ANNUAL REPORTS ON N M R SPECTROSCOPY Edited by E. F. MOONEY Anacon (Instruments) Limited, Bourne End, Buckinghamshire, England Volume 5B ACADEMIC PRESS A Subsidiary of Harcourt Brace Jovanovich, Publishers London and New York 1973 ACADEMIC PRESS INC. (LONDON) LTD. 24-28 Oval Road, London, NW1 7DX US.Edition published by ACADEMIC PRESS INC. 11 1 Fifth Avenue, New York, New York 10003 & 0 1973 by ACADEMIC PRESS INC. (LONDON) LTD. G a y be reproduced in any form by photostat, microfilm, or any other means, without written permission from the publishers Library of Congress Catalog Card Number: 68-17678 ISBN: 0-12-505345-2 PRINTED IN GREAT BRITAIN BY WILLIAM CLOWES & SONS, LIMITED, LONDON, BECCLES AND COLCHESTER ACKNOWLEDGMENTS For permission to reproduce, in whole or in part, certain figures and diagrams we are grateful to the following publishers : American Chemical Society, NorthHolland Publishing Company and JEOL Ltd. Detailed acknowledgments are given in the legends to the figures. PREFACE The division of Volume 5 into two parts is a new venture in this series. It has become evident that these volumes are continually growing. Perhaps correctly, criticism has been made that certain topics are out-weighing the balance of the volumes. This is especially true with such topics as 19F resonance. Certainly had this chapter, which constitutes Volume 5B, been published 6 t h Yolume 5A as one volume the number of pages would have been in cscess of one thousand. Therefore this Volume 5B is in some way an experiment which is reasonable as many would be interested in the 31P data without necessarily wishing to have Volume 5A. This will become especially evident on inspection of the Compound Indices which are exhaustive and basically forming a catalogue of some hundred and ninety pages giving data on various phosphorus compounds. Comments on this new move would be most welcome and it may be more convenient in future years to run the second part of each volume on some special topic such as 19F or 31Presonance studies which, by virtue of the nature of the investigations, tends to become a vast catalogue. \-ohme 6, which is now in preparation, is again a single volume work. I must finally express my gratitude to Professor Mavel for his patience with my editing and for his efforts in preparing the manuscript and producing a very valuable contribution to this series. ERICF. MOONEY -4nacon (Instruments) Ltd, Burkinghamshire, October,1973 (VZ?) T H E CHEMICAL S H I F T SCALES Readers are reminded of the convention for the presentation of chemical shift data i n d u c e d into Volume Three of this series. This self-consistent convention b+s now been used for some two years in various places and is gradually being universally accepted. Convention adopted for Chemical Shift Scales 1. =U1 shifts will be denoted by the delta scale, low-field shifts being shown as positive and high-field shifts as negative values. In all cases the standard m11 take the reference shift of 6 0.0. 2 S o other symbols to denote shifts at infinite dilution will be used. NMR Studies of Phosphorus Compounds ( 1965-1 969) G. MAVEL Ircha-12, Quai Henn' IV, Paris, France I. INTRODUCTION THEIMPORTANCE of NMR in phosphorus chemistry is today not a matter for dispute-this was already clearly evident at the time of writing my earlier review on this to pi^."^^^*^) This earlier review was concerned with nearly four hundred and fifty publications from the early days of NMR (about 1950) until the end of 1965. Papers specifically restricted to 31P data were not included but these were, however, reviewed by Van Wazer d U Z . ( ~ ~ ~ 'l) * who at approximately the same time presented results for about three thousand compounds. The years 1966