Latest Developments in NMR

This book is part of the Analytical Spectroscopy Library series, and is devoted to high-resolution NMR, specifically applications in the structure elucidation of organic molecules of moderate molecular weight. The book contains 16 loosely connected chapters written by some of today s most accomplished NMR scientists. Much emphasis has been given to the latest developments in NMR, in particular to selective pulses and pulsed field gradients. 

This section highlights the typical applications of 13C- and 1H-detected INADEQUATE and details a selection of examples from different areas of chemistry. These include primary structure determination of small molecules, the use of partially 13C-enriched compounds in biosynthetic studies, the recent structural analysis of fullerenes and the latest development in NMR hardware that promises to advance the use of high-resolution INADEQUATE experiments for polymers. 

Nuclear Magnetic Resonance (NMR) is one of only a few scientific techniques that have been widely applied in many different areas such as physics, chemistry, biology and medicine. Today, NMR plays a crucial role in structure-function studies of organic and inorganic compounds and of large biomolecules, particularly proteins and DNA. In medicine it is one of the most important imaging techniques available to physicians and it also has extensive applications in pharmaceutical research. In this special issue of NMR of Proteins and Small Biomolecules, review chapters cover a wide-range of topics on some of the latest developments in NMR techniques and their applications. 

Readers new to NMR will find extensive information within the book on the available techniques, allowing full exploration of the many polymer science applications. Readers already established within a branch of NMR will find the book an excellent guide to the practical study of polymers and the interpretation of experimental data. Readers who have specialised in polymer NMR will find the book a valuable dictionary of proven methodologies, as well as a guide to the very latest developments in the subject. 

We expect that with this suite of NMR, GCMS and LCMS based methods we will reveal many novel metabolites. Their identification currently exists as a challenge but we expect to benefit Irom latest developments in hyphenation of separation, enrichment and spectroscopy such as LC-SPE-cryoNMR-MS. 

Solid-state NMR spectroscopy has been demonstrated as a well established technique for characterization of zeolites and other porous materials with respect to structure elucidation, pore architecture, catalytic behaviour and mobility properties. The latest progress in the development of NMR techniques, both with respect to software and hardware improvements, has contributed to the present state of the art for NMR within the field of characterization of zeolitic materials. Furthermore, the introduction of NMR imaging (110), two-dimensional quintuple-quantum NMR spectroscopy (111) and transfer of populations in double resonance (TRAPDOR) NMR (112,113) will extent the horizons of zeolite characterization science. As a final example, the Al => Si TEDOR experiment directly proves, for the first time, that silicon substitutes for phosphorous atoms in the framework of SAPO-37 (114). The Al... 

I hope that this paper could contribute to highlight recent advances in solid-state NMR spectroscopy related to the charactoization of zeolidc materials as well as at the same time presents the latest developments related to new techniques and methods for the zeolite scientists not so familiar with all the details about solid-state NMR spectroscopy. 

During the last decades of the twentieth century, a substantial development of experimental and especially, computational techniques took place. Thus, new measurement methods and mathematical processing of data appeared. This new information is not given anywhere in a comprehensive form and therefore, a lot of people working in this field are not acquainted with it. This book thus fills a substantial gap in this field of science. The book also documents the latest research in molten salt chemistry and brings new results and new insights into the study of molten salt systems using the results of X-ray diffraction and XSAF methods, Raman spectroscopy, and NMR measurements. 

Since the publication of the first edition of this book, there have been many important developments in the field of NMR spectroscopy. These developments have included the award of two Nobel prizes in 2002 to Kurt Wiithrich for his major contributions to biomolecular NMR spectroscopy and in 2003 to Paul C. Lauterbur and Sir Peter Mansfield for their work on MRI, both awards confirming the scientific importance of the general method and its wide application. Consequently, this second edition has been extended to incorporate a number of these pulse sequence developments. Nevertheless, to understand these sophisticated methods it is still necessary that students and newcomers start with the basic experiments and proceed on a step-by-step basis. In this context NMR-SIM is an outstanding, user-friendly simulation program that may be used by both the novice and the expert as an efficient training tool. Therefore, it is no surprise that BRUKER have included NMR-SIM in their latest spectrometer software package TOPSPIN. 

The chapter is organized as follows first are reviewed the force fields developed or improved during the last year making use of NMR data in the parameterization and/or in validation, then we summarize the latest works in combining MD and NMR to study the structure and dynamics of Biomolecules, including proteins, sugars and polysaccharides, lipids. Then we review the papers where the combined approach has been used to study solvent and mixtures, surfaces, and porous materials. 

Carbohydrate NMR spectroscopy has developed rapidly during the last few years and has been reviewed several times.1-9 In this review, predominantly the latest techniques and applications will be reported. The focus is on the measurement and application of coupling constants in the conformational analysis of flexible regions of carbohydrates, such as glycosidic linkages, exocyclic hydroxymethyl, and hydroxyl groups. 

---