Chemical Crystallography with Pulsed Neutrons and Synchroton X-rays PDF
Preview Chemical Crystallography with Pulsed Neutrons and Synchroton X-rays
Chemical Crystallography with Pulsed Neutrons and Synchrotron X-Rays NATO ASI Series Advanced Science Institutes Series A Series presenting the results of activities sponsored by the NA TO Science Committee, which aims at the dissemination of advanced scientific and technological knowledge, with a view to strengthening links between scientific communities. The series is published by an international board of publishers in conjunction with the NATO Scientific Affairs Division A Life Sciences Plenum Publishing Corporation B PhysiCS London and New York C Mathematical D. Reidel Publishing Company and Physical Sciences Dordrecht, Boston, Lancaster and Tokyo D Behavioural and Social Sciences Martinus Nijhoff Publishers E Applied Sciences Dordrecht, Boston and Lancaster F Computer and Systems Sciences Springer-Verlag G Ecological Sciences Berlin, Heidelberg, New York, London, H Cell Biology Paris, and Tokyo Series C: Mathematical and Physical Sciences Vol. 221 Chemical Crystallography with Pulsed Neutrons and Synchrotron X-Rays edited by Maria Armenia Carrondo Centro de Ouimica Estrutural, Instituto Superior Tecnico, Lisboa, Portugal and George A. Jeffrey Department of Crystallography, University of Pittsburgh, Pennsylvania, U.S.A. D. Reidel Publishing Company Dordrecht / Boston / Lancaster / Tokyo Published in cooperation with NATO Scien1ific Affairs Division Proceedings of the NATO Advanced Study Institute on Chemical Crystallography with Pulsed Neutrons and Synchrotron X-Rays Alvor, Algarve, Portugal March 17-27, 1987 Library of Congress Cataloging in Publication Data NATO Advanced Study Institute on Chemical Crystallography with Pulsed Neutrons and Synchrotron X-Rays (1987: Alvor, Portugal) Chemical crystallography with pulsed neutrons and synchrotron X-rays I edited by Maria Armenia Carrondo and George A. Jeffrey. p. cm. - (NATO ASI series. Series C, Mathematical and physical sciences; vol. 221.) "Proceedings of the NATO Advanced SLdy Institute on Chemical Crystallography with Pulsed Neutrons and Synchroton X-Rays, Alvor, Algarve, Portugal, March 17-27, 1987"-t.p. verso. "Published in cooperation with NATO Scientific Affairs Division." Includes index. ISBN-13: 978-94-010-8287-7 e-ISBN-13: 978-94-009-4027-7 001: 10.1007/978-94-009-4027-7 1. Crystallography-4Angresses. 2. Pulsed neutron techniques-Congresses. 3. X-Ray crystallography-Congresses. I. Carrondo, Maria Armenia, 1948- II. Jeffrey, George A., 1915- . III. Title. IV. Series: NATO ASI series. Series C, Mathematical and physical sciences; no. 221. QD951.N38 1987 548'.3--c!c 19 87-26853 CIP Published by D. Reidel Publishing Company P.O. Box 17, 3300 AA Dordrecht, Holland Sold and distributed in the U.S.A. and Canada by Kluwer Academic Publishers, 101 Philip Drive, Assinippi Park, Norwell, MA 02061, U.S.A. In all other countries, sold and distributed by Kluwer Academic Publishers Group, p.o. Box 322, 3300 AH Dordrecht, Holland D. Reidel Publishing Company is a member of the Kluwer Academic Publishers Group All Rights Reserved © 1988 by D. Reidel Publishing Company, Dordrecht, Holland. Softcover reprint of the hardcover 1s t edition 1988 No part of the material protected by this copyright notice may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying, recording or by any information storage and retrieval system, without written permission from the copyright owner. Contents Preface IX G.A. JEFFREY - « Chemical Crystallography: Past, Present and Future» Discussion 7 G.H. LANDER - « Scientific Opportunities With Neutron Scattering" 9 Discussion 25 W.LF. DAVID - « The Scope and Possibilities of Crystallography With Pulsed Neutrons» 27 Discussion 58 B. T.M. WILLIS - « Some Aspects of Diffraction Physics With Pulsed Neutrons» 61 Discussion 75 H. FUESS - « Applications of Neutron Scattering in Chemistry: Pulsed and Continuous Sources in Comparison » 77 Discussion 115 J. B. FORSYTH - « Single Crystal Pulsed Neutron Diffraction» 117 Discussion 134 A. K. CHEETHAM - • Pulsed Neutron Powder Diffraction» 137 Discussion 157 J. D. JORGENSEN - « Pulsed Neutron Diffraction in Special Sample Environments» 159 Discussion 185 A. KVICK - « Applications of Synchrotron X-rays to Chemical CrystallograpllY " 187 Discussion 203 W. SAENGER and - « Synchrotron X-Ray and Neutron Radiation in Protein C. BETZEL CrystallograpllY - Present and Future» 205 Discussion 216 P. J. BECKER - « Synchrotron Radiation For Electron Density Studies» 217 Discussion 244 J. GOULON, M. Laos, - « Structural Applications of X-ray Absorption P. FRIANT, and Spectroscopy (EXAFS and XANES) in Coordination M. RUlz- LOPEZ Chemistry" 247 Discussion 292 A. ALBINATI • « Use of tile Rietveld Profile Analysis for Crystal Structure Determination and Refinement» 295 Discussion 311 J. PANNETIER - « Real-Time Neutron Powder Diffraction" 313 Discussion 355 H. B. STUHRMANN - « Chemical Crystallography With Pulsed Neutrons and SYllcluotron Radiation» %7 Discussion :n5 J. KARLE - « Recent Theoretical Advances in Macromolecular Structure Determina.tion » 379 Discussion 385 vi I.L. KARLE - « Solving Difficult Structures" 419 Discussion 441 C. RIEKEL - « Real Time Synchrotron Radiation Diffraction Experiments on Polymers" 443 Discussion 485 H. D. BARTUNIK - « Time-Resolved Applications of Synchrotron Radiation in Protein Crystallography" 487 Discussion S06 P. LINDLEY - « Crystallographic Studies of Biological Macromolecules Using Synchrotron Radiation" 509 Discussion S36 M. M. HARDING - « The Use of Synchrotron Radiation for Laue Diffraction and for the Study of Very Small Crystals" .537 Discussion .560 FINAL PANEL DISCUSSION S6:~ Posters C. BETZEL et al - « Structure of Proteinase K Using Synchrotron Radiation, and Binding of two Dipeptide Chloromethyl Ketone Inhibithors to the Active Site" 567 C. BETZEL et al - « Protein CrystallograpllY Using Synchrotron Radiation at the EMBL Oustation Hamburg" 568 P. LIGHTFOOT et al - « The Structure of MnP04 .H"!.O by SynclLrotron X-ray Powder Diffraction" 569 E. HOVERSTREYDT et al - « ENDIX - a Computer Program to Simulate Energy Dispersive X-ray and Syncllrotron Powder Diffraction Diagram" 571 R.W. DATE etal - « An Investigation of the Structure and Molecular Ordering of Liquid Crystal Phases" 573 L. VAN MEERVELT et al - « Relation Betwen The Crystalline Structure and the S E Phase of Vinyl - P - (PI - N - H exyloxyphenyl)benzoate " 575 J .A. ALONSO et al - « On TILe Influence of tiLe Non-bonded Pair of Pb(I/) in the Novel Ordered Perovskite Pb[ScodTio.2[,Tefl.2[,)I 0 3 ' 57i 1.A. ALONSO et al - « Synthesis and Crystal Structure of Ta? Te20~ , 579 W. DEPMEIER - « Remarks on the Structures and Pilase Transitions in Aluminate Sodalites " 582 M. PERRIN et al - « Relationship Between CILemical Reactivity and Crystal Structure in the Organic Solid State" 583 P. ESTEBAN et al - « Study by EXAFS of Pt - Ru/ Al203 Catalysts" 585 M. COSTA et al - « Electron Distribution in the Laves Phase, TiFe? " 586 W. T. A. HARRISON et al - « The Structure of Squaric Acid by Powder ~eutron Diffraction" 587 J. RODRIGUEZ et al - « Data Analysis in Time Resolved Powder Diffractometry , 589 J. RODRIGUEZ et al - « Phase Transition; in Sr2C020,.,: A Neutron Diffraction Study" 590 A. GlBAUD - « A Rietveld Profile Analysis Treatment of Line-Bro<l:dening in K AlF4 layered compound" 592 Organizing Committee P. Becker Laboratoire de Cristallographie, C.N.R.S., Grenoble, France M.A. Carrondo t Centro de Qufmica Estrutural Complexo I, Instituto Superior Tecnico Lisboa, Portugal M.B. Hursthouse Department of Chemistry, Queen Mary College, University of London, U.K G.A. Jeffrey t Department of Crystallography University of Pittsburgh, Pittsburgh, U.S.A. G.H. Lander European Institut for Transuranian Elements, Karlsruhe W. Saenger Institur fur Kristallographie, Freie Universitat Berlin, F .R.G. t Co-Directors * We deeply regret the absence of Prof. Simonetta from the Universita. di Milano, Italy, who had agreed to be a member of the Organizing Committee just before his death, in January 1986. Preface X-ray and neutron crystallography have played an increasingly impor- tant role in the chemical and biochemical sciences over the past fifty years. The principal obstacles in this methodology, the phase problem and com- puting, have been overcome. The former by the methods developed in the 1960's and just recognised by the 1985 Chemistry Nobel Prize award to Karle and Hauptman, the latter by the dramatic advances that have taken place in computer technology in the past twenty years. Within the last decade, two new radiation sources have been added to the crystallographer's tools. One is synchrotron X-rays and the other is spallation neutrons. Both have much more powerful fluxes than the pre- vious sources and they are pulsed rather than continuos. New techniques are necessary to fully exploit the intense continuos radiation spectrum and its pulsed property. Both radiations are only available from particular National Laboratories on a guest-user basis for scientists outside these Na- tional Laboratories. Hitherto, the major emphasis on the use of these facilities has been in solid-state physics, and the material, engineering and biological sciences. We believe that there is equivalent potential to applications which are pri- marily chemical or biochemical. We have combined synchrotron X-rays and pulsed spallation neutrons in this ASI for two reasons. One is because they have important common properties such that concepts developped by the instrumental scientists us- ing one radiation could be useful to those using the other. The other reason is that both sources have new major facilities which have very recently be- come operational as for example, the Daresbury and Brookhaven dedicated X-ray synchrotrons and the Rutherford, Argonne and Los Alamos spalla- tion neutron sources. For the near future more sources of both types are planned or in construction in Europe (ESRF), USA (6 GeV synchrotron source), Japan (ALS) and U.K. (ISIS II at RAL). We have therefore brought to this meeting scientists who know the fun- damental properties, advantages and limitations of both the pulsed neu- trons and the synchrotron X-rays to interact with chemists, specially che- mical crystallographers. The majority of these scientists have had no actual experience in using these national facilities. The portuguese and spanish ix x scientific communities, in particular, shoul benefit not only from the lec- tures and tutorials but also from the opportunities to make direc~ contact with some of these instrumental scientists. Since the participants are mainly chemists, the first part of the course had a strong educational component with emphasis on the basic physics involved in the production and use of these radiations. The second part was aimed at discussing these techniques, at the fron- tiers of their applications, such as the exciting potential for real-time struc- tural studies. The book is organised with the lectures in the same sequence as pre- sented. Each lecture was followed by a discussion, the main points of which are summarized after the lecture. Prof. Jeffrey has always showed a great enthusiasm for spreading the knowledge of Chemical Crystallography among young researchers providing they are willing to learn the relevant Physics and Mathematics required to be masters of their science. He deplores the crescent trend towards "black- box" science. This course was designed to overcome this type of deficiency. Prof Jeffrey's long-standing love for Portugal and the Portuguese people, was the "seed" of our association on the organization of this course. The very special climate and scenary of the Algarve, particularly in the early spring, proved to be ideal for the site of the course. Historically the sea was always an inspiration for creative ideias in the human minds. And so it was in the XV century with Infante D. Henrique, son of the Portuguese King D. Joao I, who devoted his life to the great enterprise of the Portuguese discoveries departing from the Algarve. The scientific backgrOund for these explorations was developped in Sagres, in what is now considered as one of the first Naval Research Laboratories, created by D. Henrique. Appropriately, this was chosen as the site of our excursion. We wish to thank the sponsors, NATO Scientific Affairs Division in Brussels, and to Instituto Nacional de Investiga<;ao Cientifica, Junta Na- cional de Investiga<;ao Cientifica e Tecnol6gica and Funda<;ao Calouste Gul- benkian in Lisbon, for their generous contributions. We also thank the Organizing Committee for their help and guidance on the choice of lecturers. We are grateful to Prof. Skyes from Queen Mary
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