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Topics in carbon-13 NMR spectroscopy
BOOK REVIEWS
541
polarized nuclear targets for the study of the spin dependence of nuclear interactions. Willis Lamb tells about “Five Encounters with Felix Bloch,” several of which are related to the early development of NMR. John Roberts gives a fairly extensive and detailed review of work in his group on natural-abundance nitrogen15 NMR spectroscopy of organic molecules. In addition to the sections mentioned, there are another ten contributions dealing primarily with various aspects of the structure of solids not related to magnetic resonance. Perhaps the most interesting and valuable feature of the book is the incorporation in many of the sections of personal and historical sidelights on Bloch’s personality and approach to research. A biography of Bloch, written by the editors, introduces the volume. W.S.B.
Topics in Carbon-13 NMR Spectroscopy, Vol. 3, edited by George C. Levy. John Wiley, New York, 1979. 397 pages. $35.00. Chapter 1 of the third volume in this series contains six sections on experimental techniques contributed by experts in the respective areas of spin decoupling, sensitivity optimization, m icro samples, large-sample probes, software, two-dimensional FT, variation of temperature, and pulsed excitation methods. By no means comprehensive, these articles afford considerable insight into applicable methods and provide help for the potential user of these methods. Chapter 2 describes applications of carbon-13 spin relaxation measurements and the additional information to be gained from analysis of cross-correlation and internal rotation effects. The bibliography is extensive. In Chapter 3, Eliel and Pietrusiewicz consider in detail data on nonaromatic heterocyclic compounds. This is a comprehensivereview, with complete bibliography through 1977, omitting, however, natural products. Monocyclic rings are discussed in order of size, and polycyclic rings are then considered more briefly. Principal emphasis is on chemical shifts, but some information on coupling constants and relaxation times is also included. Chapters 4 and 5 are devoted to accounts of the study of solid and semisolid materials. Schaefer and Stejskal review line-narrowing techniques and cross-polarization methods and describe their cross-polarization spectrometer. Applications of these “high-resolution” methods to carbon-13 spectra of poly(phenylene oxide), drawn crystalline polyethylene, biological solids, poly(methy1 methacrylate), and polycarbonates are described. An interesting aspect of these results is that certain conformational differences which are not distinguishable in solution are locked in by the environment in the solid polymer. Torchia and VanderHart show how similar techniques can be employed for studying biological macromolecules. Examples cited are the proteins elastin and collagen, the proteoglycans in cartilage, hemoglobin S, and unsonicated phospholipid bilayers. In Chapter 6, Moniz, Poranski, and Sojka consider mechanistic and kinetic applications of carbon- 13 CIDNP. Techniques for using the method and for analyzing the results are described.
542
BOOK REVIEWS
This volume contains a great deal of useful information, of immediate help to the investigator wishing to design various experiments. It is unfortunately marred by a larger than usual number of typographical errors. Pages 2 and 3 get the volume off to a poor start with lines of type repeated, a plural verb with singular subject, and Dr. Overhauser’s name uncapitalized. On page 297, the results of an analysis of spin-locking versus adiabatic demagnetization in the rotating frame as cross-polarization methods are garbled by an obvious typographical error. On page 372, some “greater than” signs appear to have been disconcertingly reversed. Furthermore, it is not clear why, when space is at a premium, all of page 110 is devoted to writing out the equations derived by Grant and Werbelow for the correlation functions of an asymmetric rotor without using or discussing them further. W.S.B.
541
polarized nuclear targets for the study of the spin dependence of nuclear interactions. Willis Lamb tells about “Five Encounters with Felix Bloch,” several of which are related to the early development of NMR. John Roberts gives a fairly extensive and detailed review of work in his group on natural-abundance nitrogen15 NMR spectroscopy of organic molecules. In addition to the sections mentioned, there are another ten contributions dealing primarily with various aspects of the structure of solids not related to magnetic resonance. Perhaps the most interesting and valuable feature of the book is the incorporation in many of the sections of personal and historical sidelights on Bloch’s personality and approach to research. A biography of Bloch, written by the editors, introduces the volume. W.S.B.
Topics in Carbon-13 NMR Spectroscopy, Vol. 3, edited by George C. Levy. John Wiley, New York, 1979. 397 pages. $35.00. Chapter 1 of the third volume in this series contains six sections on experimental techniques contributed by experts in the respective areas of spin decoupling, sensitivity optimization, m icro samples, large-sample probes, software, two-dimensional FT, variation of temperature, and pulsed excitation methods. By no means comprehensive, these articles afford considerable insight into applicable methods and provide help for the potential user of these methods. Chapter 2 describes applications of carbon-13 spin relaxation measurements and the additional information to be gained from analysis of cross-correlation and internal rotation effects. The bibliography is extensive. In Chapter 3, Eliel and Pietrusiewicz consider in detail data on nonaromatic heterocyclic compounds. This is a comprehensivereview, with complete bibliography through 1977, omitting, however, natural products. Monocyclic rings are discussed in order of size, and polycyclic rings are then considered more briefly. Principal emphasis is on chemical shifts, but some information on coupling constants and relaxation times is also included. Chapters 4 and 5 are devoted to accounts of the study of solid and semisolid materials. Schaefer and Stejskal review line-narrowing techniques and cross-polarization methods and describe their cross-polarization spectrometer. Applications of these “high-resolution” methods to carbon-13 spectra of poly(phenylene oxide), drawn crystalline polyethylene, biological solids, poly(methy1 methacrylate), and polycarbonates are described. An interesting aspect of these results is that certain conformational differences which are not distinguishable in solution are locked in by the environment in the solid polymer. Torchia and VanderHart show how similar techniques can be employed for studying biological macromolecules. Examples cited are the proteins elastin and collagen, the proteoglycans in cartilage, hemoglobin S, and unsonicated phospholipid bilayers. In Chapter 6, Moniz, Poranski, and Sojka consider mechanistic and kinetic applications of carbon- 13 CIDNP. Techniques for using the method and for analyzing the results are described.
542
BOOK REVIEWS
This volume contains a great deal of useful information, of immediate help to the investigator wishing to design various experiments. It is unfortunately marred by a larger than usual number of typographical errors. Pages 2 and 3 get the volume off to a poor start with lines of type repeated, a plural verb with singular subject, and Dr. Overhauser’s name uncapitalized. On page 297, the results of an analysis of spin-locking versus adiabatic demagnetization in the rotating frame as cross-polarization methods are garbled by an obvious typographical error. On page 372, some “greater than” signs appear to have been disconcertingly reversed. Furthermore, it is not clear why, when space is at a premium, all of page 110 is devoted to writing out the equations derived by Grant and Werbelow for the correlation functions of an asymmetric rotor without using or discussing them further. W.S.B.