Four-Dimensional Heteronuclear Triple-Resonance NMR Spectroscopy of Interleukin-1β in Solution
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Abstract:
A method is presented that dramatically improves the resolution of protein nuclear magnetic resonance (NMR) spectra by increasing their dimensionality to four. The power of this technique is demonstrated by the application of four-dimensional carbon-13--nitrogen-15 (13C-15N)--edited nuclear Overhauser effect (NOE) spectroscopy to interleukin-1 beta, a protein of 153 residues. The NOEs between NH and aliphatic protons are first spread out into a third dimension by the 15N chemical shift of the amide 15N atom and subsequently into a fourth dimension by the 13C chemical shift of the directly bonded 13C atoms. By this means ambiguities in the assignment of NOEs between NH and aliphatic protons that are still present in the three-dimensional 15N-edited NOE spectrum due to extensive chemical shift overlap and degeneracy of aliphatic resonances are completely removed. Consequently, many more approximate interproton distance restraints can be obtained from the NOE data than was heretofore possible, thereby expanding the horizons of three-dimensional structure determination by NMR to larger proteins.Keywords:
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Nuclear magnetic resonance (NMR) spectroscopy is the most effective means for structural analysis of substances,which is rapidly developed in recent years. This article reviews applications of one-dimensional nuclear magnetic resonance spectroscopy (1D-1H NMR),2D-1H NMR including COSY(Correlation Spectroscopy),TOCSY(Total Correlation Spectroscopy),NOESY(Nuclear Overhauser Effect Spectroscopy),and ROESY(Rotating Frame Overhauser Effect Spectroscopy) in structure analysis of cyclodextrin and cyclodextrin complexes.
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Molecular formulas and what can be learned from them infrared spectroscopy nuclear magnetic resonance spectroscopy. Part One Basic concepts: nuclear magnetic resonance spectroscopy. Part Two Carbon-13 spectra, including heteronuclear coupling with other nuclei: nuclear magnetic resonance spectroscopy. Part Three Spin-spin coupling: nuclear magnetic resonance spectroscopy. Part Four Other topics in one-dimensional nmr: ultraviolet spectroscopy mass spectrometry combined structure problems nuclear magnetic resonance spectroscopy. Part Five Advanced nmr techniques.
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Nuclear magnetic resonance (NMR) spectroscopy is usually combined with infrared (IR) spectroscopy for the complete analysis of the structure of an unknown molecule. IR spectroscopy is used to detect a functional group in the sample, whereas NMR spectroscopy detects number of atoms and their type in sample. NMR technique can detect many nuclei but mostly identifies carbon-hydrogen frameworks. In this chapter, we have comprehensively discussed the NMR spectroscopy, its types, basic mechanism along with its instrumentation, applications, advantages, and disadvantages.
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In order to help provide a more detailed structural analysis of poly(4,5,6,7-tetrafluorobenzo[c]thiophene), a series of aromatic fluorinated oligomers (n = 1−4) and 1,3-dithienyl-4,5,6,7-benzo[c]thiophene have been synthesized. Structure analysis of these compounds by means of 1D and 2D NMR techniques provides a set of spectroscopic NMR data which can be considered as characteristic for the aromatic structure of the corresponding polymer. In addition to 19F-decoupled 13C NMR spectroscopy and attached fluorine tests, the method of full chemical shift assignment based on two-dimensional 1H−13C heteronuclear correlation (HETCOR) experiments optimized for JCH = 140 Hz and JCH = 8 Hz was extended with two-dimensional 19F−13C heteronuclear correlation (HETCOR) experiments optimized for JCF = 255 Hz and JCF = 45 Hz and 19F−19F homonuclear correlation spectroscopy (COSY).
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Heteronuclear molecule
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The sections in this article are 1 Introduction 2 31 P Magnetic Resonance Spectroscopy 3 2 H Magnetic Resonance Spectroscopy 4 13 C Magnetic Resonance Spectroscopy 5 19 F Magnetic Resonance Spectroscopy 6 1 H Magnetic Resonance Spectroscopy 7 Summary 8 Biographical Sketches Related Articles
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Fundamentals of Nuclear Magnetic Resonance. Experimental Techniques of NMR Spectroscopy. The Parameters of NMR Spectroscopy. 15N NMR Spectroscopy. 17O NMR Spectroscopy. 19F NMR Spectroscopy. 31P NMR Spectroscopy. 33S NMR Spectroscopy. 129Xe NMR Spectroscopy. Appendix. Indexes.
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