Annual Reports on NMR Spectroscopy (ANNU REP NMR SPECTRO)

Publications in this journal

• Article: 2 A Review of REDCRAFT: Simultaneous Investigation of Structure and Dynamics of Proteins from RDC Restraints

  H Valafar, M Simin, S Irausquin
  Annual Reports on NMR Spectroscopy 01/2012; 76:23.
• Article: Recent Developments in Heteronuclear Multiple-Bond Correlation Experiments

  Wolfgang Schoefberger, Judith Schlagnitweit, Norbert Muller, GA Webb
  Annual Reports on NMR Spectroscopy 01/2010; 70:1-60.
• Article: Recent Developments in Heteronuclear Multiple-Bond Correlation Experiments

  Wolfgang Schoefberger, Judith Schlagnitweit, Norbert Müller
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  ABSTRACT: Today, structure elucidation of complex organic molecules relies heavily on the application of proton-detected heteronuclear NMR techniques. Among these techniques, the HMBC experiment is one of the most useful 2D NMR methods. Carbon–proton HMBC experiments allow the assignment of structural fragments through correlations between protons and carbons separated by more than one bond, usually two or three bonds via small 1H–13C couplings, usually 2JCH and 3JCH, but also over longer bond chains, n > 3JCH, especially in conjugated systems. In the decade preceding this review, several significant extensions to the basic HMBC experiment have been made. The main directions of developments were widening the range of accessible long-range J-coupling constants, improving sensitivity, refining resolution, suppressing one-bond correlations and accurately determining long-range coupling constants. In addition, increasing the efficiency of multi-dimensional NMR techniques, an important contemporary trend in NMR, has also had its impact on HMBC, with multiplex approaches and parallel acquisition techniques emerging. Structure elucidation and signal assignment of proton-deficient molecules like condensed aromatics has benefited most substantially from the new possibilities for a detailed analysis of long-range correlations. In this review, we summarize the basic variants of HMBC and discuss recent developments related to the technique, focusing on developments of new pulse sequences and processing protocols.
  Annual Reports on NMR Spectroscopy 01/2010; 70:1-60.
• Article: 129 Xe NMR Studies Of Xenon Adsorption

  K. V. Romanenko
  Annual Reports on NMR Spectroscopy 01/2009; 69.
• Article: Recent advances in NMR studies of cyclophanes

  L. Ernst
  Annual Reports on NMR Spectroscopy 01/2007; 60:77-143.
• Article: Application of Multi-Way Analysis to 2D NMR Data

  Henrik T. Pedersen, Marianne Dyrby, Søren B. Engelsen, Rasmus Bro
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  ABSTRACT: Two- and three-dimensional or even higher-dimensional NMR spectroscopy is changing from specialised techniques to more commonly used ones. As the complexity of the acquired NMR data increases, the task of analysing these data constantly becomes more and more demanding and new methods are required to facilitate the analysis. With one-dimensional NMR data multivariate data analysis has proven to be a strong tool, but how should one analyse higher-dimensional NMR data in order to extract as much relevant information as possible without having to break data down into smaller dimensions and thus lose the inherent structure? A class of multivariate data analytical techniques called multi-way analysis encompass techniques that have been designed to handle and analyse such data structures directly. In this paper, the theory of some of the most commonly used multi-way methods will be described and examples of their application to three-way arrays of NMR data reported in the literature will be given. The focus will be on the generic principles of multi-way analysis using three-way data in order to gently introduce the new concepts.
  Annual Reports on NMR Spectroscopy 01/2006; 59:207-233.
• Article: Long-range 1H--15N 2D NMR methods

  GE Martin, AJ Williams
  Annual Reports on NMR Spectroscopy 01/2005; 55:1-119.
• Article: Long-Range< sup> 1</sup> H--< sup> 15</sup> N Heteronuclear Shift Correlation

  G E Martin, A J Williams
  Annual Reports on NMR Spectroscopy 01/2005; 55:1-119.
• Article: Applications of NMR to thermostable proteins

  Alberti E, Consonni R, Zetta L
  Annual Reports on NMR Spectroscopy 01/2003; 50:121.
• Article: Aspects of Coherence Transfer in High Molecular Weight Proteins

  PERTTU PERMI
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  ABSTRACT: In order to understand the molecular mechanisms of life at atomic resolution, nuclear magnetic resonance (NMR) spectrocopy is among the most powerful biophysical methods available to study the structure and function of biological macromolecules. During the past 20 years, progress in NMR methodology together with instrumental development has pushed the protein size-limit amenable to solution state NMR studies from 10 kDa to 100–200 kDa. Thanks to the discovery of transverse relaxation optimized spectroscopy (TROSY), records on molecular size-limit were again broken and most likely new heights will soon be reached. In this chapter, we take a look into the performance of TROSY based triple-resonance experiments devised for the sequential assignment of high molecular weight proteins. In addition, a survey is made of basic building blocks for the coherence transfer under governing relaxation mechanisms during the course of triple-resonance experiments.
  Annual Reports on NMR Spectroscopy 53:245-296.
• Article: Intramolecular Interactions of Polyethers and Polysulfides, Investigated by NMR, Ab Initio Molecular Orbital Calculations, and Rotational Isomeric State Scheme: An Advanced Analysis of NMR Data

  YUJI SASANUMA
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  ABSTRACT: Intramolecular interactions of representative polyethers and polysulfides such as poly(methylene oxide) (PMO), poly(ethylene oxide) (PEO), poly (propylene oxide) (PPO), poly(methylene sulfide) (PMS), poly(ethylene sulfide) (PES), and poly(propylene sulfide) (PPS) have been investigated by NMR, ab initio molecular orbital (MO) calculations, and statistical mechanics of chain molecules, viz., the so-called rotational isomeric state (RIS) scheme. A conformational analysis of isotactic PPO was carried out from vicinal 1H–1H coupling constants observed from its monomeric model compound, 1,2-dimethoxypropane, and the gauche preference of the OCC∗O bond was found to due to intramolecular (CH)⋯O hydrogen bonds formed in the g±g∓ conformations for the CO/CC∗ bond pair. Carbon-13 NMR chemical shifts of six PPO dimers having different regio- and stereosequences were assigned and simulated by RIS calculations based on γ- and δ-effects of substituents. As a consequence, the hydrogen bonds were proved to exist in the PPO dimers as well. Conformational analyses of PMS, PES, and PPS were carried out from vicinal 1H–1H and 13C–1H coupling constants to determine their conformational energies defined on the RIS approximation. In parallel, conformational characteristics of PMO and PEO were investigated, and the origin and nature of intramolecular interactions of the polyethers and polysulfides were successfully elucidated as follows: (1) gauche stabilizations of CX bonds (X=O and S) of PMO and PMS, due to lone pair (nX)→antibonding orbital () hyperconjugations and intramolecular dipole–dipole interactions; (2) a competitive equilibrium between the intramolecular (CH)⋯O hydrogen bond and the so-called attractive gauche effect of PEO; (3) gauche preferences of CS bonds of PES and PPS, mainly due to and delocalizations; (4) trans preferences of CC bonds of PES and PPS, due to steric S⋯S repulsions in the gauche conformations; (5) induced dipole–dipole interactions in g±tg∓ states of PES. The NMR experiments combined with ab initio MO calculations and the RIS scheme have been demonstrated to be a powerful methodology for conformational analysis of polymers.
  Annual Reports on NMR Spectroscopy 49:213-280.
• Article: Multinuclear NMR of azo dyes and their metal complexes

  Antonín Lyčka
  Annual Reports on NMR Spectroscopy 42:1-57.
• Article: NMR Spectroscopy of Paramagnetic Haem Proteins

  James D. Satterlee
  Annual Reports on NMR Spectroscopy 17:79-178.
• Article: Structural studies of amino acids, polypeptides and proteins in the solid state by 1H cramps NMR

  Akira Shoji, Hideaki Kimura, Hisashi Sugisawa
  Annual Reports on NMR Spectroscopy 45:69-150.
• Article: Wide-line and High-resolution 1H NMR of Food Materials

  Thomas M. Eads
  Annual Reports on NMR Spectroscopy 31:143-156.
• Article: Structural Characterization of Si-based Polymer Materials by Solid-State NMR Spectroscopy

  Shigeki Kuroki, Hideaki Kimura, Isao Ando
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  ABSTRACT: Structural characterization of silicon-based polymers, with the properties of both organic materials such as light weight, high flexibility and modability and inorganic materials such as high thermal stability and high strength, by means of solid-state 1H, 13C, 29Si, and 11B NMR methods have been reviewed. These studies lead to the development of new molecular designs which improve upon the already excellent material properties.
  Annual Reports on NMR Spectroscopy 52:201-243.
• Article: NMR Spectroscopy of Biofluids

  John C. Lindon, Jeremy K. Nicholson, Jeremy R. Everett
  Annual Reports on NMR Spectroscopy 38:1-88.
• Article: Variable Temperature 1H MAS NMR: A Powerful Tool for the Investigation of Dynamic Properties of Acidic Protons in Zeolites and Heteropoly Compounds

  Toshihide Baba, Yoshio Ono
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  ABSTRACT: The dynamic nature of the protons in zeolites such as H-ZSM-5, metallosilicates molecular sieves and heteropoly compounds was examined by temperature dependence of 1H MAS NMR in the range of 298 and 473K. The temperature-dependent lineshape of 1H MAS NMR spectra of acidic protons in zeolites showed the first and unambiguous evidence for proton migration in zeolite structure. The dynamic property of protons was a more sensitive measure for the activity of protons than the static parameters such as NMR chemical shifi and I R band position of OH bonds.The temperature-dependent 1H MAS NMR also revealed the mobility of protons in heteropoly compounds (H3PWI2O40 Ag3PW12O40 and palladium metal loaded on H3PW12O40). This method gave the information of the dynamical process between protons and hydrogen molecules in the gas phase.The variable temperature 1H MAS NMR is a very useful technique for understanding dynamic properties of protons in solid acids The dynamic property is an important factor infiuencing the catalytic activity of a solid acid catalyst.The various experimental facts described above show that the temperature variable 1H MAS NMR could reveal the dynamics of protons in solid acids. Information obtained by this technique offers new insights, which could not be obtained by other means, on the acidic properties of solid acids and their catalysis. The significance of proton mobility in catalysts will be able to be discussed in the future.
  Annual Reports on NMR Spectroscopy 38:355-390.
• Article: Structural Studies of Peptides and Polypeptides in the Solid State by Nitrogen-15 NMR

  A. Shoji, S. Ando, S. Kuroki, I. Ando, G.A. Webb
  Annual Reports on NMR Spectroscopy 26:55-98.
• Article: Local Dynamics in Polypeptides Studied by Solid State 2H NMR: Side Chain Dynamics of Poly(γ-benzyl l-glutamate) and Racemic Poly(γ-benzyl glutamate)

  T. HIRAOKI, S. KITAZAWA, A. TSUTSUMI
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  ABSTRACT: Side chain dynamics of right-handed α-helical poly(γ-benzyl L-glutamate) (PBLG) was investigated by solid state 2H NMR. Two main motional modes composed of the large amplitude motions and the rapid and small-amplitude librations along the side chain were extracted from line shapes and T1 data above the glass-like transition temperature. The motional correlation times and amplitudes of the former are widely distributed, showing the heterogeneity of the side chain region. The phenyl rings at the end of the side chain also undergoes π-flipping. This reorientation is slightly restricted in the racemic complex of PBLG and its enantiomer, left-handed α-helical poly(γ-benzyl D-glutamate), in which phenyl rings from each L and D polymer are considered to stack regularly. The large amplitude motions and the librations are rather restricted in the stack state. About 75% of the side chain participate in the stacking. It is noted that the stacking structure is very flexible on the NMR time scale and the model for the ‘static’ stacks of the phenyl rings should be modified.
  Annual Reports on NMR Spectroscopy 53:297-339.