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Structure Determination from Powder Diffraction Data W INTERNATIONAL UNION OF CRYSTALLOGRAPHY BOOK SERIES lUCr BOOK SERIES COMMITTEE E. N. Baker, New Zealand J. Bernstein, Israel P. Coppens, USA G. R. Desiraju, India E. Dodson, UK A. M. Glazer, UK J. R. Helliwell, UK P. Paufler, Germany H. Schenk (Chairman), The Netherlands ILJCr Monographs on Crystallography 1 Accurate molecular structures A. Domenicano, I. Hargittai, editors 2 P. P. Ewald and his dynamical theory of X-ray diffraction D. W. J. Cruickshank, H. J. Juretschke, N. Kato, editors 3 Electron diffraction techniques, Vol. 1 J. M. Cowley, editor 4 Electron diffraction techniques, Vol. 2 J. M. Cowley, editor 5 The Rietveld method R. A. Young, editor 6 Introduction to crystallographic statistics U. Shmueli, G. H. Weiss 7 Crystallographic instrumentation L. A. Aslanov, G. V. Fetisov, G. A. K. Howard 8 Direct phasing in crystallography C. Giacovazzo 9 The weak hydrogen bond G. R. Desiraju, T. Steiner 10 Defect and microstructure analysis by diffraction R. L. Snyder, J. Fiala and H. J. Bunge 11 Dynamical theory of X-ray diffraction A. Authier 12 The chemical bond in inorganic chemistry I. D. Brown 13 Structure determination from powder diffraction data W. I. F. David, K. Shankland, L. B. McCusker, Ch. Baerlocher, editors 14 Polymorphism in molecular crystals J. Bernstein 15 Crystallography of modular materials G. Ferraris, E. Makovicky, S. Merlino 16 Diffuse x-ray scattering and models of disorder T. R. Welberry 17 Crystallography of the polymethylene chain: an inquiry into the structure of waxes D. L. Dorset 18 Crystalline molecular complexes and compounds: structure and principles F. H. Herbstein 19 Molecular aggregation: structure analysis and molecular simulation of crystals and liquids A. Gavezzotti ILJCr Texts on Crystallography 1 The solid state A. Guinier, R. Julien 4 X-ray charge densities and chemical bonding P. Coppens 5 The basics of crystallography and diffraction, second edition C. Hammond 6 Crystal structure analysis: principles and practice W. Clegg, editor 7 Fundamentals of crystallography, second edition C. Giacovazzo, editor 8 Crystal structure refinement: a crystallographer's guide to SHELXL P. Miiller, editor Structure Determination from Powder Diffraction Data Edited by W. I. F. DAVID Rutherford Appleton Laboratory, Oxfordshire, UK K. SHANKLAND Rutherford Appleton Laboratory, Oxfordshire, UK L. B. McCUSKER Laboratory of Crystallography, ETH Zurich, Switzerland Ch. BAERLOCHER Laboratory of Crystallography, ETH Zurich, Switzerland OXFORD UNIVERSITY PRESS OXFORD UNIVERSITY PRESS Great Clarendon Street, Oxford OX2 6DP Oxford University Press is a department of the University of Oxford. It furthers the University's objective of excellence in research, scholarship, and education by publishing worldwide in Oxford New York Auckland Cape Town Dar es Salaam Hong Kong Karachi Kuala Lumpur Madrid Melbourne Mexico City Nairobi New Delhi Shanghai Taipei Toronto With offices in Argentina Austria Brazil Chile Czech Republic France Greece Guatemala Hungary Italy Japan Poland Portugal Singapore South Korea Switzerland Thailand Turkey Ukraine Vietnam Oxford is a registered trade mark of Oxford University Press in the UK and in certain other countries Published in the United States by Oxford University Press Inc., New York © Oxford University Press 2002 The moral rights of the author have been asserted Database right Oxford University Press (maker) First published 2002 First published in paperback 2006 All rights reserved. No part of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, without the prior permission in writing of Oxford University Press, or as expressly permitted by law, or under terms agreed with the appropriate reprographics rights organization. Enquiries concerning reproduction outside the scope of the above should be sent to the Rights Department, Oxford University Press, at the address above You must not circulate this book in any other binding or cover and you must impose the same condition on any acquirer British Library Cataloguing in Publication Data Data available Library of Congress Cataloging in Publication Data Structure determination from power diffraction data/edited by W. I. F. David ... [et al.]. p. cm—(lUCr monographs on crystallography; 13) Includes bibliographical references and index. 1. X-ray crystallography. 2. Crystals—Structures. 3. Powders— Measurement. I. David, W. I. F. (William I. F.) II. International Union of Crystallography monographs on crystallography; 13. QD945.S88 2002 548—dc21 2001047555 Typeset by Newgen Imaging Systems (P) Ltd., Chennai, India Printed in Great Britain on acid-free paper by Biddies Ltd., King's Lynn ISBN 0-19-850091-2 978-0-19-850091-9 ISBN 0-19-920553-1 (Pbk.) 978-0-19-920553-0 (Pbk.) 13579 10 864 2 Preface to the Paperback Edition In the few years that have elapsed since this book first appeared in hardback, structure determination from powder diffraction data (SDPD) methods have been refined and accepted into the structural communities as a powerful alter- native for use when single-crystal diffraction methods are not appropriate. This is clearly reflected in the number of papers being published that involve the use of SDPD and it is particularly gratifying to see SDPD-derived structures appearing regularly in volumes of Act a Crystallogr. B, C, and E, confirming the truly routine nature of the technique in many instances. This surely also reflects the fact that instrumental developments, both in laboratories and at synchro- tron sources, have made measuring very high-quality X-ray powder diffraction data easier than ever before. Many of the more recent developments in methods, algorithms and computer programs are covered in a special issue of Zeitschrift Fur Kristallographie (volume 219,12,2004) which is dedicated to the subject of SDPD. It is probably true to say that the majority of developments have been incremental rather than revolutionary; there has been no step change in the level of structural com- plexity that can be tackled as a result of the introduction of, for example, novel optimisation methods, new evaluation functions or the closer coupling of direct methods/global optimisation. The change in complexity represented by the study of protein structures using powder diffraction still lies more in the domain of structure refinement than determination but regardless, it represents an exciting new research topic. Preface The art of solving a structure from powder diffraction data has developed rapidly over the last ten years. Prior to 1990, very few unknown crystal struc- tures had been determined directly from powder diffraction data, and each structure solved could be regarded as a tour de force of ingenuity and perse- verance. Today, the situation is quite different and numerous crystal structures, both organic and inorganic, have been solved from powder data. Developments in instrumentation, computer technology and powder diffraction methodology have all contributed to this increased success rate. However, the route to a successful structure determination is still by no means as straightforward and routine as it is with single-crystal diffraction data. In the chapters that follow, experts in the field discuss both the fundamental and applied aspects of structure solution from powder diffraction data. The process is sequential, with any particular stage depending crucially on the successful completion of all the previous steps, and the ordering of the chapters within the book essentially reflects this flow. Although the Rietveld method of structure refinement from powder diffraction data is often loosely considered to be synonymous with structure determination, it is not. The Rietveld method only comes into play in the final stage of the structure solution process when an approximate structural model has been found. The subject of this book is how that structural model is determined. Despite the sequential nature of the structure determination process, there are nevertheless various paths that can be taken through it. The art of structure solution from powder diffraction data lies not only in the correct application of a specific technique or computer program, but also in the selection of the optimal path for the problem at hand. The limitations inherent to the data available and to each of the methods used must be recognized. This book is designed to help the reader find his or her way through the maze of possibilities. Readers will find that while every effort has been made to ensure that the chapters present a consistent and coherent approach to structure determination, no attempt has been made to gloss over differences of opinion, as expressed by individual authors, regarding the benefits or limitations of particular methods. This is particularly apparent in the case of the key step of intensity extraction, PREFACE vii where the relative merits of the Pawley and Le Bail methods are raised in several chapters. Such differences are, however, minor and should not overly concern the reader. Indeed, probably the most significant legacy of the past decade lies in the diversity of methods that have been developed. William I. F. David Kenneth Shankland Lynne B. McCusker Christian Baerlocher This page intentionally left blank Contents List of contributors xvii 1 Introduction William I. F. David, Kenneth Shankland, Lynne B. McCusker and Christian Baerlocher 1 1.1 Crystal structures from powder diffraction data 1 1.2 The structure determination process 4 1.3 Adapting single-crystal
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