Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198 www.elsevier.com/locate/pnmrs

Forty years of Progress in Nuclear Magnetic Resonance Spectroscopy

J.W. Emsley a, J. Feeney b,*

a Chemistry Department, University of Southampton, Southampton SO17 1BJ, UK b Molecular Structure Division , MRC National Institute for Medical Research, The Ridgeway, Mill Hill, London NW7 1AA, UK

Received 6 January 2007 Available online 17 January 2007

Keywords: NMR history; Progress in NMR Spectroscopy; NMR Milestones

Contents

1. Introduction ...... 179 2. Milestones in NMR spectroscopy covered by Progress in NMR Spectroscopy...... 180 3. The editors of Progress in NMR Spectroscopy ...... 184 Acknowledgements ...... 184 Appendix A. Contents of Volumes 1–50 of Progress in NMR Spectroscopy...... 185 References...... 196

1. Introduction Press and latterly (since 1991) with Elsevier. We encourage our selected authors to write thorough, detailed and This issue completes the 50th volume of Progress in authoritative review articles that will be seen by the NMR Spectroscopy, edited since its initiation 40 years NMR community as being the primary source for learning ago by Jim Emsley, Jim Feeney and Les Sutcliffe (Fig. 1). about a topic. The extent to which this has been successful The journal was founded in 1966 shortly after the publica- can be judged by an examination of the contents of the first tion of their comprehensive (at the time) NMR text-book 50 volumes given in Appendix A. The electronic versions of [1]. This was written when the authors were at Liverpool any of these articles can be accessed via Science Direct. University during a period when NMR was expanding at From the diversity of the review titles in Appendix A it an astonishing rate. After its publication it was realised can be seen that our aim to cover all aspects of NMR that it would be virtually impossible for such a comprehen- and its wide application in chemistry, biology and medicine sive text to be kept up-to-date by simply publishing further is being met. editions. For this reason Les Sutcliffe approached our pub- Progress in NMR Spectroscopy is now published simulta- lisher with the proposal to set up a review series based on neously on the Internet as part of Science Direct, as well as in invited articles from carefully chosen NMR experts to pro- the traditional print form. Making articles available on the vide updated coverage of selected areas across a broad Internet, not only for our own journal, but generally for most front of the subject. His proposal was readily accepted scientific publications, has been a very significant advance and Progress in NMR Spectroscopy was born. The journal and is revolutionizing how we gain access to properly refer- has continued to grow and flourish initially with Pergamon eed material. It is very encouraging how the publishers, both ‘‘commercial’’, such as Elsevier, and ‘‘academic’’, such as the * Corresponding author. Tel.: +44 208 959 3666x2023; fax: +44 208 906 Learned Societies, have risen to the challenge posed by such a 4477. momentous change in how the results of research can be E-mail address: [email protected] (J. Feeney). made available. Writing papers describing original research

0079-6565/$ - see front matter Ó 2007 Elsevier B.V. All rights reserved. doi:10.1016/j.pnmrs.2007.01.002 180 J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198

Fig. 1. The editors of Progress in NMR Spectroscopy, Jim Emsley, Jim Feeney and Les Sutcliffe (July 2001). in primary journals is regarded as an essential part of doing involved only one dimensional NMR obtained in the contin- research, and needs no encouragement, whereas writing a uous wave mode at relatively low magnetic fields (100 MHz review is an extra, and competing task, that requires an 1H instruments had just become commercially available). At exceptional effort. Writing a review is an opportunity to chal- this time solution studies mainly used 1H NMR and were pri- lenge one’s understanding of a subject in a more general way marily involved in determinations of molecular structures than is done in writing a research paper, and in our view ben- and quantitative analysis of complex mixtures. The potential efits not only the individual authors but also the research of the technique for providing dynamic information from community in general. line-width studies and structural information from NOE measurements was already well known. When commercial 2. Milestones in NMR spectroscopy covered by Progress in FT spectrometers became available in the late 1960s the dra- NMR Spectroscopy matic increase in sensitivity resulted in 13C NMR studies at natural abundance becoming routine. In an earlier historical article [2] we charted the mile- The early volumes of JPNMRS were mainly concerned stones in NMR advances up till 1994: we have now updated with reviewing the developments in the basics of NMR: thus this list to include more recent advances covering the articles appeared on the theory and calculation of chemical period 1995–2006 (see Table 1). Over the last 40 years shifts, coupling constants, and how molecular dynamics Progress in NMR Spectroscopy has covered most of the can be studied via relaxation rates. Methods of analyzing areas mentioned here with articles exploring each of the spectra were described, and detailed descriptions of some new emerging areas. of the exciting new techniques of double and multiple reso- When PNMRS first appeared in 1966 the great advances nance were provided. Articles appeared in these early vol- which were to revolutionize experimental NMR had already umes on MAS and multi-pulse line narrowing, and one been initiated. In 1958 magic angle spinning (MAS) of solid other emerging NMR method was described, namely that samples to provide higher resolution spectra had been dem- of using liquid crystalline solvents to obtain partially-aver- onstrated, and Andrew described these experiments in an aged quantities such as chemical shift anisotropies and resid- article in Volume 8. In this same volume, Mansfield ual dipolar couplings. described some of the pulse methods used for line-narrowing A little later, in 1973, Lauterbur and independently Mans- of spectra in solid state NMR, developed by himself and also field and Grannell published the papers which introduced by Waugh and his colleagues. These two techniques, when MRI, and which soon led to the now familiar medical imaging combined with methods for polarization transfer, would techniques. MRI continued to develop at a rapid rate with first eventually lead to the wonderful array of experiments which reports of studies of limbs, organs and then of whole bodies now make solid-state NMR such a powerful method of being reported [82]. The quality of the images improved studying materials including, recently, microcrystalline and greatly following implementation of new techniques such as fibrous proteins. When PNMRS was first published in echo planar imaging [83] and spin-warp imaging [91] together 1966 it was just one year after Ernst and Anderson had intro- with 3D projection reconstruction methods [94]. duced the pulse Fourier transform experiment, which would The early 1970s also saw the development of a completely eventually revolutionize the whole of NMR. However, most new area of NMR application when Moon and Richards NMR experiments on liquids and solutions in 1966 still [23] and Hoult and co-workers [24] demonstrated for the J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198 181

Table 1 Milestones in the development of nuclear magnetic resonance spectroscopya 1924–1939 Early work characterizing nuclear magnetic moments and using beam methods [3–5] 1936 First attempt (unsuccessful) to detect NMR in solids [45,46] 1938 First NMR experiment using molecular beam method [5] 1945 Detection of NMR signals in bulk materials [6,7] 1948 Bloembergen, Purcell and Pound (BPP) paper on relaxation [8] 1948 Van Vleck expression for second and fourth moments [63] 1949 Knight shift in metals [9] 1949–1950 Discovery of chemical shift [9–11] Discovery of spin–spin coupling [12–14] 1950 Hahn spin echoes [16] 1950 Discovery of nuclear quadrupolar resonance [31] 1951 Discovery of 1H chemical shifts [30] 1952 First commercial NMR spectrometer (Varian 30 MHz) 1952 Bloch [6] and Purcell [7] receive Nobel Prize for NMR 1953 Bloch equations for NMR relaxation [6,32] 1953 Overhauser effect [18] 1953 Theory for effects of exchange on NMR spectra [33,34] 1954 Carr-Purcell spin echoes [35] 1955 Solomon equations for NMR relaxation [36] 1955 Relaxation in the rotating frame [37] 1956 Early NMR studies on body fluids and tissues [120,121] 1953–1958 Sample-spinning used for resolution improvement [32] Field gradient shimming with electric currents [38] Magnetic flux stabilization (Varian) Spin-decoupling [39] Variable temperature operation ([40] and Varian) 1957 Redfield theory of relaxation [41] 1957 Analysis of second-order spectra [42,43,92,93] 1957 NMR spectrum shown to be Fourier transform (FT) of Free Induction Decay (FID) [44] 1958 Magic angle spinning used for high resolution studies of solids [19,20] 1959 Blood flow measurements in vivo [47] 1959 Vicinal coupling constant dependence on dihedral angle [48] 1961 First 60 MHz field/frequency locked NMR spectrometer (Varian A60) 1962 First superconducting magnet NMR spectrometer (Varian 220 MHz) 1962 Indirect detection of nuclei heteronuclear double resonance (INDOR) [49] 1963 Liquid crystal solvents used [54] 1964 Spectrum accumulation for signal averaging [52] 1965 Nuclear Overhauser enhancements (NOE) used in conformational studies [50] 1965 Pulsed field gradients used for transport and diffusion studies [122,123] 1965 Deuterium spectrum of a liquid crystal [51] 1965 Fourier transform (FT) techniques introduced [17,52] 1967 Spin multiplets detected in solids [53] 1969 Nuclear ferromagnetism [56] 1969 First commercial FT NMR spectrometer (Bruker 90 MHz) 1969 Computer controlled pulse programmers 1969 Lanthanide paramagnetic shift reagents [57] 1970–1975 13C studies at natural abundance become routine

1970 Rotating frame T1 relaxation used for chemical exchange studies [15] 1970 First commercial FT spectrometer with superconducting magnet (Bruker 270 MHz) 1971 Pulse sequences for solvent signal suppression [58]

1971 T1 relaxation measurements in FT mode [60] 1971 Two-dimensional (2D) NMR concept suggested [61] 1971 Photo CIDNP (chemically induced dynamic nuclear polarization) [64,65] 1972 13C studies of cellular metabolism [62] 1972 Transferred NOE [21] and its use in studies of bound ligand conformations [29] 1973 31P detection of intracellular phosphates [23] 1973 NMR analysis of body fluids [23] and tissues [24] 1973 Spin-imaging methods proposed [27,28,119] 1973 NMR diffraction used for NMR imaging [28] 1973 Zeugmatography: first two-dimensional NMR image [27] 1973 360 MHz superconducting NMR spectrometer (Bruker) 1974 Sensitive point imaging method [66] 1974 2D-NMR techniques developed [67] 1975 Slice selection in imaging by selective excitation [68–70] (continued on next page) 182 J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198

Table 1 (continued) 1975 Fourier zeugmatography [71] 1976–1979 31P studies of muscle metabolism [72–80] 1976 Cross polarization/magic angle spinning for solids [81] 1976 Cryogenic probes [124,125] 1977 First 600 MHz spectrometer (non-persistent) (Mellon Institute) 1977–1980 Spin-imaging of human limbs and organs [82] 1977 Echo-planar imaging [83] 1977–1978 Whole-body scanning 1979 Detection of insensitive nuclei enhanced by polarization transfer (INEPT) [84] 1979 Detection of heteronuclear multiple quantum coherence (HMQC) [55,85] 1979 500 MHz superconducting spectrometer (Bruker) 1979 Chemical shift imaging [86–89] 1980 Surface coils used for in vivo NMR [90] 1980 Spin warp-imaging [91] 1980 3D-projection reconstruction [94] 1980 Pulse field gradients used for coherence selection [115] 1981 Composite pulse decoupling [98,109] 1981 NMR used to diagnose a medical condition [95] 1981–1983 Perfusion methods used for NMR studies of cell metabolism [96,97] 1982 Full assignments for small protein [99] 1983 First 3D structures of proteins from NMR data [22,100] 1983 Whole body imaging at 1.5 T [101] 1984–1987 Gradient methods used for spatial localization [102–104] 1984 Combined imaging and spectroscopy (human brain) [105] 1985 FLASH imaging [106] 1985 MR Angiographic images [107] 1986 NMR microscopy imaging on live cell [108] 1987 600 MHz superconducting spectrometer (Bruker; Varian; Oxford Instruments) 1987 Para-hydrogen and synthesis used to provide enhanced nuclear alignment [126] 1987 Echo-planar imaging at 2 T [110] 1987 RARE imaging [127,128] 1988 2D-NMR combined with isotopically labelled proteins for full assignments [111] 1988 Whole body imaging and spectroscopy at 4T [112] 1988 Averaging 2nd order effects in solid state NMR using a double rotor (DOR) [129] 1988 Solid state MAS re-coupling experiments [153–156,200] 1989 17O NMR in solids by dynamic-angle spinning and double rotation (DAS) [130] 1989 3D-NMR on isotopically labelled proteins [113] 1990 4D-NMR on isotopically labelled proteins – assignment and conformation [114] 1990 Pulse field gradients routinely incorporated into pulse sequences [115,116] 1991 Functional MR-detection of cognitive responses [25,26] 1991 Richard Ernst receives Nobel Prize for contributions to the development of NMR methodology 1992 750 MHz spectrometers (Bruker; Varian; Oxford Instruments) 1992 Diffusion-ordered spectroscopy DOSY [131,144] 1993 NMR microscopy using superconducting receiver coil [117] 1994 NMR force detection [118] 1995–1997 Residual dipolar coupling use for protein structure determination [132–134] 1995 Microcoil 1H detection in nanolitre volumes [135] 1995 Determinations of chirality using NMR of solutions in liquid crystalline solvents [136] 1996 Structure activity relationships (SAR) by NMR [137] 1996–1999 Automated protein assignments [138,139,206,207] 1994–1997 Sensitivity increase in NMR and MRI using hyperpolarized inert gases [140–143] 1997–1999 TROSY [145], CRINEPT [146] and CRIPT [147] sequences for structural studies of large proteins >100 kDa 1997 Measurement of angles between bond vectors using dipole–dipole cross-correlated relaxation [148] 1998 Scalar couplings across hydrogen bonds measured in liquids [149,199] 1998 Assignment of MAS spectra via scalar couplings [150,151] 1993 Commercial cryoprobe and preamplifiers for increasing sensitivity (Bruker) 1998 Whole body 8T MRI for patient scanning [152] 1999 NMR structural genomics programs initiated [157–159,201] 1999 Sensitivity-Encoded Magnetic Resonance Imaging [160] 2000 Targeted contrast reagents [161] 2000 Fast spinning for narrowing 1H solid state signals [162] 2001 Symmetry based re-coupling schemes for MAS [163] 2001 High resolution protein NMR spectroscopy inside living cells [164] 2002 Protein structures from solid state NMR studies [165] 2002 Kurt Wu¨thrich awarded Nobel Prize for NMR protein structure determination 2002 Automated protein structure determination [166,167] (continued on next page) J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198 183

Table 1 (continued) 2002 Scalar couplings across hydrogen bonds measured in solids [168] 2002 Single scan 2D spectrum [202] 2002 Solid state NMR of amyloid protein structures [169] 2002–2005 Fast multidimensional NMR experiments [170–172,203,204] 2003 New methods for DNP [173,174] 2003 Peter Mansfield and Paul Lauterbur awarded Nobel Prize for MRI 2003 High resolution spectra from disordered solids [175] 2003 MQ-MAS experiment for 1/2 integer quadrupolar nuclei [176] 2003 3D structures of membrane proteins in micelles [177,178] 2004 ‘Open’ and ‘Short-bore’ magnets used for MRI 2006 Molecular imaging using a targeted hyperpolarized biosensor [179] 2006 950 MHz actively shielded magnets used for NMR (Bruker)

a Most of the earlier milestones (1926–1994) were taken from Emsley and Feeney [2], and Feeney [59].

first time that high resolution NMR 31P spectra could be have also resulted from the improved NMR technology obtained on cells and tissues. These so called MRS (mag- [191–195]. The determinations of the structures of large netic resonance spectroscopy) methods were initially used proteins dissolved in aqueous solution have been greatly to examine human muscle metabolism and later extended facilitated by the development of new techniques. For to include diagnostic studies of solid tumours and cancer example, by exploiting dipole-CSA (chemical shift anisotro- cells [180]. In 1974, the spectacular developments in multidi- py) cross-correlation (instead of ignoring it) TROSY [145] mensional NMR spectroscopy by Ernst and co-workers [67] and CRINEPT [146] pulse sequences for detecting the nar- triggered acceleration in NMR activity with new possibilities row components of multidimensional signals have vastly being further opened up by an avalanche of novel ideas from extended the molecular weight range (to >100 kDa) of large many laboratories. The manufacturers also played a major macromolecules that can be successfully studied by NMR. role by providing the pulse programmers and probe hard- Likewise the clever application of various alignment meth- ware that allowed everyone to join in the fun. New tech- ods for extracting residual dipolar coupling constants is niques were developed in the late 1970s that were to leading to determinations of improved protein structures revolutionize multidimensional NMR (most notably INEPT [196–198]. [84] and HMQC [55,85] and the use of pulsed field gradients Improvements in NMR technology and techniques have for coherences selection [115,116]). By 1982 application of often stimulated renewed and profitable activity in existing this methodology had led to full structural assignments for well-established research areas. For example, paramagnetic small proteins and soon after to the first 3D structure deter- probes are now being increasingly used to obtain long mination of a protein in solution using only NMR data range distance information in proteins. Likewise the appli- [22,100] (part of the work that earned Kurt Wu¨thrich the cation of dynamic nuclear polarization to enhance sensitiv- Nobel Prize for Chemistry in 2002). The late 1980s saw fur- ity in studies of biological samples and metabolic processes ther improvements in technology with the availability of has enjoyed a renaissance [173,174]. The availability of high field instruments (up to 750 MHz) and the development increased sensitivity afforded by modern spectrometers of 2D, 3D and 4D novel pulse sequences for use with isoto- equipped with cryoprobes now allows routine application pically (13C/15N) labelled molecules: these were applied with of the elegant pulse sequence INADEQUATE used for great success to assign signals from proteins and other com- detecting nuclei involved in 13C–13C spin coupling [208– plex biological molecules [111,113,114,181,205]. Deutera- 210]. The full potential of this method can now be realised tion became commonly used for diluting protons (giving particularly in monitoring the fate of 13C labels in biosyn- sharper lines for detected nuclei) at 50–80% deuteration lev- thetic pathway studies. els [182,183]. Later >95% deuteration was used to capitalized In the last 40 years there have been many clever innova- on TROSY experiments on large proteins. tions in NMR and MRI, with the major developments Over the last 10 years important advances have also being undoubtedly in the spectrometers and imaging sys- been made in metabolomics studies where the power of tems. The three elements which go to producing a spec- NMR in the analysis of complex mixtures is demonstrated trometer or imaging system namely the magnet, the perfectly by providing detailed profiles of the metabolites radiofrequency generation and detection system, and the in body fluids and tissues under various physiological con- integral computer used to control the data acquisition ditions and toxicological challenges [184–186]. High and processing required to produce the spectrum or image, throughput screening of potential drugs binding to target have all changed beyond the wildest dreams of the scien- proteins achieved using NMR is another application mak- tists in 1966. NMR has also benefited enormously from ing valuable contributions to the drug discovery process in the advances in computing, which in 2007 makes it possible the pharmaceutical industries [187–190]. Applications of to calculate chemical shifts, spin–spin coupling constants NMR to fundamental studies in materials such as polymers and electric field gradients to a precision undreamt of 184 J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198

40 years ago. Such computations, and those used to con- J. Feeney (Ph.D., D.Sc., F.R.S.C.): Jim Feeney gradu- vert NMR data into molecular structures, or spatial imag- ated with a degree in Chemistry from the University of Liv- es, are at the heart of modern uses of NMR. erpool in 1958 and completed his Ph.D.on NMR solution Magnet technology has brought us to the threshold of studies in 1960 at the same University. From 1960 to the stable, high-resolution, gigahertz spectrometer, and 1964 he was a Lecturer in the Chemistry Department at some whole body MRI systems are now operating at 8 T. Liverpool University before joining Varian Associates This is a far cry from the unstable, power-hungry electro- (1964–1969) where he was appointed Director of European magnets of 1966, which were the state-of-the-art for most Laboratories in 1967. He joined the Medical Research laboratories at that time. Council first in Cambridge (Molecular Pharmacology) Other essential features of the NMR spectrometer have 1969–1972 and afterwards at the National Institute for also seen great progress. Thus, for liquid samples it is now Medical Research, Mill Hill, London 1972–2007 where he routine to select coherences using digital phase shifting, or became Centre Controller, MRC Biomedical NMR Centre with field gradients. The development of gradient-selection and Head, Molecular Structure Division. He has been a pulse sequences also led to the revitalization of pulse field Visiting Professor at the Universities of Essex and Surrey. gradient spin-echo experiments, both to measure self-diffu- His main research interests are in the use of NMR to study sion, and to separate spectra of components in a mixture protein structures and protein ligand interactions. on the basis of their masses [123]. For solid samples the L.H. Sutcliffe (Ph.D., M.R.S.C.): Les Sutcliffe received modern NMR spectrometer is even more dramatically dif- his B.Sc. for Chemistry in London and his doctorate for ferent from the systems used by the early pioneers. Magic Physical Chemistry from Leeds University. He was on angle spinning at speeds up to 60 kHz is now available the staff in the Inorganic and Physical Chemistry Depart- (by using small rotors), and together with many adroit ment at the University of Liverpool from 1958 to 1985, manipulations of the nuclear spins enable high resolution being appointed Reader in 1971. He moved to the Chemis- spectra of carbons to be obtained on medium sized mole- try Department at Royal Holloway and Bedford New Col- cules that rival those obtained on the same sample dis- lege in 1985, becoming Honorary Professor and solved in a solvent. Solid state equivalents of 2D subsequently to the University of Surrey in 1990 as Visiting experiments such as COSY and INADEQUATE have been Professor. In 1995 he moved to the Institute of Food demonstrated, and it has even proved possible using proton Research in Norwich. His special research interests include MAS to determine the structure of a protein in the solid the study of molecular dynamics using nuclear and electron state [165]. This development circumvents the limitation magnetic resonance techniques as applied to the under- of molecular weight, which applies in solution state inves- standing and development of functional fluids and the rhe- tigations of macromolecular structure. Solid state methods, ology of foods. particularly re-coupling experiments, now make it possible to obtain structural information for biological materials, Acknowledgements such as membrane proteins, which are difficult to study by diffraction methods. In addition to thanking the 665 authors who have con- Both NMR and MRI/MRS continue to develop, and to tributed to articles in the 50 volumes of Progress in NMR find new applications, and the amount of published material Spectroscopy we would also like to gratefully acknowledge increases every year showing the continuing need for review the tremendous support and professional help we have re- articles to summarize, and to critically evaluate the mass of ceived from the Elsevier publishing and production teams information being produced. We intend that Progress in over the years. We have been fortunate in having had excel- NMR Spectroscopy will fulfil this need, but to achieve this lent Publishing Editors who have been active in developing goal requires our fellow NMR spectroscopists to continue the journal (most recently Karel Nederveen, Rob van to rise to the challenge of writing review articles. Daalen, Egbert van Wezenbeek, Michiel Thijssen, Andy Gent and Swan Go) and dedicated production teams (most 3. The editors of Progress in NMR Spectroscopy recently Rebecca Monahan, Mary Murphy and Owen Hynes). Finally we would particularly like to acknowledge J.W. Emsley (Ph.D., F.R.S.C.): Jim Emsley graduated the contributions of their colleagues Cecilia Hughes, with a degree in Chemistry from the University of Leeds in Angelique Janssen and April Nishimura who have had a 1956 and then studied in the Department of Inorganic and major impact on the smooth running of the journal by Structural Chemistry at that University from 1956 to 1960 providing the editors with the vital day-to-day helpful for a Ph.D. on solid state nuclear magnetic resonance. He contact with Elsevier. We would also like to thank Berry was an ICI Research Fellow from 1960 to 1962 in the Univer- Birdsall, Lyndon Emsley, Geoff Kelly, Malcolm Levitt, sity of Liverpool. He was a Lecturer in Chemistry in the Uni- Andrew Lane and Peter Morris for their helpful comments versity of Durham from 1962 to 1967 before moving to on the review, particularly on the list of Milestones. Southampton University where he has been a Professor since However we have used our own judgement in deciding 1995. His main research interests are in NMR studies of which contributions to include and apologise if we have liquid crystalline samples. overlooked any important references. J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198 185

Appendix A. Contents of Volumes 1–50 of Progress in NMR R.A. Wind and J.Z. Hu Spectroscopy In vivo and ex vivo high-resolution 1HNMRin biological systems using low-speed magic angle 207–259 Volume 50 spinning Paul S. Pregosin Valentina Domenici, Marco Geppi and Ion pairing using PGSE diffusion methods 261–288 Carlo Alberto Veracini NMR in chiral and achiral smectic phases: Volume 48 structure, orientational order and dynamics 1–50 M.L. Johns and K.G. Hollingsworth John Battiste and Richard A. Newmark Characterization of emulsion systems using Applications of 19F multidimensional NMR 1–23 NMR and MRI 51–70 Wolfgang Bermel, Ivano Bertini, Gil Goobes, Patrick S. Stayton and Gary P. Drobny Isabella C. Felli, Mario Piccioli and Solid state NMR studies of molecular Roberta Pierattelli recognition at protein–mineral interfaces 71–85 13C-detected protonless NMR R. Bo¨hmer, K.R. Jeffrey and M. Vogel spectroscopy of proteins in solution 25–45 Solid-state Li NMR with applications to the Charles D. Schwieters, John J. Kuszewski translational dynamics in ion conductors 87–174 and G. Marius Clore Rob van Daalen Using Xplor-NIH for NMR molecular Publisher’s note 175 structure determination 47–62 Sture Forse´n Mark S. Conradi, Brian T. Saam, Congratulations 177 Dmitriy A. Yablonskiy and Jason C. Woods J.W. Emsley and J. Feeney Hyperpolarized 3He and perfluorocarbon Forty years of Progress in Nuclear Magnetic gas diffusion MRI of lungs 63–83 Resonance Spectroscopy 179–198 Sergey V. Dvinskikh, Dick Sandstrom, Steven P. Brown Herbert Zimmermann and Arnold Maliniak Probing proton–proton proximities in the solid Carbon-13 NMR spectroscopy applied to state 199–251 columnar liquid crystals 85–107 Jinyuan Zhou and Peter C.M. van Zijl Chemical exchange saturation transfer Volume 49 imaging and spectroscopy 109–136 Jeremy Flinders and Thorsten Dieckmann N. Rama Krishna and V. Jayalakshmi NMR spectroscopy of ribonucleic acids 137–159 Complete relaxation and conformational J. Mitchell, P. Blomler and P.J. McDonald exchange matrix analysis of STD-NMR Spatially resolved nuclear magnetic spectra of ligand–receptor complexes 1–25 resonance studies of planar samples 161–181 Maya Dadiani, Edna Furman-Haran and Wenyi Zhang, Takeshi Sato and Hadassa Degani Steven O. Smith The application of NMR in tumor NMR spectroscopy of basic/aromatic angiogenesis research 27–44 amino acid clusters in membrane proteins 183–199 Lothar Helm Lukas K. Tamm and Binyong Liang Relaxivity in paramagnetic systems: theory NMR of membrane proteins in solution 201–210 and mechanisms 45–64 Maggy Hologne, Veniamin Chevelkov Susan J. Berners-Price, Luca Ronconi and Peter and Bernd Reif J. Sadler Deuterated peptides and proteins in Insights into the mechanism of action of MAS solid-state NMR 211–232 platinum anticancer drugs from multinuclear Stephen J. Kadlecek, Kiarash Emami, NMR spectroscopy 65–98 Martin C. Fischer, Masaru Ishii, Jiangsheng Yu, Peter B. Barker and Doris D.M. Lin John M. Woodburn, Mehdi NikKhah, In vivo proton MR spectroscopy of the human Vahid Vahdat, David A. Lipson, brain 99–128 James E. Baumgardner and Rahim R. Rizi Carole Gardiennet-Doucet, Bernard Henry and Corrigendum to Imaging physiological Piotr Tekely parameters with hyperpolarized gas MRI 233–235 Probing the ionisation state of functional groups by chemical shift tensor fingerprints 129–149 Volume 47 Glenn H. Penner and Xiaolong Liu Silver NMR spectroscopy 151–167 Alexey Krushelnitsky and Detlef Reichert R.M. Claramunt, C. Lo´pez, M.D. Santa Marı´a, Solid-state NMR and protein dynamics 1–25 D. Sanz and J. Elguero Christopher A. Hunter, The use of NMR spectroscopy to study Martin J. Packer and Cristiano Zonta tautomerism 169–206 From structure to chemical shift and vice-versa 27–39 186 J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198

Alessandro Bagno, Federico Rastrelli Book review. M.H. Levitt: Melinda J. Duer, and Giacomo Saielli Editor, ‘‘Introduction to Solid-State NMR NMR techniques for the investigation Spectroscopy’’, Blackwell of solvation phenomena and non-covalent Science (2004) 157–158 interactions 41–93 Torsten Brand, Eurico J. Cabrita and Stefan Berger Clement R. Yonker and John C. Linehan Intermolecular interaction as investigated by The use of supercritical fluids as solvents NOE and diffusion studies 159–196 for NMR spectroscopy 95–109 Paul Hodgkinson S. Ramaprasad Heteronuclear decoupling in the NMR of solids Magnetic resonance spectroscopic 197–222 imaging studies of lithium 111–121 Terry Gullion and Alexander J. Vega Volume 45 Measuring heteronuclear dipolar couplings for I = 1/2, S > 1/2 spin pairs by T. Dziembowska, P.E. Hansen and REDOR and REAPDOR NMR 123–136 Z. Rozwadowski Eduardo Ribeiro deAzevedo, Tito Jose Studies based on deuterium isotope effect on Bonagamba and Detlef Reicher 13C chemical shifts 1–29 Molecular dynamics in solid polymers 137–164 Peter F. Flynn Tracy L. Whitehead and Multidimensional multinuclear solution NMR Thomas Kieber-Emmons studies of encapsulated macromolecules 31–51 Applying in vitro NMR spectroscopy and Sharon E. Ashbrook and Stephen Wimperis 1H NMR metabonomics to breast cancer High-resolution NMR of quadrupolar nuclei characterization and detection 165–174 in solids: the satellite-transition magic angle Mikko I. Kettunen and Kevin M. Brindle spinning (STMAS) experiment 53–108 Apoptosis detection using magnetic John C. Lindon, Elaine Holmes and resonance imaging and spectroscopy 175–185 Jeremy K. Nicholson Stephen J. Kadlecek, Kiarash Emami, Toxicological applications of magnetic Martin C. Fischer, Masaru Ishii, Jiangsheng resonance 109–143 Yu, John M. Woodburn, Mehdi NikKhah, Ingo Schnell Vahid Vahdat, David A. Lipson, Dipolar recoupling in fast-MAS solid-state James E. Baumgardner and Rahim R. Rizi NMR spectroscopy 145–207 Imaging physiological parameters with L.A. Cardoza, A.K. Korir, W.H. Otto, hyperpolarized gas MRI 187–212 C.J. Wurrey and C.K. Larive Applications of NMR spectroscopy in Volume 46 environmental science 209–238 A. Suter Anne S. Ulrich The magnetic resonance force microscope 239–274 19 Solid state F NMR methods for studying Stephan Grzesiek, Florence Cordier, biomembranes 1–21 Victor Jaravine and Michael Barfield Martin Blackledge Insights into biomolecular hydrogen Recent progress in the study of biomolecular bonds from hydrogen bond scalar structure and dynamics in solution from couplings 275–300 residual dipolar couplings 23–61 Colan E. Hughes Alexej Jerschow Spin counting 301–313 From nuclear structure to the quadrupolar NMR Chris A.E.M. Spronk, Sander B. Nabuurs, interaction and high-resolution spectroscopy 63–78 Elmar Krieger, Gert Vriend and Daniel Huster Geerten W. Vuister Investigations of the structure and dynamics of Validation of protein structures derived by membrane-associated peptides by magic angle NMR spectroscopy 315–337 spinning NMR 79–107 Daniel Malmodin and Martin Billeter High-throughput analysis of protein NMR Volume 44 spectra 109–129 Helena Kovacs, Detlef Moskau and J. Frahm, P. Dechent, J. Baudewig and Manfred Spraul K. D. Merboldt Cryogenically cooled probes – a leap in NMR Advances in functional MRI of the human 1–32 technology 131–155 brain J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198 187

Wolfram Gronwald and Hans Robert Kalbitzer Robert Tycko Automated structure determination of Applications of solid state NMR to the structural proteins by NMR spectroscopy 33–96 characterization of amyloid fibrils: methods and Perttu Permi and Arto Annila results 53–68 Coherence transfer in proteins 97–137 Luisa Ciobanu, Andrew G. Webb and R.K. Harris: book review. ‘‘Annual Reports on Charles H. Pennington NMR Spectroscopy’’, Volume 49, ed. G.A. Magnetic resonance imaging of biological cells 69–93 Webb: Academic Press (Elsevier Science), Eriks Kupce, Toshiaki Nishida and Ray Freeman Oxford, England Hadamard NMR spectroscopy 95–122 ISBN 0-12-505449-1, ISSN 0066-4103 (2003) 139 R. Andrew Atkinson and Bruno Kieffer The role of protein motions in molecular Volume 41 recognition: insights from heteronuclear NMR Marc Baldus relaxation measurements 141–187 Correlation experiments for assignment and David Fushman, Ranjani Varadan, structure elucidation of immobilized Michael Assfalg and Olivier Walker polypeptides under magic angle spinning 1–47 Determining domain orientation in R. Blinc and T. Apih macromolecules by using spin-relaxation and NMR in multidimensionally modulated residual dipolar coupling measurements 189–214 incommensurate and CDW systems 49–82 Pellegrino Conte, Riccardo Spaccini and Zeev Luz, Piotr Tekely and Detlef Reichert Alessandro Piccolo Slow exchange involving equivalent sites in State of the art of CPMAS 13C NMR solids by one-dimensional MAS NMR 83–113 spectroscopy applied to natural organic matter 215–223 techniques Jeffrey W. Peng, Jonathan Moore Ronald Y. Dong and Norzehan Abdul-Manan Relaxation and the dynamics of molecules in NMR experiments for lead generation in drug the liquid crystalline phases 115–151 discovery 225–256 Cecil Dybowski and Guenther Neue Rainer Kimmich and Esteban Anoardo Solid state 207Pb NMR spectroscopy 153–170 Field-cycling NMR relaxometry 257–320 B.M. Fung 13C NMR studies of liquid crystals 171–186 Volume 43 Brian J. Stockman and Claudio Dalvit M.D. Mantle and A.J. Sederman NMR screening techniques in drug discovery Dynamic MRI in chemical process and reaction and drug design 187–231 engineering 3–60 Juha Vaara, Jukka Jokisaari, Roderick E. Andres Ramos Wasylishen and David L. Bryce Book Review: Protein NMR for the Millennium, Spin–spin coupling tensors as determined by Vol. 20 of the Biological Magnetic Resonance experiment and computational chemistry 233–304 Book Series, N.Rama Krishna, Lawrence J. Dominique Frueh Berliner (Eds.); Kluwer Academic/Plenum Internal motions in proteins and interference Publishers, New York, 2002 61–62 effects in nuclear magnetic resonance 305–324 Alex D. Bain Chemical exchange in NMR 63–103 Volume 40 Peter Gu¨ntert Automated NMR protein structure Ian C.P. Smith and Laura C. Stewart calculation 105–125 Magnetic resonance spectroscopy in medicine: clinical impact 1–34 T.N. Huckerby Volume 42 The keratan sulphates: structural investigations using NMR spectroscopy 35–110 Andrea Cherubini and Angelo Bifone M.P. Augustine Hyperpolarized xenon in biology 1–30 Transient properties of radiation damping 111–150 G. Klein and M.E. Ries S.L. Maunu The dynamics and physical structure of polymers NMR studies of wood and wood products 151–174 above the glass transition–transverse relaxation Eva de Alba and Nico Tjandra studies of linear chains, star polymers and NMR dipolar couplings for the structure networks 31–52 determination of biopolymers in solution 175–197 188 J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198

Peter Luginbuhl and Kurt Wu¨thrich V.A. Mandelshtam Semi-classical nuclear spin relaxation theory FDM: the filter diagonalization method for revisited for use with biological macromolecules 199–247 data processing in NMR experiments 159–196 Ivano Bertini, Claudio Luchinat and Giacomo D.M. Korzhnev, M. Billeter, A.S. Arseniev and Parigi V.Y. Orekhov Magnetic susceptibility in paramagnetic NMR 249–273 NMR studies of Brownian tumbling and E.T. Ahrens, P.T. Narasimhan, T. Nakada and internal motions in proteins 197–266 R.E. Jacobs M. Pons and O. Millet Small animal neuroimaging using magnetic Dynamic NMR studies of supramolecular resonance microscopy 275–306 complexes 267–324 C. Mayer J.A. Jones Nuclear magnetic resonance on dispersed NMR quantum computation 325–360 nanoparticles 307–366 Volume 37

Volume 39 F.C. Oliveira, M.J.P. Ferreira, C.V. Nunez, G.V. Rodriguez and V.P. Emerenciano J.C. Lindon, E. Holmes and J.K. Nicholson 13C NMR spectroscopy of eudesmane Pattern recognition methods and applications sesquiterpenes 1–45 in biomedical magnetic resonance 1–40 L. Ernst Maria L. Garcia-Martin, Paloma Ballesteros and NMR studies of cyclophanes 47–190 Sebastian Cerdan Anil Kumar, R. Christy Rani Grace The metabolism of water in cells and tissues as and P.K. Madhu detected by NMR methods 41–77 Cross-correlations in NMR 191–319 Isao Ando, Shigeki Kuroki, Hiromichi Kurosu R.H. Contreras and J.E. Peralta and Takeshi Yamanobe Angular dependence of spin–spin coupling NMR chemical shift calculations and constants 321–425 structural characterizations of polymers 79–133 Christopher E. Dempsey Volume 36 Hydrogen exchange in peptides and proteins using NMR spectroscopy 135–170 P. Lazzeretti Lu-Yun Lian and David A. Middleton Ring currents 1–88 Labelling approaches for protein structural J.J. van der Klink and H.B. Brom studies by solution-state and solid-state NMR 171–190 NMR in metals, metal particles and metal R. Bohmer, G. Diezemann, G. Hinze cluster compounds 89–201 and E. Rossler P. Hodgkinson and L. Emsley Dynamics of supercooled liquids and glassy Numerical simulation of solid-state NMR solids 191–267 experiments 201–239 R. George Ratcliffe, Albrecht Roscher D. Grucker and Yair Shachar-Hill Oxymetry by magnetic resonance: applications Plant NMR spectroscopy 267–300 to animal biology and medicine 241–270 Chenhua Zhao and Tetsuo Asakura J.C. Martins, M. Biesemans and R. Willem Structure of Silk studied with NMR 301–352 Tin NMR based methodologies and their use in structural tin chemistry 271–322 Volume 38 Alexander L. Breeze Isotope-filtered NMR methods for the study N. Nestle, A. Schaff and W.S. Veeman of biomolecular structure and interactions 323–372 Mechanically detected NMR, an evaluation of the applicability for chemical investigations 1–35 Volume 35 E.C. Reynhardt and G.L. High Nuclear magnetic resonance studies of 37–81 J.H. Davis and M. Auger diamond Static and magic angle spinning NMR of N. Jamin and F. Toma membrane peptides and proteins 1–84 NMR studies of protein-DNA interactions 83–114 Raymond J. Abraham R. Sharp, L. Lohr and J. Miller A model for the calculation of proton Paramagnetic NMR relaxation enhancement: chemical shifts in non-conjugated organic recent advances in theory 115–158 compounds 85–152 J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198 189

M.J. Shapiro and J.S. Gounarides M. Luhmer and J. Reisse NMR methods utilized in combinatorial Quadrupole NMR relaxation of the noble chemistry research 153–200 gases dissolved in simple liquids and solutions: S. Williams a critical review of experimental data in the Book Review: In vivo NMR spectroscopy: 201 light of computer simulation results 57–76 principles and techniques, R.A. de Graaf, Aaron Sodickson and David G. Cory Wiley, Chichester, 1998 A generalized k-space formalism for treating O.N. Antzutkin the spatial aspects of a variety of NMR Sideband manipulation in magic-angle- experiments 77–108 spinning nuclear magnetic resonance 203–266 Brian J. Stockman H. Fukui NMR spectroscopy as a tool for Theory and calculation of nuclear spin–spin structure-based drug design 109–151 coupling constants 267–294 M.J.P. Ferreira, V.P. Emerenciano, H. Desvaux and P. Berthault G.A.R. Linia, P. Romoff, P.A. T. Macari Study of dynamic processes in liquids using and G.V. Rodrigues off-resonance rf irradiation 295–340 13C NMR spectroscopy of monoterpenoids 153–206 G. Vlahov Mark W.F. Fischer, Ananya Majumdar and Erik Application of NMR to the study of olive oils 341–357 R.P. Zuiderweg J. Horsewill Protein NMR relaxation: theory, applications Quantum tunnelling aspects of methyl group and outlook 207–272 rotation studied by NMR 359–389 J.B. Miller NMR imaging of materials 273–308 Volume 34

J.H. Kristensen, H. Bildsoe, H.J. Jakobsen and Volume 32 N.C. Nielsen Application of Lie algebra to NMR R. Bruschweiler spectroscopy 1–69 Dipolar averaging in NMR Spectroscopy: Simon B. Duckett and Christopher J. Sleigh from polarization transfer to cross Applications of the parahydrogen relaxation 1–19 phenomenon: a chemical perspective 71–92 Eike Brunner and Ulrich Sternberg Michael Sattler, Jurgen Schleucher and Christian Solid-state NMR investigations on the nature Griesinger of hydrogen bonds 21–57 Heteronuclear multidimensional NMR Ray Freeman experiments for the structure determination of Shaped radiofrequency pulses in high proteins in solution employing pulsed field resolution NMR 59–106 gradients 93–158 Michael Nilges and Sean I. O’Donoghue M.E. Smith and E.R.H. van Eck Ambiguous NOEs and automated NOE Recent advances in experimental solid state assignment 107–139 NMR methodology for half-integer spin P.M. Kentgens quadrupolar nuclei 159–201 Off-resonance nutation nuclear magnetic C.S. Johnson, Jr resonance spectroscopy of half-integer Diffusion ordered nuclear magnetic resonance quadrupolar nuclei 141–164 spectroscopy: principles and applications 203–256 Doree Sitkoff and David A. Case P. Koehl Theories of chemical shift anisotropies in Linear prediction spectral analysis of NMR proteins and nucleic acids 165–190 data 257–299 Gottfried Otting S. Williams Erratum to ‘‘NMR studies of water bound to Cerebral amino acids studied by nuclear biological molecules: Progr. NMR Spectrosc., magnetic resonance spectroscopy in vivo 301–326 31 (1997) 259–285 191 G.W. Buchanan Gerhard Wider Nuclear magnetic resonance studies of crown Technical aspects of NMR spectroscopy with ethers 327–377 biological macromolecules and studies of Volume 33 hydration in solution 193–275 Cheryl H. Arrowsmith and Yu-Sung Wu Peter Bachert NMR of large (s > 25 kDa) proteins and Pharmacokinetics using fluorine NMR in vivo 1–56 protein complexes 277–286 190 J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198

Sybren S. Wijmenga and Bernd N.M. van Buuren Reginald Waldeck, Philip W. Kuchel, The use of NMR methods for conformational Alison J. Lennon and Bogdan E. Chapman studies of nucleic acids 287–387 NMR diffusion measurements to characterize membrane transport and solute binding 39–68 P.J. McDonald Volume 31 Stray field magnetic resonance imaging 69–99 Daniel Canet Andrew G. Webb Radiofrequency field gradient experiments 101–135 Radiofrequency microcoils in magnetic Stefan Berger resonance 1–42 NMR techniques employing selective John A. Chudek and Geoffrey Hunter radiofrequency pulses in combination with Magnetic resonance imaging of plants 43–62 pulsed field gradients 137–156 Vladimir A. Daragan and Kevin H. Mayo Richard Kemp-Harper, Steven P. Brown, Colan Motional model analyses of protein and E. Hughes, Peter Styles and Stephen Wimperis peptide dynamics using NMR relaxation 63–105 NMR methods for selective observation of Barry J. Hardy, Stephen W. Doughty, sodium ions in ordered environments 157–181 Martin F. Parretti, Jenifer Tennison, W.A. Thomas Bryan E. Finn and Kevin Gardner Unravelling molecular structure and Internet conferences in NMR conformation—the modern role of spectroscopy 107–117 coupling constants 183–207 Clifford B. LeMaster Jerome W. Rathke, Robert J. Klingler, Nuclear magnetic resonance spectroscopy of Rex E. Gerald II, Kurt W. Kramarz molecules in the gas phase 119–154 and Klaus Woelk R. Kreis Toroids in NMR spectroscopy 209–253 Quantitative localized 1H MR spectroscopy for clinical use 155–195 Volume 29 Gareth A. Morris, Herve´ Barjat and Timothy J. Horne John C. Lindon, Jeremy K. Nicholson Reference deconvolution methods 197–257 and Ian D. Wilson Gottfried Otting Direct coupling of chromatographic NMR studies of water bound to biological separations to NMR spectroscopy 1–49 molecules 259–285 Gabriele Varani, Fareed Aboul-ela and Richard Kemp-Harper, Steven P. Brown, Colan Friedric H.-T. Allain E. Hughes, Peter Styles and Stephen Wimperis NMR investigation of RNA structure 51–127 Erratum to ‘‘23Na NMR methods for selective Dan Farcasiu and Anca Ghenciu observation of sodium ions in ordered Determination of acidity functions and acid environments’’: Progr. NMR Spectrosc., strengths by 13C NMR 129–168 30 (1997) 157–181’’ 287 Fritz Schick Andrew N. Lane Bone marrow NMR in vivo 169–227 Book review: NMR spectroscopy and its Angel C. de Dios applications to biomedical research: Ab initio calculations of the NMR chemical Susanta K. Sarkar (ed.) 289–291 shift 229–278 Johannes Natterer and Joachim Bargon Parahydrogen induced polarization 293–315 Volume 28 H. Fukui Theory and calculation of nuclear shielding J.W. Emsley and J. Feeney constants 317–342 Milestones in the first fifty years of NMR 1–9 Ted Watson and C.T. Philip Chang E.R. Andrew and E. Szczesniak Characterizing porous media with NMR A historical account of NMR in the solid state 11–36 methods 343–386 James N. Shoolery The development of experimental and analytical high resolution NMR 37–52 Volume 30 Jack S. Cohen, Jerzy W. Jaroszewski, Ofer Kaplan, Jesus Ruiz-Cabello Huaping Mo and Thomas C. Pochapsky and Steven W. Collier Intermolecular interactions characterized by A history of biological applications of NMR nuclear Overhauser effects 1–38 spectroscopy 53–85 J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198 191

Felix W. Wehrli Ivano Bertini, Claudio Luchinat From NMR diffraction and zeugmatography and Mario Piccioli to modern imaging and beyond 87–135 Copper-zinc superoxide dismutase: a Bertil Halle paramagnetic protein that provides a unique Spin dynamics of exchanging quadrupolar frame for the NMR investigation 91–139 nuclei in locally anisotropic systems 137–159 J. Courtieu, J.P. Bayle and B.M. Fung Teresa W.-M. Fan Variable angle sample spinning NMR in liquid Metabolite profiling by one- and crystals 141–169 two-dimensional NMR analysis of 161–219 Ioannis P. Gerothanassis complex mixtures Multinuclear and multidimensional NMR Kunisuke Asayama, Yoshio Kitaoka, Guo-qing methodology for studying individual Zheng and Kenji Ishida water molecules bound to peptides and NMR studies of high Tc superconductors 221–253 proteins in solution: principles and Jack M. Miller applications 171–237 Fluorine-19 magic-angle spinning Ioannis P. Gerothanassis NMR 255–281 17O NMR studies of hemoproteins and J.A. Peters, J. Huskens and D.J. Raber synthetic model compounds in the solution Lanthanide induced shifts and relaxation rate and solid states 239–292 enhancements 283–350 J.T. Gerig Fluorine NMR of proteins 293–370 David M. LeMaster Volume 27 Isotope labelling in solution protein assignment and structural analysis 371–419 Helmut Duddeck Charles R. Sanders, II , Brian J. Hare, Selenium-77 nuclear magnetic resonance Kathleen P. Howard and James H. spectroscopy 1–323 Prestegard Laszlo Szilogyi Magnetically-oriented phospholipid micelles Chemical shifts in proteins come of age 325–430 as a tool for the study of membrane-associated Elizabeth F. Hounsell molecules 421–444 1 H NMR in the structural and conformational Olle Soderman and Peter Stilbs analysis of oligosaccharides and NMR studies of complex surfactant systems 445–482 glycoconjugates 445–474 Goran Lindblom and Greger Oredd Mika Ala-Korpela NMR Studies of translational diffusion in 1 H NMR spectroscopy of human blood lyotropic liquid crystals and lipid plasma 475–554 membranes 483–515 Photis Dais and Apostolos Spyros Feng Ni 13 C Nuclear magnetic relaxation and local Recent developments in transferred NOE dynamics of synthetic polymers in dilute methods 517–606 solution and in the bulk state 555–633 Martin Billeter Volume 25 Hydration water molecules seen by NMR and by X-ray crystallography 635–645 J.P. Cohen Addad Paul Jonsen 2 NMR and fractal properties of polymeric H zero field NMR spectroscopy 647–727 liquids and gels 1–316 Giovanna Barbarella Sulfur-33 NMR 317–343 Volume 26 P.J. Hore and R.W. Broadhurst Photo-CIDNP of biopolymers 345–402 Jukka Jokisaari Mark S. Searle NMR of noble gases dissolved in isotropic and NMR Studies of Drug–DNA interactions 403–480 anisotropic liquids 1–26 Andrew N. Lane Rafael Bruschweiler and David A. Case NMR studies of dynamics in nucleic acids 481–505 Characterization of biomolecular structure E.W. Lang and H.-D. Ludemann and dynamics by NMR cross relaxation 27–58 Density dependence of rotational and Alex D. Bain, Ian W. Burton and translational molecular dynamics in liquids William F. Reynolds studied by high pressure NMR 507–633 Artifacts in two-dimensional NMR 59–89 192 J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198

Volume 24 Volume 22 Pawan K. Agrawal and Dharam C. Jain 13C NMR spectroscopy of oleanane 1–90 R.V. Hosur triterpenoids Scaling in one and two dimensional NMR Patrick J. Barrie and Jacek Klinowski spectroscopy in liquids 1–53 129Xe NMR As a probe for the study of S.W. Homans microporous solids: a critical review 91–108 Oligosaccharide conformations: application of Majumdar and R.V. Hosur NMR and energy calculations 55–81 Simulation of 2D NMR spectra for Brandan A. Borgias, Miriam Gochin, Deborah determination of solution conformations of J. Kerwood and Thomas L. James nucleic acids 109–158 Relaxation matrix analysis of 2D NMR data 83–100 Hellmut Eckert Gerhard Wagner Structural characterization of noncrystalline NMR investigations of protein structure 101–139 solids and glasses using solid state NMR 159–293 Keith G. Orrell, Vladimir Sik and David Timothy J. Norwood Stephenson Multiple-quantum NMR methods 295–375 Quantitative investigations of molecular T.E. Bull stereodynamics by 1D and 2D NMR methods 141–208 Relaxation in the rotating frame in liquids 377–410 Bernd Wrackmeyer and Klaus Horchler Susan J. Kohler and Nancy H. Kolodny NMR parameters of alkynes 209–253 Sodium magnetic resonance imaging and Henrik Gesmar, Jens J. Led and Frits chemical shift imaging 411–433 Abildgaard Robin K. Harris and Alejandro C. Olivieri Improved methods for quantitative spectral Quadrupolar effects transferred to spin 1/2 analysis of NMR data 255–288 Jan Schraml magic-angle spinning spectra of solids 435–456 29 O.B. Lapina, V.M. Mastikhin, A.A. Shubin, Si N M R spectroscopy of trimethylsilyl tags 289–348 V.N. Krasilnikov and K.I. Zamaraev Isao Ando, Takeshi Yamanobe and Tetsuo 51V Solid state NMR studies of vanadia based Asakura Primary and secondary structures of synthetic catalysts 457–525 13 Detlef Brinkmann polymer systems as studied by CNMR NMR studies of superionic conductors 527–552 spectroscopy 349–400 J.-Ph. Ansermet, C.P. Slichter and J.H. Sinfelt Volume 23 Solid state NMR techniques for the study of surface phenomena 401–421 P. Jezzard, J.J. Attard, T.A. Carpenter Philip H. Bolton and L. D. Hall A primer on isotopic labelling in NMR Nuclear magnetic resonance imaging in the investigations of biopolymers 423–452 solid state 1–41 Oliver W. Howarth G. Marius Clore and Angela M. Gronenborn Vanadium-51 NMR 453–485 Applications of three- and four-dimensional Seymour H. Koenig and Rodney D. Brown III heteronuclear NMR spectroscopy to protein Field-cycling relaxometry of protein solutions structure determination 43–92 and tissue: implications for MRI 487–567 Robert Turner and Paul Keller Ajoy K. Roy and Paul T. Inglefield Angiography and perfusion measurements by Solid state NMR studies of local motions in NMR 93–133 polymers 569–603 Maurice Gueron, Pierre Plateau and Michel Decorps Solvent signal suppression in NMR 135–209 Volume 21 Roy E. Hoffman and George C. Levy J.W. Akitt Modern methods of NMR data processing Multinuclear studies of aluminium compounds 1–149 and data evaluation 211–258 V.M. Mastikhin, I.L. Mudrakovsky Robin L. Armstrong and A.V. Nosov Displacive order-disorder crossover in 1H NMR magic angle spinning (MAS) studies perovskite and antifluorite crystals undergoing of heterogeneous catalysis 259–299 rotational phase transitions 151–173 Leonid B. Krivdin and Ernest W. Della Andreas Dolle and Thorsten Bluhm Orientation of the rotational diffusion Spin–spin coupling constants between carbons principal axis system determined by nuclear separated by more than one bond 301–610 relaxation data 175–201 J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198 193

K. Ott, M.A. Haghani, C.A. Paulick and D. Wolfgang Robien, Brigitte Kopp, Quitmann Diana Schabl and Herbert Schwarz Quadrupolar relaxation and thermodynamical Carbon-13 NMR spectroscopy of cardenolides processes in liquid metallic alloys 203–235 and bufadienolides 131–181 D. Canet C. Chachaty Construction, evolution and detection of Applications of NMR methods to the physical magnetization modes designed for treating chemistry of micellar solutions 183–222 longitudinal relaxation of weakly coupled spin Katalin E. Kover and Gyula Batta 1/2 systems with magnetic equivalence 237–291 Theoretical and practical aspects of one- and Leonid B. Krivdin and Gennady A. Kalabin two-dimensional heteronuclear Overhauser 13 Structural applications of one-bond carbon– experiments and selective CT1- carbon spin–spin coupling constants 293–448 determinations of heteronuclear distances 223–266 Jeremy K. Nicholson and Ian D. Wilson P. Gerothanassis High resolution proton magnetic resonance Methods of avoiding the effects of acoustic spectroscopy of biological fluids 449–501 ringing in pulsed fourier transform nuclear Ole Winneche Sorensen magnetic resonance spectroscopy 267–329 Polarization transfer experiments in B. Blumich high-resolution NMR spectroscopy 503–569 White noise nonlinear system analysis in nuclear magnetic resonance spectroscopy 331–417 Volume 20 Volume 18 Rudolph Willem 2D NMR applied to dynamic stereochemical J.P.G. Malthouse problems 1–94 13C NMR of enzymes 1–59 O.N. Chupakhin, V.N. Charushin and Malcolm H. Levitt A.I. Chernyshev Composite pulses 61–122 Application of 1H, 13C and 15N NMR Paul Rosch in the chemistry of 1,4-diazines 95–206 NMR-studies of phosphoryl transferring Poul Erik Hansen enzymes 123–169 Isotope effects in nuclear shielding 207–255 F. Noack Kevin M. Brindle NMR field-cycling spectroscopy: principles NMR methods for measuring enzyme and applications 171–276 kinetics in vivo 257–293 Vladimir Mlynarik Alex D. Bain Measurement of spin coupling constants to The superspin formalism for pulse NMR 295–314 quadrupolar nuclei via relaxation studies 277–305 George H. Weiss and James A. Ferretti K. Dill and R.D. Carter Optimal design of relaxation time experiments 317–335 13C NMR spectral studies of the N-terminal Robert E. London portion of glycophorins 307–326 13C labelling in studies of metabolic regulation 337–383 Manfred Holz R. Kimmich, G. Schnur and M. Kopf New developments in NMR of simple The tube concept of macromolecular liquids in electrolyte solutions 327–403 the light of NMR experiments 385–421 J.F. Hinton, K.R. Metz and R.W. Briggs Thallium NMR spectroscopy 423–513 Volume 17 David S. Stephenson Angela M. Gronenborn and G. Marius Clore Linear prediction and maximum entropy Investigation of the solution structures of methods in NMR spectroscopy 515–626 short nucleic acid fragments by means of nuclear Overhauser enhancement Volume 19 measurements 1–32 R.A. Wind, M.J. Duijvestijn, C. van der Lugt, A. Peter Stilbs Manenschijn and J. Vriend Fourier transform pulsed-gradient spin-echo Applications of dynamic nuclear polarization studies of molecular diffusion 1–45 in 13C NMR in solids 33–67 J. Shaka and James Keeler A. Schwenk Broadband spin decoupling in Steady-state techniques for low sensitivity and isotropic-liquids 47–129 slowly relaxing nuclei 69–140 194 J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198

Jozef Kowalewski, Lars Nordenskiold, Nikolas Volume 14 Benetis and Per-Olof Westlund Theory of nuclear spin relaxation in Poul Erik Hansen paramagnetic systems in solution 141–185 Carbon–hydrogen spin–spin coupling Janez Stepisnik constants 175–295 Measuring and imaging of flow by NMR 187–209 J. Tabony K. Muller, P. Meier and G. Kothe Nuclear magnetic resonance studies of Multipulse dynamic NMR of liquid crystal molecules physisorbed on homogeneous polymers 211–239 surfaces 1–26 P.S. Belton and R.G. Ratcliffe J.C. Lindon and A.G. Ferrige NMR and compartmentation in biological Digitisation and data processing in Fourier tissues 241–279 transform NMR 27–66 David L. Turner Fuyuhiko Inagaki and Tatsuo Miyazawa Basic two-dimensional NMR 281–358 NMR analyses of molecular conformations and conformational equilibria with the lanthanide probe method 67–111 Volume 16 Russell E. Jacobs and Eric Oldfield NMR of membranes 113–136 David G. Gorenstein Geoffrey Bodenhausen Non-biological aspects of phosphorus-31 Multiple-quantum NMR 137–173 NMR spectroscopy 1–98 J.P. Bloxsidge and J.A. Elvidge Practical aspects of tritium magnetic resonance 99–114 Volume 13 H.G. Hertz The problem of intramolecular rotation in Dennis R. Burton, Sture Forsen, Gunnar liquids and nuclear magnetic relaxation 115–162 Karlstrom and Raymond A. Dwek O.W. Sorensen, G.W. Eich, M.H. Levitt, G. Proton relaxation enhancement (PRE) in Bodenhausen and R.R. Ernst biochemistry: a critical survey 1–45 Product operator formalism for the F. Heatley description of NMR pulse experiments 163–192 Nuclear magnetic relaxation of synthetic W.S. Veeman polymers in dilute solution 47–85 Carbon-13 chemical shift anisotropy 193–235 Lee J. Todd Allen R. Siedle J. Klinowski NMR studies of boranes, carboranes and Nuclear magnetic resonance studies of zeolites 237–309 hetero-atom boranes 87–176 Christopher J. Turner Victor Wray Multipulse NMR in liquids 311–370 Carbon–carbon coupling constants: a compilation of data and a practical guide 177–256 Volume 15 Pierre Laszlo Fast kinetics studied by NMR 257–270 R.E. Gordon, P.E. Hanley and D. Shaw R. Lenk Topical magnetic resonance 1–47 Thermodynamics of nuclear spins 271–302 R.A. Iles, A.N. Stevens and J.R. Griffiths C.W. Haigh R.B. Mallion NMR Studies of metabolites in living tissue 49–200 Ring current theories in nuclear magnetic N.A.B. Gray resonance 303–344 Computer assisted analysis of carbon-13 NMR spectral data 201–248 J. Lounila and J. Jokisaari Volume 12 Anisotropies in spin–spin coupling constants Oliver W. Howarth David M.J. Lilley and chemical shifts as determined from the Carbon-13-NMR of peptides and proteins 1–40 NMR spectra of molecules oriented by liquid D.I. Hoult crystal solvents 249–290 The NMR receiver: a description and analysis Peter L. Rinaldi of design 41–77 The determination of absolute configuration Robert L. Vold and Regitze R. Vold using nuclear magnetic resonance techniques 291–352 Nuclear magnetic relaxation in coupled spin Jeremy K.M. Sanders and John D. Mersh systems 79–133 Nuclear magnetic double resonance; the use of David B. Davies difference spectroscopy 353–400 Conformations of nucleosides and nucleotides 135–225 J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198 195

Bernd Wrackmeyer Volume 8 Carbon-13 NMR spectroscopy of boron compounds 227–259 E.R. Andrew R.N. Young The narrowing of NMR spectra of solids by NMR spectroscopy of carbanions and high-speed specimen rotation and the carbocations 261–286 resolution of chemical shift and spin multiplet structures for solids 1–39 Volume 11 P. Mansfield Pulsed NMR in solids 43–101 Jozef Kowalewski J.H. Goldstein, V.S. Watts and L.S. Rattet 13 Calculations of nuclear spin–spin coupling CH Satellite NMR Spectra 104–162 constants 1–78 G.J. Martin and M.L. Martin J.N. Shoolery The stereochemistry of double bonds 166–259 Some quantitative applications of 13C NMR spectroscopy 79–93 Brian E. Mann Volume 7 Dynamic 13C NMR spectroscopy 95–114 V.S. Petrosyan J.W. Emsley, L. Phillips NMR Spectra and structures of organotin Fluorine chemical shifts 1–520 compounds 115–148 K.A.K. Ebraheem and G.A. Webb Semi-empirical calculations of the chemical Volume 6 shifts of nuclei other than protons 149–181 J.N. Murrell S. Aime and L. Milone The theory of nuclear spin–spin coupling in Dynamic 13C NMR spectroscopy of metal high resolution NMR spectroscopy 1–60 carbonyls 183–210 E.G. Finer and R.K. Harris Henry H. Mantsch, Hazime Saito and Spin–spin coupling between phosphorus Ian C.P. Smith nuclei 61–118 Deuterium magnetic resonance, applications E.W. Randall and D.G. Gillies in chemistry, physics and biology 211–272 Nitrogen nuclear magneticresonance 119–174 Volume 10

P.D. Buckley, K.W. Jolley and D.N. Pinder Volume 5 Application of density matrix theory to NMR line-shape calculations 1–26 V.J. Kowalewski J. Hilton and L.H. Sutcliffe The indor technique in high-resolution nuclear The ‘‘through-space’’ mechanism in spin–spin magnetic resonance 1–31 coupling 27–39 T.H. Siddall and W.E. Stewart V.F. Bystrov Magnetic non-equivalence related to Spin–spin coupling and the conformational symmetry considerations and restricted states of peptide systems 41–82 molecular motion 33–147 J.W. Emsley, L. Phillips and V. Wray Harold Booth Flourine coupling constants 83–752 Applications of 1H nuclear magnetic resonance spectroscopy to the Volume 9 conformational analysis of cyclic compounds 149–381 J. Reuben Paramagnetic lanthanide shift reagents in NMR spectroscopy: principles, methodology Volume 4 and applications 3–70 N.M. Sergeyev Roy Foster and Colin A. Fyfe Nuclear magnetic resonance spectroscopy of Nuclear magnetic resonance of organic cyclopentadienyl compounds 71–144 charge-transfer complexes 1–89 Ronald G. Lawler Norman S. Ham, T. Mole Chemically induced dynamic nuclear The application of NMR to organometallic polarization 147–210 exchange reactions 91–192 196 J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198

L.W. Reeves G. Mavel The study of water in hydrate crystals by Studies of phosphorus compounds using the nuclear magnetic resonance 193–233 magnetic resonance spectra of nuclei other C. Deverell than phosphorus-31 251–373 Nuclear magnetic resonance studies of electrolyte solutions 235–334 Monisha Bose References Nuclear magnetic resonance in magnetic materials 335–444 [1] High Resolution Nuclear Magnetic Resonance Spectroscopy, 2 Volumes, Pergamon Press 1965, 1966, J.W. Emsley, J. Feeney, L.H. Volume 3 Sutcliffe (Available on Science Direct website for Progress in NMR Spectroscopy as Volume 1, Part 1 pp.1–663 (1965): Volume 1, Part 2 pp. 665–1154 (1966)). P. Diehl, R.K. Harris and R.G. Jones [2] J.W. Emsley, J. Feeney, Prog. NMR Spectrosc. 28 (1995) 1. Sub-spectral analysis 1–61 [3] W. Pauli, Naturwisschaften 12 (1924) 741. H. Batiz-Hernandez and R.A. Bernheim [4] W. Gerlach, O. Stem, Ann. Phys. Leipzig. 74 (1924) 673. The isotope shift 63–85 [5] I.I. Rabi, S. Millman, P. Kusch, J.R. Zacharias, Phys. Rev. 55 (1939) K.J. Packer 526, 53 (1938) 318. [6] F. Bloch, W.W. Hansen, M.E. Packard, Phys. Rev. 69 (1946) 127. Nuclear spin relaxation studies of molecules [7] E.M. Purcell, H.C. Torrey, R.V. Pound, Phys. Rev. 69 (1946) 37. adsorbed on surfaces 87–128 [8] N. Bloembergen, E.M. Purcell, R.V. Pound, Phys. Rev. 73 (1948) 679. E.L. Mackor and C. Maclean [9] W.D. Knight, Phys. Rev. 76 (1949) 1259. Relaxation processes in systems of two non- [10] W.G. Proctor, F.C. Yu, Phys. Rev. 77 (1950) 717. identical spins 129–157 [11] W.C. Dickinson, Phys. Rev. 77 (1950) 736. [12] W.G. Proctor, F.C. Yu, Phys. Rev. 81 (1951) 20. H.G. Hertz [13] H.S. Gutowsky, D.W. McCall, Phys. Rev. 82 (1951) 748. Microdynamic behaviour of liquids as studied [14] E.L. Hahn, D.E. Maxwell, Phys. Rev. 84 (1951) 1246. by NMR relaxation times 159–230 [15] C. Deverell, R.E. Morgan, J.H. Strange, Mol. Phys. 18 (1970) 553. Pierre Laszlo [16] E.L. Hahn, Phys. Rev. 80 (1950) 580. Solvent effects and nuclear magnetic resonance 231–402 [17] R.R. Ernst, W.A. Anderson, Rev. Sci. Instrum. 37 (1966) 93. [18] A.W. Overhauser, Phys. Rev. 92 (1953) 411. [19] E.R. Andrew, A. Bradbury, R.G. Eades, Nature 182 (1958) 1659, Volume 2 183 (1959) 1802. [20] I.J. Lowe, Phys. Rev. Lett. 2 (1959) 285. D.E. O’Reilly [21] A.A. Bothner-By, R. Gassend, Ann. NY Acad. Sci. 222 (1972) 668. Chemical shift calculations 1–61 [22] M.P. Williamson, T. Havel, K. Wu¨thrich, J. Mol. Biol. 182 (1985) A.D. Buckingham, K.A. McLauchlan 195. High resolution nuclear magnetic resonance in [23] R.B. Moon, J.H. Richards, J. Biol. Chem. 248 (1973) 7276. [24] D.I. Hoult, S.J.W. Busby, D.G. Gadian, G.K. Radda, R.E. partially oriented molecules 63–109 Richards, P.J. Seeley, Nature 252 (1974) 285. E. De Boer and H. Van Willigen [25] J.W. Belliveau, D.N. Kennedy, R.C. McKinstry, B.R. Buchbinder, Nuclear magnetic resonance of paramagnetic R.M. Weisskoff, M.S. Cohen, J.M. Vevea, T.J. Brady, B.R. Rosen, systems 111–161 Science 254 (1991) 716. Ruth M. Lynden-Bell [26] J. Prichard, D. Rothman, E. Novotny, O. Petroff, T. Kuwabara, M. Avison, A. Howseman, C. Hanstock, R. Shulman, Proc. Natl. Acad. The calculation of line shapes by density Sci. USA 88 (1991) 5829. matrix methods 163–204 [27] P.C. Lauterbur, Nature 242 (1973) 190. R.F. Zurcher [28] P. Mansfield, P.K. Grannell, J. Phys. C: Solid State Phys. 6 (1973) The cause and calculation of proton chemical L422. shifts in non-conjugated organic compounds 205–257 [29] J.P. Albrand, B. Birdsall, J. Feeney, G.C.K. Roberts, A.S.V. Burgen, Int. J. Biol. Macromol. 1 (1979) 37. [30] J.T. Arnold, S.S. Dharmatti, M.E. Packard, J. Chem. Phys. 19 Volume 1 (1951) 507. [31] H.G. Dehmelt, H. Kruger, Naturwissenschaften 37 (1950) 111. R.E. Richards [32] F. Bloch, Phys. Rev. 94 (1954) 946. Foreword xix [33] H.S. Gutowsky, D.W. McCall, C.P. Slichter, J. Chem. Phys. 21 O. Haworth and R.E. Richards (1953) 279. [34] H.M. McConnell, J. Chem. Phys. 28 (1958) 430. The use of modulation in magnetic resonance 1–14 [35] H.Y. Carr, E.M. Purcell, Phys. Rev. 94 (1954) 630. Ragnar A. Hoffman and Sture Forsen [36] I. Solomon, Phys. Rev. 99 (1955) 559. High resolution nuclear magnetic double and [37] A.G. Redfield, Phys. Rev. 98 (1955) 1787. multiple resonance 15–204 [38] M.J.E. Golay, Rev. Sci. Instrum. 29 (1958) 313. J.D. Swalen [39] A.L. Bloom, J.N. Shoolery, Phys. Rev. 97 (1955) 1261. [40] H.S. Gutowsky, L.H. Meyer, R.E. McClure, Rev. Sci. Instrum. 24 Computer techniques in the analysis of NMR (1953) 644. spectra 205–250 [41] A.G. Redfield, IBM J. Res. Dev. 1 (1957) 19. J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198 197

[42] H.S. Gutowsky, C.H. Holm, A. Saika, G.A. Williams, J. Am. Chem. [88] A.A. Maudsley, S.K. Hilal, W.H. Perman, H.E. Simon, J. Magn. Soc. 79 (1957) 4596. Reson. 51 (1983) 147. [43] H.J. Bernstein, J.A. Pople, W.G. Schneider, Can. J. Chem. 35 (1957) [89] A.A. Maudsley, A. Oppelt, A. Ganssen, Siemens Forsch. Entwickl. 65; Ber. 8 (1979) 326. H.J. Bernstein, J.A. Pople, W.G. Schneider, Can. J. Chem. 35 (1957) [90] J.J.H. Ackerman, T.H. Grove, G.G. Wong, D.G. Gadian, G.K. 1060. Radda, Nature 283 (1980) 167. [44] I.J. Lowe, R.E. Norberg, Phys. Rev. 107 (1957) 46. [91] W.A. Edelstein, J.M.S. Hutchison, G. Johnson, T. Redpath, Phys. [45] C.J. Gorter, Physica 3 (1936) 995. Med. Biol. 25 (1980) 751. [46] C.J. Gorter, L.F.J. Broer, Physica 9 (1942) 591. [92] J.T. Arnold, Phys. Rev. 102 (1956) 136. [47] J.R. Singer, Science 130 (1959) 1652. [93] W.A. Anderson, Phys. Dev. 102 (1956) 151. [48] M. Karplus, J. Chem. Phys. 30 (1959) 11; [94] C.M. Lai, P.C. Lauterbur, J. Phys. E. Sci. Instrum. 13 (1980) 747. M. Karplus, J. Phys. Chem. 64 (1960) 1793. [95] B.D. Ross, G.K. Radda, D.G. Gadian, G. Rocker, M. Esiri, J. [49] E.B. Baker, J. Chem. Phys. 37 (1962) 911. Falconer-Smith, J. New Engl. J. Med. 304 (1981) 1338. [50] F.A.L. Anet, A.J.R. Bourn, J. Am. Chem. Soc. 87 (1965) 5250. [96] K. Ugurbil, D.L. Guernsey, T.R. Brown, P. Glynn, N. Tobkes, I.S. [51] W.D. Phillips, J.C. Rowell, L.R. Melby, J. Chem. Phys. 41 (1964) Edelman, Proc. Natl. Acad. Sci. USA 78 (1981) 4843. 2551. [97] D.L. Foxall, J.S. Cohen, J. Magn. Reson. 52 (1983) 346. [52] R.R. Ernst, Rev. Sci. Instrum. 36 (1965) 1689. [98] M.H. Levitt, R. Freeman, J. Magn. Reson. 43 (1981) 502. [53] E.R. Andrew, L.F. Farnell, T.D. Gledhill, Phys. Rev. Lett. 19 (1967) 6. [99] G. Wagner, K. Wu¨thrich, J. Mol. Biol. 155 (1982) 347. [54] A. Saupe, G. Englert, Phys. Rev. 11 (1963) 462. [100] W. Braun, G. Wider, K.H. Lee, K. Wu¨thrich, J. Mol. Biol. 169 (1983) [55] L. Mueller, J. Am. Chem. Soc. 101 (1979) 4481. 921. [56] M. Chapellier, M. Goldman, V.H. Chan, A. Abragam, C. R. Acad. [101] H.R. Hart, P.A. Bottomley, W.A. Edelstein, S.J. Karr, W.M. Leue, Sci. 268 (1969) 1530. O. Mueller, R.W. Redington, J.F. Schenck, L.S. Smith, D. Vatis, [57] R.E. Sievers (Ed.), NMR Shift Reagents, Academic Press, New Am. J. Roentgenol. 141 (1983) 1195. York, 1973. [102] P.A. Bottomley, US Patent, 4 480 228, 1984. [58] S.L. Patt, S.B. Sykes, J. Chem. Phys. 54 (1971) 1148. [103] R.J. Ordidge, A. Connelly, J.A.B. Lohman, J. Magn. Reson. 66 [59] J. Feeney, in: R. Budd, S.E. Cozzens (Eds.), Invisible Connections: (1986) 283. Instruments, Institutions and Science, SPIE Optical Engineering [104] J. Frahm, K.D. Merboldt, W. Hgnicke, J. Magn. Reson. 72 (1987) Press, Chapter 10, 1992. 502. [60] R.L. Vold, J.S. Waugh, M.P. Klein, D.E. Phelps, J. Chem. Phys. 48 [105] P.A. Bottomley, H.R. Hart Jr., W.A. Edelstein, J.F. Schenck, L.S. (1968) 3831. Smith, W.M. Leue, O.M. Mueller, R.W. Redington, Radiology 150 [61] J. Jeener, Ampere International Summer School, Basko Polje, (1984) 441. Yugoslavia, 1971, (unpublished). [106] A. Haase, J. Frahm, D. Matthaei, W. Hgnicke, K.D. Merboldt, J. [62] N.A. Matwiyoff, T.E. Needham, Biochem. Biophys. Res. Commun. Magn. Reson. 67 (1986) 258. 49 (1972) 1158. [107] V.J. Wedeen, R.A. Mueli, R.R. Edelman, S. Geller, L. Frank, T. [63] J.H. Van Vleck, Phys. Rev. 74 (1948) 1168. Brady, B. Rosen, Science 230 (1985) 946. [64] R. Kaptein, J.C.S. Chem. Commun. (1971) 732. [108] J. Aguayo, S. Blackband, J. Schoeniger, M. Mattingly, M. Hinter- [65] R. Kaptein, K. Dijkstra, K. Nicolay, Nature 247 (1978) 293. mann, Nature 322 (1986) 190. [66] W.S. Hinshaw, Phys. Lett. 48 (1974) 87. [109] J.S. Waugh, J. Magn. Reson. 49 (1982) 517. [67] W.P. Aue, E. Bartholdi, R.R. Ernst, J. Chem. Phys. 64 (1976) 229. [110] I.L. Pykett, R.R. Rzedzian, Magn. Reson. Med. 5 (1987) 563. [68] A.N. Garroway, P.K. Grannell, P. Mansfield, J. Phys. C: Solid State [111] D.H. Torchia, S.W. Sparks, A. Bax, Biochemistry 27 (1988) 5135. Phys. 7 (1974) L457. [112] H. Barfuss, H. Fischer, D. Hentschel, R. Ladebeck, J. Vetter, [69] R.J. Sutherland, J.M.S. Hutchison, J. Phys. E. 11 (1978) 79. Radiology 169 (1988) 811. [70] D.I. Hoult, J. Magn. Reson. 26 (1977) 165; [113] D. Marion, P.C. Driscoll, L.E. Kay, P.T. Wingfield, A. Bax, A.M. D.I. Hoult, J. Magn. Reson. 35 (1979) 69. Gronenborn, G.M. Clore, Biochemistry 28 (1989) 6150. [71] A. Kumar, D. Welti, R.R. Ernst, J. Magn. Reson. 18 (1975) 69. [114] L.E. Kay, G.M. Clore, A. Bax, A.M. Gronenborn, Science 249 (1990) [72] C.T. Burt, T. Glonek, M. Barany, J. Biol. Chem. 251 (1976) 2584. 411. [73] C.T. Burt, T. Glonek, M. Barany, Science 195 (1977) 145. [115] A. Bax, P.G. De Jong, A.F. Mehlkopf, J. Schmidt, Chem. Phys. [74] B. Garlick, G.K. Radda, P.J. Seeley, Biochem. Biophys. Res. Lett. 69 (1980) 567. Commun. 74 (1977) 1256. [116] R.E. Hurd, J. Magn. Reson. 87 (1990) 422. [75] E. Jacobus, G.J. Taylor, D.P. Hollis, R.L. Nunnally, Nature 265 [117] R.D. Black, T.A. Early, P.B. Roemer, O.M. Mueller, A. Morgo- (1977) 756. Campero, L.G. Turner, G.A. Johnson, Science 259 (1993) 793. [76] P. Hollis, R.L. Nunnally, Biochem. Biophys. Res. Commun. 75 [118] D. Rugar, O. Zugar, S. Hoen, C.S. Yannoni, H.M. Vieth, R.D. (1977) 1086. Kendrick, Science 264 (1994) 1560. [77] J. Yoshizaki, J. Biochem. 84 (1977) 11. [119] R. Damadian, K. Zaner, D. Hor, R. Dimaio, Proc. Natl. Acad. Sci. [78] M. Cohen, C.T. Burt, Proc. Natl. Acad. Sci. USA 7 (1977) 4271. USA 71 (1974) 1471. [79] A. Sehr, G.K. Radda, Biochem. Biophys. J. Commun. 77 (1977) [120] O. Jardetzky, J.E. Wertz, Arch. Biochem. Biophys. 65 (1956) 569. 195. [121] E. Odeblad, N. Bhar, G. Lindstrom, Arch. Biochem. Biophys. 63 [80] C.T. Burt, S.M. Cohen, M. Bbriny, Ann. Rev. Biophys. Bioeng. 8 (1956) 221. (1979) 1. [122] E.O. Stejskal, J.E.J. Tanner, Chem. Phys. 42 (1965) 288. [81] J. Schaefer, E.O. Stejskal, J. Am. Chem. Soc. 98 (1976) 1030. [123] C.S. Johnson, Prog. NMR Spectrosc. 34 (1999) 203. [82] P.G. Morris, NMR Imaging in Medicine and Biology, Oxford [124] D.I. Hoult, R.E. Richards, J. Magn. Reson. 24 (1976) 71. University Press, 1986. [125] P. Styles, N.F. Soffe, C.A. Scott, D.A. Cragg, D.J. White, P.C.J. [83] P. Mansfield, I.L. Pykett, J. Magn. Reson. 29 (1978) 355. White, J. Magn. Reson. 60 (1984) 397. [84] G.A. Morris, R. Freeman, J. Am. Chem. Soc. 101 (1979) 760. [126] C.R. Bowers, D.P. Weitekamp, J. Am. Chem. Soc. 109 (1987) 5541. [85] D.P. Burum, R.R. Ernst, J. Magn. Reson. 39 (1980) 163. [127] H.G. Friedburg, B. Wimmer, J. Hennig, A. Frankenschmidt, K.H. [86] J. Cox, P.J. Styles, J. Magn. Reson. 40 (1980) 209. Hauenstein, Urologe. A. 26 (1987) 309. [87] T.R. Brown, P.M. Kincaid, K. Ugurbil, Proc. Natl. Acad. Sci. USA [128] J. Hennig, H. Friedburg, Magn. Reson. Imaging 6 (1988) 391. 79 (1982) 3523. [129] A. Samoson, E. Lippmaa, A. Pines, Mol. Phys. 65 (1988) 1013. 198 J.W. Emsley, J. Feeney / Progress in Nuclear Magnetic Resonance Spectroscopy 50 (2007) 179–198

[130] B.F. Chmelka, K.T. Mueller, A. Pines, J. Stebbins, Y. Wu, J.W. [167] A. Grishaev, M. Llinas, Proc. Natl. Acad. Sci. USA 99 (2002) 6713. Zwanziger, Nature 339 (1989) 42. [168] S.P. Brown, M. Perez-Torralba, D. Sanz, R.M. Claramunt, L. [131] K.F. Morris, C.S. Johnson Jr., J. Am. Chem. Soc. 114 (1992) 3139. Emsley, Chem. Commun. 17 (2002) 1852. [132] J.R. Tolman, J.M. Flanagan, M.A. Kennedy, J.H. Prestegard, Proc. [169] A.T. Petkova, Y. Ishii, J.J. Balbach, O.N. Antzutkin, R.D. Natl. Acad. Sci. USA 92 (1995) 9279. Leapman, F. Delaglio, R. Tycko, Proc. Natl. Acad. Sci. USA 99 [133] N. Tjandra, S. Grzesiek, A. Bax, J. Am. Chem. Soc. 118 (1996) 6264. (2002) 16742. [134] N. Tjandra, A. Bax, J. Magn. Reson. 124 (1997) 512. [170] E. Kupcˇe, R. Freeman, J. Biomol. NMR 27 (2003) 383. [135] D.L. Olson, M.E. Lacey, J.V. Sweedler, Anal. Chem. 70 (1998) 645. [171] M. Mishkovsky, L. Frydman, J. Magn. Reson. 173 (2005) 344. [136] I. Canet, J. Courtieu, A. Loewenstein, A. Meddour, J.M. Pechine´,J. [172] S. Kim, T. Szyperski, J. Am. Chem. Soc. 125 (2003) 1385. Am. Chem. Soc. 117 (1995) 6520. [173] J.H. Ardenkjær-Larsen, B. Fridlund, A. Gram, G. Hansson, L. [137] S.B. Shuker, P.J. Hajduk, R.P. Meadows, S.W. Fesik, Science 274 Hansson, M.H. Lerche, R. Servin, M. Thaning, K. Golman, Proc. (1996) 1531. Natl. Acad. Sci. USA 100 (2003) 10158. [138] C. Bartels, M. Billeter, P. Gu¨ntert, K. Wu¨thrich, J. Biomol. NMR 7 [174] V.S. Bajaj, C.T. Farrar, M.K. Hornstein, I. Mastovsky, J. Vieregg, J. (1996) 207. Bryant, B. Elena, K.E. Kreischer, R.J. Temkin, R.G. Griffin, J. [139] H.N.B. Moseley, G.T. Montelione, Curr. Opin. Struct. Biol. 9 (1999) Magn. Reson. 160 (2003) 85. 635. [175] D. Sakellariou, S.P. Brown, M. Bardet, A. Lesage, S. Hediger, C.A. [140] M.S. Albert, G.D. Cates, B. Driehuys, W. Happer, B. Saam, C.S. Meriles, A. Pines, L. Emsley, J. Am. Chem. Soc. 125 (2003) 4376. Springer Jr., A. Wishnia, Nature 370 (1994) 199. [176] J. Grinshtein, L. Frydman, J. Am. Chem. Soc. 125 (2003) 7451. [141] J.R. MacFall, H.C. Charles, R.D. Black, H. Middleton, J.C. Swartz, [177] C. Fernandez, K. Wu¨thrich, FEBS Lett. 555 (2003) 144. B. Saam, B. Driehuys, C. Erickson, W. Happer, G.D. Cates, G.A. [178] L.K. Tamm, B. Liang, Prog. NMR Spectrosc. 48 (2006) 201. Johnson, C.E. Ravin, Radiology 200 (1996) 553. [179] L. Schroder, T.J. Lowery, C. Hilty, D.E. Wemmer, A. Pines, Science [142] A. Bifone, Y.Q. Song, R. Seydoux, R.E. Taylor, B.M. Goodson, T. 314 (2006) 446. Pietrass, T.F. Budinger, G. Navon, A. Pines, Proc. Natl. Acad. Sci. [180] R.A. Iles, A.N. Stevens, J.R. Griffiths, Prog. NMR Spectrosc. 15 USA 93 (1996) 12932. (1982) 49. [143] B.M. Goodson, Y. Song, R.E. Taylor, V.D. Schepkin, K.M. [181] G. Wagner, Prog. NMR Spectrosc. 22 (1990) 101. Brennan, G.C. Chingas, T.F. Budinger, G. Navon, A. Pines, A. [182] C.H. Arrowsmith, Y.-S. Wu, Prog. NMR Spectrosc. 32 (1998) 277. Proc. Natl. Acad. Sci. USA 94 (1997) 14725. [183] L-Y. Lian, D.A. Middleton, Prog. NMR Spectrosc. 39 (2001) 171. [144] H. Barjat, G.A. Morris, S. Smart, A.G. Swanson, S.C.R. Williams, [184] T.W.-M. Fan, Prog. NMR Spectrosc. 28 (1996) 161. J. Magn. Reson. Ser. B 108 (1995) 170. [185] J.C. Lindon, J.K. Nicholson, I.D. Wilson, Prog. NMR Spectrosc. 29 [145] K. Pervushin, R. Riek, G. Wider, K. Wu¨thrich, Proc. Natl. Acad. (1996) 1. Sci. USA 94 (1997) 12366. [186] J.C. Lindon, E. Holmes, J.K. Nicholson, Prog. NMR Spectrosc. 45 [146] R. Riek, G. Wider, K. Pervushin, K. Wu¨thrich, Proc. Natl. Acad. (2004) 109. Sci. USA 96 (1999) 4918. [187] B.J. Stockman, Prog. NMR Spectrosc. 31 (1997) 109. [147] R. Bru¨schweiler, R.R. Ernst, J. Chem. Phys. 96 (1991) 1758. [188] P. Bachert, Prog. NMR Spectrosc. 33 (1998) 1. [148] B. Reif, M. Hennig, C. Griesinger, Science 276 (1997) 1230. [189] B.J. Stockman, C. Dalvit, Prog. NMR Spectrosc. 41 (2002) 187. [149] A.J. Dingley, S. Grzesiek, J. Am. Chem. Soc. 120 (1998) 8293. [190] J.W. Peng, J. Moore, N. Abdul-Manan, Prog. NMR Spectrosc. 44 [150] A. Lesage, D. Sakellariou, S. Steuernagel, L. Emsley, J. Am. Chem. (2004) 225. Soc. 120 (1998) 13194. [191] F. Heatley, Prog. NMR Spectrosc. 13 (1979) 47. [151] A. Lesage, L. Emsley, J. Magn. Reson. 148 (2001) 449. [192] P. Dais, A. Spyros, Prog. NMR Spectrosc. 27 (1995) 555. [152] P-M.L. Robitaille, A.M. Abduljalil, A. Kangarlu, X. Zhang, [193] I. Ando, S. Kuroki, H. Kurosu, T. Yamanobe, Prog. NMR Y.Yu.R. Burgess, S. Bair, P. Noa, L. Yang, H. Zhu, B. Palmer, Z. Spectrosc. 39 (2001) 79. Jiang, D.M. Chakeres, D. Spigos, NMR Biomed. 11 (1998) 263. [194] P.G. Klein, M.E. Ries, Prog. NMR Spectrosc. 42 (2003) 31. [153] T.G. Oas, R.G. Griffin, M.H. Levitt, J. Chem. Phys. 89 (1988) 692. [195] E. Ribeiro deAzevedo, T.J. Bonagamba, D. Reicher, Prog. NMR [154] M.H. Levitt, T.G. Oas, R.G. Griffin, Isr. J. Chem. 28 (1988) 271. Spectrosc. 47 (2005) 13. [155] T. Gullion, M.D. Poliks, J. Schaefer, J. Magn. Reson. 80 (1988) 553. [196] E. de Alba, N. Tjandra, Prog. NMR Spectrosc. 40 (2002) 175. [156] T. Gullion, J. Schaefer, J. Magn. Reson. 81 (1989) 196. [197] D. Fushman, R. Varadan, M. Assfalg, O. Walker, Prog. NMR [157] G.T. Montelione, D. Zheng, Y.J. Huang, K.C. Gunsalus, T. Spectrosc. 44 (2004) 189. Szyperski, Nat. Struct. Biol. 7 (2000) 982. [198] M. Blackledge, Prog. NMR Spectrosc. 46 (2005) 23. [158] D. Christendat, A. Yee, A. Dharamsi, Y. Kluger, A. Savchenko, [199] K. Pervushin, A. Ono, C. Ferna´ndez, T. Szyperski, M. Kainosho, K. J.R. Cort, V. Booth, C.D. Mackereth, V. Saridakis, I. Ekiel, G. Wu¨thrich, Proc. Natl. Acad. Sci. USA 95 (1998) 14147. Kozlov, K.L. Maxwell, N. Wu, L.P. McIntosh, K. Gehring, M.A. [200] C.P. Jaroniec, B.A. Tounge, C.M. Rienstra, J. Herzfeld, R.G. Kennedy, A.R. Davidson, E.F. Pai, M. Gerstein, A.M. Edwards, Griffin, J. Am. Chem. Soc. 121 (1999) 10237. C.H. Arrowsmith, Nat. Struct. Biol. 7 (2000) 903. [201] M.A. Kennedy, G.T. Montelione, C.H. Arrowsmith, J.L. Markley, [159] S. Yokoyama, H. Hirota, T. Kigawa, T. Yabuki, M. Shirouzu, T. J. Struct. Funct. Genomics 2 (2002) 155. Terada, Y. Ito, Y. Matsuo, Y. Kuroda, Y. Nishimura, Y. Kyogoku, [202] L. Frydman, T. Scherf, A. Lupulescu, Proc. Natl. Acad. Sci. USA 99 K. Miki, R. Masui, S. Kuramitsu, Nat. Struct. Biol. 7 (2000) 943. (2002) 15858. [160] K.P. Pruessmann, M. Weiger, M.B. Scheidegger, P. Boesiger, Mag. [203] T. Szyperski, D.C. Yeh, D.K. Sukumaran, H.N.B. Moseley, G.T. Reson. Med. 42 (1999) 952. Montelione, Proc. Natl. Acad. Sci. USA 99 (2002) 8009. [161] A.Y. Louie, M.M. Huber, E.T. Ahrens, U. Rothbacher, R. Moats, [204] Y. Shrot, B. Shapira, L. Frydman, J. Magn. Reson. 171 (2004) 163. R.E. Jacobs, S.E.D. De Lange, J.P. Mugler III, J.R. Brookeman, J. [205] G.M. Clore, A.M. Gronenborn, Prog. NMR Spectrosc. 23 (1991) 43. Knight-Scott, J.D. Truwit, C.D. Teates, T.M. Daniel, P.L. Bogorad, [206] W. Gronwald, H.R. Kalbitzer, Prog. NMR Spectrosc. 44 (2004) 33. G.D. Cates, Radiology 210 (1999) 851. [207] T. Herrmann, P. Gu¨ntert, K. Wu¨thrich, J. Biomol. NMR 24 (2002) 171. [162] I. Schnell, H.W. Spiess, J. Magn. Reson. 151 (2001) 153. [208] A. Bax, R. Freeman, S.P. Kempsell, J. Am. Chem. Soc. 102 (1980) [163] A. Brinkmann, M.H. Levitt, J. Chem. Phys. 115 (2001) 357. 4849. [164] Z. Serber, V. Do¨tsch, Biochemistry 40 (2001) 14317. [209] A. Bax, R. Freeman, T.A. Frenkiel, J. Am. Chem. Soc. 103 (1981) [165] F. Castellani, B. van Rossum, A. Diehl, M. Schubert, K. Rehbein, 2102. H. Oschkinat, Nature 420 (2002) 98. [210] A. Bax, R. Freeman, T.A. Frenkiel, M.H. Levitt, J. Magn. Reson. 43 [166] T. Herrmann, P. Gu¨ntert, K. Wu¨thrich, J. Mol. Biol. 24 (2002) 171. (1981) 478.