Basic one- and two-dimensional NMR spectroscopy. Wiley-VCH, Weinheim, 1998, 3rd edn, 386 pp. Price...

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MAGNETIC RESONANCE IN CHEMISTRY Magn. Reson. Chem. 2001; 39: 656 Book Review HORST FRIEBOLIN Basic one- and two-dimensional NMR spectroscopy Wiley-VCH, Weinheim, 1998, 3rd edn, pp. 386, Price DM 72. ISBN 3 527 29513 5 This book is a slightly revised and extended version of the second edition published in 1993. The aim and organization of the book remain unchanged. The book consists of 14 reasonably well balanced chapters. In the first chapter (The Physical Basis of NMR Spectroscopy, 41 pp.), the reader is given a short summary of the basic principles of NMR focusing on pulsed FT methods and important spectral parameters. Chapters 2 (41 pp.) and 3 (22 pp.) describe the charac- teristic 1 H and 13 C NMR chemical shifts of organic compounds, and also indirect H,H and C,H spin–spin couplings. Both chap- ters give practical and detailed advice on how to extract structural and stereochemi- cal information from these data. Chapter 4 (Spectrum Analysis and Calculation, 16 pp.) summarizes the spectral information obtain- able from spectra, and introduces the nomen- clature of spin systems. I think it would have been better to have incorporated this section into Chapter 1. Chapter 5 (Double Resonance Experi- ments, 9 pp.) is rather outdated, discussing techniques such as off-resonance, selective 13 C decoupling, etc., that have only histori- cal significance. In Chapter 6 (Assignment of 1 H and 13 C Signals, 20 pp.), the traditional approach based on empirical substituent effects, and utilization of data basis are described. Chapter 7 (18 pp.) is devoted to an introduction of T 1 and T 2 relaxations uti- lizing a vector description of the phenomena. Chapter 8 (One-dimensional NMR Exper- iments Using Complex Pulse Sequences, 48 pp.) has been substantially extended with an introductory discussion of the principles of the pulsed field gradient technique. Even the efficiency of the pulsed gradient spin- echo experiment is emphasized for studying diffusion, but without mentioning the rel- evant name DOSY. The high efficiency of the selective TOCSY experiment is lucidly demonstrated on an interesting example. A unique and comprehensive introduction to the power of modern two-dimensional NMR methods (2D J-resolved NMR, C,H- COSY, H,H-COSY, proton detected H,C- correlated methods HSQC, HMQC and HMBC, and also TOCSY, NOESY, EXSY and INADEQUATE) in structure chemistry is given in Chapter 9 (55 pp.). The section on COSY is slightly disappointing, failing to reflect the importance of phase sen- sitive double (multiple) quantum filtered experiments, but discussing the outdated long-range COSY. Unfortunately, no exam- ples of the indispensable, currently more often used ROESY experiments are shown. Chapter 10 (13 pp.) treats the nuclear Over- hauser effect. The NOE has proven to be of fundamental importance in the struc- tural analysis of organic compounds. A major improvement over classical differ- ence NOE spectroscopy was introduced by the inclusion of ‘double pulsed field gradi- ent selective excitation,’ resulting ultra-high- quality NOE spectra. It is disappointing to note that the author missed incorporating this powerful, new DPFGSE NOE experi- ment, which recently replaced the traditional 1D NOE difference spectroscopy. Chap- ters 11, 12 and 13 (Dynamic NMR Spec- troscopy, 28 pp.; Shift Reagents, 10 pp.; and Macromolecules, 7 pp.) are unchanged from the previous edition. The last chap- ter (NMR Spectroscopy in Biochemistry and Medicine, 22 pp.) offers an interesting out- look on some applications of NMR in the field of biochemistry and medical diagnosis (MRI). The book is based mainly on a traditional approach, and the techniques are explained wherever possible by means of vector dia- grams, showing in a clear way what happens as a result of applying the different pulses. However, considering the large number of methods, a short introductory description of the quantum mechanical approach apply- ing matrix operators would have been really desirable. In summary, this book is written in a very clear way and is enhanced by many instructive figures and examples. It provides an excellent introduction to practical liquid- state NMR. A further attractive feature is the reasonable price. I consider that the book can be highly recommended for graduate students and also for researchers in organic chemistry, for whom NMR is a common and indispensable method. abor T ´ oth Budapest University of Technology and Economics, Budapest, Hungary [DOI: 10.1002/mrc.889] Copyright 2001 John Wiley & Sons, Ltd.

Transcript of Basic one- and two-dimensional NMR spectroscopy. Wiley-VCH, Weinheim, 1998, 3rd edn, 386 pp. Price...

MAGNETIC RESONANCE IN CHEMISTRYMagn. Reson. Chem. 2001; 39: 656

Book Review

HORST FRIEBOLIN

Basic one- and two-dimensional NMRspectroscopy

Wiley-VCH, Weinheim, 1998, 3rd edn, pp. 386,Price DM 72. ISBN 3 527 29513 5

This book is a slightly revised and extendedversion of the second edition published in1993. The aim and organization of the bookremain unchanged. The book consists of 14reasonably well balanced chapters. In thefirst chapter (The Physical Basis of NMRSpectroscopy, 41 pp.), the reader is givena short summary of the basic principles ofNMR focusing on pulsed FT methods andimportant spectral parameters. Chapters 2(41 pp.) and 3 (22 pp.) describe the charac-teristic 1H and 13C NMR chemical shifts oforganic compounds, and also indirect H,Hand C,H spin–spin couplings. Both chap-ters give practical and detailed advice onhow to extract structural and stereochemi-cal information from these data. Chapter 4(Spectrum Analysis and Calculation, 16 pp.)summarizes the spectral information obtain-able from spectra, and introduces the nomen-clature of spin systems. I think it would havebeen better to have incorporated this sectioninto Chapter 1.

Chapter 5 (Double Resonance Experi-ments, 9 pp.) is rather outdated, discussingtechniques such as off-resonance, selective13C decoupling, etc., that have only histori-cal significance. In Chapter 6 (Assignment of1H and 13C Signals, 20 pp.), the traditionalapproach based on empirical substituenteffects, and utilization of data basis are

described. Chapter 7 (18 pp.) is devoted toan introduction of T1 and T2 relaxations uti-lizing a vector description of the phenomena.Chapter 8 (One-dimensional NMR Exper-iments Using Complex Pulse Sequences,48 pp.) has been substantially extended withan introductory discussion of the principlesof the pulsed field gradient technique. Eventhe efficiency of the pulsed gradient spin-echo experiment is emphasized for studyingdiffusion, but without mentioning the rel-evant name DOSY. The high efficiency ofthe selective TOCSY experiment is lucidlydemonstrated on an interesting example.A unique and comprehensive introductionto the power of modern two-dimensionalNMR methods (2D J-resolved NMR, C,H-COSY, H,H-COSY, proton detected H,C-correlated methods HSQC, HMQC andHMBC, and also TOCSY, NOESY, EXSYand INADEQUATE) in structure chemistryis given in Chapter 9 (55 pp.). The sectionon COSY is slightly disappointing, failingto reflect the importance of phase sen-sitive double (multiple) quantum filteredexperiments, but discussing the outdatedlong-range COSY. Unfortunately, no exam-ples of the indispensable, currently moreoften used ROESY experiments are shown.Chapter 10 (13 pp.) treats the nuclear Over-hauser effect. The NOE has proven to beof fundamental importance in the struc-tural analysis of organic compounds. Amajor improvement over classical differ-ence NOE spectroscopy was introduced bythe inclusion of ‘double pulsed field gradi-ent selective excitation,’ resulting ultra-high-quality NOE spectra. It is disappointing tonote that the author missed incorporating

this powerful, new DPFGSE NOE experi-ment, which recently replaced the traditional1D NOE difference spectroscopy. Chap-ters 11, 12 and 13 (Dynamic NMR Spec-troscopy, 28 pp.; Shift Reagents, 10 pp.;and Macromolecules, 7 pp.) are unchangedfrom the previous edition. The last chap-ter (NMR Spectroscopy in Biochemistry andMedicine, 22 pp.) offers an interesting out-look on some applications of NMR in thefield of biochemistry and medical diagnosis(MRI).

The book is based mainly on a traditionalapproach, and the techniques are explainedwherever possible by means of vector dia-grams, showing in a clear way what happensas a result of applying the different pulses.However, considering the large number ofmethods, a short introductory description ofthe quantum mechanical approach apply-ing matrix operators would have been reallydesirable.

In summary, this book is written in avery clear way and is enhanced by manyinstructive figures and examples. It providesan excellent introduction to practical liquid-state NMR. A further attractive feature is thereasonable price. I consider that the bookcan be highly recommended for graduatestudents and also for researchers in organicchemistry, for whom NMR is a common andindispensable method.

Gabor TothBudapest University of Technology and

Economics, Budapest, Hungary

[DOI: 10.1002/mrc.889]

Copyright 2001 John Wiley & Sons, Ltd.