment of B800 and B850 bacteriochlorophylls in uniforml
Selective chemical shift assignment of B800 and B850 bacteriochlorophylls in uniformly -labeled light-harvesting complexes by solid-state NMR spectroscopy at ultra-high magnetic field.
Related Articles Selective chemical shift assignment of B800 and B850 bacteriochlorophylls in uniformly -labeled light-harvesting complexes by solid-state NMR spectroscopy at ultra-high magnetic field.
J Am Chem Soc. 2005 Mar 9;127(9):3213-9
Authors: van Gammeren AJ, Buda F, Hulsbergen FB, Kiihne S, Hollander JG, Egorova-Zachernyuk TA, Fraser NJ, Cogdell RJ, de Groot HJ
...
nmrlearner
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11-24-2010 11:14 PM
[NMR paper] Four-dimensional NMR spectroscopy of a 723-residue protein: chemical shift assignment
Four-dimensional NMR spectroscopy of a 723-residue protein: chemical shift assignments and secondary structure of malate synthase g.
Related Articles Four-dimensional NMR spectroscopy of a 723-residue protein: chemical shift assignments and secondary structure of malate synthase g.
J Am Chem Soc. 2002 Aug 28;124(34):10025-35
Authors: Tugarinov V, Muhandiram R, Ayed A, Kay LE
A four-dimensional (4-D) NMR study of Escherichia coli malate synthase G (MSG), a 723-residue monomeric enzyme (81.4 kDa), is described. Virtually complete backbone (1)HN,...
nmrlearner
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11-24-2010 08:58 PM
Small Molecule NMR Scientist (B.S./ M.S.) at Novartis Ag (Cambridge, MA)
Small Molecule NMR Scientist (B.S./ M.S.) at Novartis Ag (Cambridge, MA)
using the state-of-the-art NMR methodologies. As an NMR scientist within the team, you will be responsible for ... in small molecular NMR with demonstrated success in modern NMR methodologies. Demonstrated skills in data collection...
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08-19-2010 02:32 AM
A probabilistic approach for validating protein NMR chemical shift assignments
Abstract It has been estimated that more than 20% of the proteins in the BMRB are improperly referenced and that about 1% of all chemical shift assignments are mis-assigned. These statistics also reflect the likelihood that any newly assigned protein will have shift assignment or shift referencing errors. The relatively high frequency of these errors continues to be a concern for the biomolecular NMR community. While several programs do exist to detect and/or correct chemical shift mis-referencing or chemical shift mis-assignments, most can only do one, or the other. The one program...
nmrlearner
Journal club
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08-14-2010 04:19 AM
Four-dimensional heteronuclear correlation experiments for chemical shift assignment of solid proteins
Four-dimensional heteronuclear correlation experiments for chemical shift assignment of solid proteins
W. Trent Franks, Kathryn D. Kloepper, Benjamin J. Wylie and Chad M. Rienstra
Journal of Biomolecular NMR; 2007; 39(2); pp 107 - 131
Abstract:
Chemical shift assignment is the first step in all established protocols for structure determination of uniformly labeled proteins by NMR. The explosive growth in recent years of magic-angle spinning (MAS) solid-state NMR (SSNMR) applications is largely attributable to improved methods for backbone and side-chain chemical shift correlation...
stewart
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08-05-2008 01:33 PM
chemical shift anisotropy (CSA) in model-free approach
Hi !
I have a quite general question about the value used for the CSA while studying protein dynamics of 15N-1H vectors with model-free approach.
In the litterature, we mainly find two values for the CSA (-160 and -172 ppm).
There is, if I understand well, a link between the bond length and the CSA, but everyone seems to agree about using the same value of 1.02 A which should give rise to a mean S2 of 0.85 for secondary structure when combined to a CSA of -172 ppm. When using a CSA of -160 ppm, the mean S2 for secondary structure should slightly rise up from 0.85.
The manuals for...
semor
NMR Questions and Answers
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09-29-2006 12:08 AM
Hi guys I need to help to restate this small pragraph? Chemical shift?solid state physics?
The chemical shift The chemical shift is one of the most important observables in nuclear magnetic resonance. It provides valuable information about the chemical environment around a nucleus. In a real spin system, nuclei are surrounded by atomic and molecular electron clouds which interact with the nuclear spin angular moment. The principal influence of the surrounding electrons is the magnetic screening which results when electronic orbitals are perturbed by the applied magnetic field BO. The effect of the magnetic screening (shielding), called nuclear shielding, can enhance or oppose the...
Two-dimensional concurrent HMQC-COSY as an approach for small molecule chemical shift assignment and compound identification
Linear Mode
