Phosphorus-31 Nmr Spectral Properties in

This is a methods-oriented book, which contains enormous amounts of information on 31P NMR, in a concise and well-edited format. It is an invaluable resource for every NMR spectroscopist. This book consists of 33 chapters, which together 'constitute a compendium that will be of optimal utility to the majority of 31P NMR spectroscopy users as well as to those perhaps not as familiar with the technique but curious about potential applications in their own research.' (From the editors' preface) There have been a number of new developments in NMR techniques in the 6 years since Verkade and Quin edited the first, successful book on 31P NMR. This new book does not supersede the previous book; it offers a wide cross-section of recent research. Compard to the first, basic, grounding volume, this book presents more results (it is more applied); it directly reflects a more mature science. Arguably, VCH has published the best NMR books in recent years (Neuhaus/Williamson, Croasmun/Carlson, etc.). This new addition to VCH's NMR list ensures the continued visibility and excellence of VCH in this field.

Louis D. Quin, PhD, is Distinguished Visiting Professor in the Department of Chemistry at the University of North Carolina at Wilmington, and James B. Duke Professor Emeritus at Duke University and Professor Emeritus at the University of Massachusetts.

John G. Verkade, PhD, is a professor at Iowa State University. In 1994 he and one of his graduate students were national winners of the BF Goodrich Collegiate Team Inventors Award for work on their patented superbase catalysts. In 1995 he won the Iowa State University LAS College Award for Excellence in Research. He has served as chairman of the Editorial Board of Chemical and Engineering News, and as an associate editor of Phosphorus, Sulfur and Silicon.

Contributors

I. Chemical Shift Theory

1. Ab Initio Calculations of Phosphorus Chemical Shielding

D. B. Chesnut and B. E. Rusiloski

II. Conformational Analysis of Phosphorus-Containing Ring Systems

2. Application of Various 31P NMR Techniques in Conformational Studies of 1,3-Dithianes and Their Oxoand Seleno-Analogues Containing Organophosphorus Substituents at the Anomeric Carbon Atom

Marian Mikolajczyk and Piotr P. Graczyk

3. Phosphorus (III) and Phosphorus (V) Heterocyclic Compounds

Robert R. Holmes, T. K. Prakasha, and Stephen D. Pastor

4. Use of JHP Values to Determine the Conformations of Saturated Six-Membered Rings Containing Phosphorus

Wesley G. Bentrude

III. Compounds with Three-, Four-, and Five-Coordinate Phosphorus (Saturated)

5. Elucidation of Small Ring and Macrocycle Structures Using 31P NMR

Jean-Pierre Majoral, Anne-Marie Caminade, and Alain Igau

6. 1λ5,3λ5-Diphosphetes and Phosphorus-Fluoro-Ylides

Ekkehard Fluck and Gernot Heckmann

7. Identification and Structural Elucidation of the Novel Polyphosphide LiH5P8

Marianne Baudler, Doris Düster, and Rudolf Heumüller

8. NMR Studies of Phosphorus-Substituted Allenes, Acetylenes, and Dienes

Robert H. Neilson, William R. Kucera, and Christo M. Angelov

9. Applications of 31P NMR Spectroscopy in Cyclophosphazene Chemistry

Christopher W. Allen

10. 31p, 13C, and 15N NMR Studies of Aryl-Substituted λ5-Phosphazenes, Phosphine Oxides, and Phosphines 115 Martin Pomerantz

IV. Low-Coordinate Phosphorus Compounds

11. From Donor-Stabilized Metaphosphate Derivatives to Heterocyclic Phosphorus Compounds Using NMR as a Guide

Manfred Meisel, Jutta Pauli, and Christiane Donath

12. The Cyclotetramerization of Phosphaalkynes and Its 31p NMR Spectroscopic Consequences

Manfred Regitz, Bernhard Breit, and Holger Memmesheimer

13. 31P NMR Spectroscopic Investigations of Low-Coordinated Multiple Bonded PN Systems

Edgar Niecke and Dietrich Gudat

14. 31P NMR in Studies of Some One- and Two-Coordinate Phosphorus Compounds

Masaaki Yoshifuji

15. The Bis(Diisopropylamino)Phosphino Group: A Wonderful Tool For the Stabilization and NMR Characterization of Highly Reactive Species

Robert W. Reed and Guy Bertrand

V. Metal Complexes of Phosphorus Ligands

16. Transition Metal-Promoted Intramolecular [4 + 2] DielsAlder Cycloadditions of Phospholes with Dienophilic Ligands

John H. Nelson

17. Applications of 31P NMR Spectroscopy in the Investigation of the Dynamic Behavior of Five-Membered EtherPhosphine Metal Complexes

Ekkehard Lindner, Hermann August Mayer, and Andrea Möckel

18. 31P NMR Studies on Transition-Metal Complexes Derived from Phosphaalkynes, Phosphirenes, and Phosphiranes

Florence A. Ajulu, Rainer Bartsch, Duncan Carmichael, Julian A. Johnson, Cameron Jones, Robson M. Matos, and John F. Nixon

19. Applications of 31P Shift and P-P Coupling Data in the Chemistry of Organometallics Containing Two or More Phosphorus Atoms

Alan N. Hughes

VI. Biological Phosphorus Systems

20. Stereochemical Analysis of Chiral Inorganic [16O, 17O, 18O]-Thiophosphate

Gordon Lowe

21. 31P NMR of Nucleic Acids 267

David G. Gorenstein

22. 31P NMR in the Analysis of Extracted Tissue Phospholipids

Thomas Glonek

VII. Mechanism Elucidation in Phosphorus Chemistry

23.31P NMR Detection and Analysis of Wittig Intermediates

E. Vedejs and C. F. Marth

24. Applications of Oxygen Isotopes and 31P NMR Spectroscopy in Stereochemical and Mechanistic Studies

Paul M. Cullis

25. Reversible Coordination Isomerism of Organophosphorus Compounds

Leonid N. Markovsky, Vitaly I. Kalchenko, and Mark I. Povolotsky

VIII. Analytical and Interpretive Aspects

26. P-P and P-H Correlation Experiments for the Analysis of Mixtures of Phosphorus Compounds

Martin Murray

27. Industrial 31P NMR Spectroscopy: Advances and Applications

Janice K. Gard

28. 31P NMR Spectroscopy in the Analysis of Coal Materials

John G. Verkade

29. Fully Coupled Spectra in the Analysis of Reaction Mixtures

Michael J. Gallagher

30. NMR-Controlled Titrations of Phosphorus-Containing Acids and Bases in Protolysis and Complex Formation

Gerhard Hägele

IX. NMR with Solid Phosphorus-Containing Systems

31. 31P High-Resolution Solid-State NMR Studies of Thiophosphoroorganic Compounds

Marek J. Potrzebowski and Jan Michalski

32. Characterization by CP/MAS 31P NMR of Solids Used as Trapping Agents for Transient, Electrophilic Phosphorus Species

Louis D. Quin

33. Magic-Angle Spinning Frequency-Dependent NMR Spectra Arising from a Pair of Crystallographically Equivalent Phosphorus Nuclei

Gang Wu, Klaus Eichele, and Roderick E. Wasylishen

Index

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Phosphorus-31 Nmr Spectral Properties in Compound Characterization and Structural Analysis

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Table of Contents

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