ISSN 1467-2790 CRYSTALLOGRAPHY NEWS British Crystallographic Association

No.78 September 2001

BCA Spring Meeting 2002

Dorothy Hodgkin - RSC Landmark

Fibre Diffraction

Crystallography and Antiquities

2001 Walter Hälg Prize

Quarterly Book Reviews

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Contents September 2001 Contents BCA Administrative Office, Northern Networking Ltd, Bellway House, From the President ...... 2 813 South Street, Glasgow G14 0BX, Scotland, UK Council Members ...... 3 Tel: + 44 141 954 4441 Fax: + 44 141 954 2656 From the Editor ...... 4 e-mail: [email protected] BCA Spring Meeting 2002 ...... 4

NEXT ISSUE OF People in the News ...... 5 CRYSTALLOGRAPHY NEWS Presentation of the Royal Society of Chemistry CRYSTALLOGRAPHY NEWS is published quarterly (March, June, Landmark to Commemorate the Work of September and December) by the Dorothy Crowfoot Hodgkin ...... 6 British Crystallographic Association. MSword97 Fibre Diffraction: highlights for X-rays, documents (or earlier versions) may be sent on a PC disk or neutrons and CCP13 ...... 8 electronically, (only small files < 500K please, image formats JPEG, Crystallography and Antiquities ...... 10 GIF). Items may include technical articles, news about people (e.g. The dehydration of -lactose monohydrate ...... 13 awards, honours, retirements α etc.), reports on past meetings of interest to crystallographers, Book Reviews ...... 14 notices of future meetings, historical reminiscences, letters to Meeting Reports ...... 16 the editor, book, hardware or software reviews. Please ensure that items for inclusion in the Forthcoming BCA Meetings ...... 20 December 2001 issue are sent to the Editor to arrive before 26th Other Meetings of Interest ...... 21 October 2001. Corporate Members ...... 22 JO JUTSON, Tel: (01691) 671033 The 2001 Walter Hälg Prize ...... 23 EDITOR CRYSTALLOGRAPHY NEWS, 4, Henlle Gardens, Gobowen, PCG/SCMPG Bursaries ...... 23 Oswestry, Shropshire, SY11 3NU. e-mail: [email protected] CLRC e-Science Centre to run UK Grid Support Centre ...... 24

The British Crystallographic Association Size Strain - III Meeting ...... 24 is a Registered Charity (#284718) Mineralogy Database ...... 24

1 From the President September 2001

The conference season is upon us, science, but it seems to me that President’s Remarks and even in non-crystallographic the excitement is increasing and meetings, crystallography is not in any way diminishing. everywhere to be seen. I was at a Despite our many reservations Gordon Conference on 3-D about the way in which Electron Microscopy in Rhode government and others handle Island in June ( I was one of just and manage science, it is a great three crystallographers!), and was time to be a crystallographer. amazed at the work in which low resolution particles whose shape Our own spring meeting has to was determined by single particle reflect all this, and the organisers electron microscopy studies were of our next meeting in filled with structures taken from Nottingham have done a splendid the protein data bank thus giving job: the plenary session is devoted a model of macromolecular to structure solution and phasing assemblies at an atomic as applied to all systems from resolution. Studies of muscle small molecules to contraction, for example, at this macromolecular assemblies using level are simply astonishing, and both single crystals and powders. the microscopists have their sights There are sessions on DNA set on whole cells and organelles recombination and repair, at a similar resolution. polymorphism, drugs and disease, Reitveld refinement, detectors, Other developments proceed thin films, crystallisation, apace: powder diffraction can education and the formation of a now relatively routinely solve new special interest group structures ten times the size of devoted to the Diamond facility. those 5 years ago, especially Many of these sessions will take organic molecules even using the form of workshops. Every laboratory data; the flood of attempt has been made to keep biological macromolecule costs to a minimum, and the structures continues unabated Nottingham campus is a (More than 14000 new structures delightful place. How can anyone were deposited in the protein resist? data bank last year.); data collection hardware continues to I hope to see many of you at the improve and computing has Krakov ECM Meeting at the end become a minor cost. of August. ECM conferences also Crystallographic software reflect the scope and diversity of becomes increasingly 21st century crystallography as sophisticated and easier for non- well as the BCA Spring Meetings. Cover pictures left to right: experts to use (although this has X-ray diffraction image of normal breast obvious dangers). Diamond, the tissue. new synchrotron, is on the way, 2Fo-Fc map calculated from cellulose II. and plans are afoot for a new

Detail of Middle Kingdom coffin from El neutron spallation source; these Bersheh. will keep the UK in the forefront Chinese underglaze-blue porcelain dish, of crystallographic technology for mid-14th century, Yuan Dynasty. the next decade. Crystallography Chris Gilmore Dorothy Hodgkin plaque. has always been an exciting August 2001

2 Council Members 2001 - 2002

BCA Council Members Prof. Paul R. Raithby (2003) Ex-officio Members Department of Chemistry, 2001 - 2002 University of Bath, Editor "Crystallography News" Claverton Down Dr. Josephine Jutson BATH BA2 7AY 4 Henlle Gardens tel: (01225) 323183, Gobowen, President (2003) [email protected] Oswestry Shropshire SY11 3NU Prof. Chris J.Gilmore GROUP REPRESENTATIVES tel: 01691 671 033 Department of Chemistry [email protected] University of Glasgow Biological Structures GLASGOW G12 8QQ Dr. A. Hadfield (2002), Education Officer tel: 0141 330 3716 Department of Biochemistry, Mrs K.M.Crennell [email protected] University of Bristol 'Fortran Friends' BRISTOL BS8 1TD, P.O.Box 64 Vice President (2004) tel: 0117 928 7436, Didcot Prof. Paul Fewster [email protected] Oxon OX11 0TH, Philips Analytical Research Centre tel: 01235 834 357 Cross Oak Lane Chemical Crystallography [email protected] Dr Harry Powell (2002) Redhill RH1 5HA MRC Lab. of Molecular Biology GROUP CHAIRMEN tel: 01293 815714 MRC Centre [email protected] Hills Road Biological Structures Group CAMBRIDGE CB2 2QH Dr. Richard Pauptit Secretary (2004) tel: 01223 402423 Protein Structure Lab Dr. Christine Cardin [email protected] AstraZeneca, University of Reading Mereside, Dept of Chemistry Industrial Alderley Park, Whiteknights Prof. C.S.Frampton Macclesfield Reading RG6 6AD Roche Discovery Welwyn SK10 4TG, tel: 0118 9318215 40 Broadwater Road tel: 01625-516135 Welwyn Garden City [email protected] [email protected] Hertfordshire HL7 3AY, tel: 01707 366272/366031 Chemical Crystallography Group Treasurer (2003) [email protected] Prof. Paul R. Raithby Mr. David J.Taylor Department of Chemistry 35 Birchley Road, Physical Crystallography University of Bath Billinge Dr C.C.Wilson, Claverton Down WIGAN Rutherford Appleton Laboratory, BATH BA2 7AY Lancs WN5 7QJ ISIS Facility, tel: (01225) 323183 tel: 01744 893108 CHILTON, [email protected] [email protected] Oxon OX11 0QX tel: 01235 82 1900 ext 5137 or 01235 Industrial Group 44 5137, Prof. C.S.Frampton Ordinary members [email protected] Roche Discovery Welwyn, Dr Margaret J. Adams (2003) 40 Broadwater Road, Lab. of Molecular Biophysics Co-opted Members Welwyn Garden City, Rex Richards Building Prof. P.Barnes, Hertfordshire HL7 3AY, South Parks Road Department of Crystallography, tel: 01707 366272/366031 OXFORD OX1 3QU Birkbeck College, [email protected] tel: 01865 275391 Malet Street, [email protected] LONDON, WC1E 7HX Physical Crystallography Group tel: 020 7631 6817 Professor J.L. Finney Dr Jeremy K. Cockcroft (2003) (Web [email protected] Department of Physics & Astronomy Master) University College London, Prof. M.M.Woolfson FRS (2002) tel: 0171 380 7850 School of Crystallography University of York [email protected] Birkbeck College Department of Physics Malet Street Heslington LONDON WC1E 7HX, York, Y01 5DD Full committee details on the tel: 020 7631 6849 tel: 01904 432 238 BCA website - [email protected] [email protected] http://bca.cryst.bbk.ac.uk/BCA/

3 From the Editor BCA Spring Meeting 2002

Have you ever wondered what bonding in cellulose. Also in The third issue goes on behind the scenes at this issue there is a report on the British Museum? In this the Presentation of the Royal issue Andrew Middleton Society of Chemistry Landmark describes how XRD plays a to Commemorate the Work of part in determining how, Dorothy Hodgkin. when and where antiquities were made. In contrast the Jo Jutson article on Fibre Diffraction by April 2001 Trevor Forsyth, ILL covers applications such as a diagnostic method for the investigation of cancer tumours in breast tissue and the study of hydrogen

recombination and repair; Monday evening, a sponsored polymorphism and structural wine reception/poster session on changes; proteins, drugs and Tuesday evening and the disease; new laboratory sources conference dinner on Wednesday. and detectors; thin films, and workshops on topics such as We think we have a great macromolecular crystallisation, programme of scientific sessions, Rietveld refinement, the and a superb venue for the Spring CRYSTALS program … and much Meeting in 2002. Full details of more. So whether you want to the Meeting will appear in the BCA Spring hear the latest results, find out December issue of about new techniques and Crystallography News: the Meeting 2002 instrumentation, hone your skills Meeting should be particularly The University of in the workshops, or simply catch attractive to students, who will up with old friends, we are sure qualify for free registration. In Nottingham, Monday 25th you will be able to enjoy doing all addition to the city itself, - Thursday 28th March of these. Nottingham is also an excellent 2002 base for visiting a wide range of The University Park campus has attractions, from the scenery of The next BCA Spring Meeting will extensive, attractive green space the Peak District to historic cities be held on the University Park and even boasts a boating lake. like Lincoln. We look forward to campus of the University of On-site cultural attractions welcoming you here next March. Nottingham. An exciting scientific include the Arts Centre and the programme, characterised by a brand new D.H. Lawrence Sandy Blake large number of joint sessions Pavilion. Accommodation in halls (email: [email protected]) between the BCA groups, has of residence is available within a been drawn up by their few minutes walk of the lecture Claire Wilson representatives. This includes a theatres and exhibition halls, all (email: [email protected]) Plenary Session on new methods of which are situated in the Pope Local organisers of structure solution and phasing, Building. The social programme along with other sessions on DNA comprises a mixer reception on

4 People in the News September 2001

People in the News OBE for Professor New ICDD Executive Julia Higgins Director

Second European Congratulations to Professor Julia The International Centre for Crystallography Prize Higgins OBE FRS, who became Diffraction Data (ICDD) have Awarded to Professor Dame Commander of the British announced that Dr. Tim Fawcett Jochen R. Schneider Empire in the Queen's Birthday has joined the ICDD as its new Honours list. Julia Higgins is Executive Director. Tim is a long Professor of Polymer Science in time ICDD member, ICDD Fellow, The European Crystallographic Imperial College. She also chairs and served on the Board of Association has awarded the the Athena project on women in Directors from 1988-1990. He second European Crystallography science, engineering and brings to the ICDD outstanding Prize to Professor Jochen R. technology (SET) in Higher experience in management and Schneider of the HASYLAB at Education in the UK, along with R&D for product development, as DESY, Hamburg, Germany. an impressive list of other well as an exceptional Professor Schneider is recognised responsibilities both to the SET background in X-ray diffraction. for his pioneering work on the community and for women in SET. application of gamma-ray The J.D. Hanawalt Award spectroscopy and his high energy Fellows of the Royal synchrotron radiation studies, as Mr. Raymond P. Goehner, and Dr. well as his more recent Society Joseph R. Michael, both of Sandia involvement in the development Congratulations to Dr. Andrew National Laboratories, of the free electron laser. Leslie and Professor George Albuquerque, New Mexico, U.S.A. Sheldrick who have been have been selected to receive the Professor Schneider was born in appointed Fellows of the Royal 2001 J.D. Hanawalt Award for Burgstädt, Saxony, Germany and Society. excellence in the field of X-ray studied Physics in Hamburg after powder diffraction. The J.D. an education as electrical Dr Leslie is Senior Scientist at the Hanawalt Award is presented engineer. He did his PhD under MRC Laboratory of Molecular every three years for important, the direction of Professor H. Biology, Cambridge. He has recent contributions to the field Maier-Leibnitz at the Institute determined the atomic detail of a of X-ray powder diffraction and Laue-Langevin in Grenoble, number of biologically important phase identification published France. His work on gamma-ray structures and most recently within the last five years. The diffractometry and Compton solved the structure of hepatitis B award consists of a scattering was performed at the virus protein. commemorative plaque, an Hahn-Meitner-Institut in Berlin, honorarium, and travel funds to the synchrotron radiation work at Professor Sheldrick is Professor of attend the meeting at which the DESY-HASYLAB in Hamburg, Structural Chemsitry at the award and lecture will be where he is now heavily involved University of Gottingen and presented. in the development of free- Director of the Institute fur electron lasers driven by linear Anorganische Chemie, Gottingen, accelerators. Professor Schneider Germany. He has been a major Retirement - is presently Head of HASYLAB and contributor to the field of Ian Langford Director of Research for chemical X-ray crystallography for Synchrotron Radiation and Free- the past three decades and Dr Ian Langford, Reader in Electron Lasers at DESY. developed the SHELX computer Powder Diffraction, University of programs, for structure Birmingham, has retired after determination and refinement. working for almost 40 years with

5 Royal Scoiety of Chemistry Landmark September 2001

Powder Diffraction, 21 of them Tom had been undergraduates with Arthur (Prof. A.J.C.) Wilson - 5 Presentation of the together at Brasenose College, in the Viriamu Jones Laboratory, Royal Society of and now Tom was Dorothy's Dept of Physics, Univiversity second most famous student. (the College, Cardiff and then in the Chemistry most famous being Margaret Physics Dept (now School of Thatcher (nee Roberts) who later Physics & Astronomy) at Landmark to abandoned chemistry for law and Birmingham. Ian is a leading became Prime Minister). international expert in high Commemorate the resolution X-ray powder Professor Tony Ledwith of the diffraction applied to many Work of Dorothy Royal Society of Chemistry then materials of environmental, presented a memorial plaque to technological and industrial Crowfoot Hodgkin Professor Richards who received it interest and is the author of many on behalf of the University. Since papers on Powder Diffraction. He On 14 May 2001 the Lecture Oxford weather is unpredictable, was a founder member of the BCA Room of the University Natural a virtual unveiling was projected and was involved at the outset in History Museum, Oxford was full on the screen. We saw crimson establishing the Industrial Group. of people eagerly anticipating the velvet curtains slowly open to Ian served on the IG Committee, as presentation of the second UK reveal the plaque which was fixed an academic representative, from Royal Society of Chemistry to the wall on the archway of the 1983 to 1989 and was the Group's landmark. The proceedings were main entrance to the Inorganic first Secretary/Treasurer (1983/87). chaired by Professor Graham Chemistry Laboratory in South He was also a member of the BCA Richards, Chairman of the Parks Road. The inscription reads: Council from 1985 to 1992, as the Department of Chemistry in the Association's Treasurer from 1988 University of Oxford. The Vice- to 1992. Chancellor of the University, the National Historic historian Dr.C.R.Lucas welcomed Chemical Landmark us to the dedication. He reminded us that Dorothy was the first The work of Dorothy Crowfoot British Woman to win a Nobel Hodgkin at the University of prize in Chemistry in 1964. The Oxford. University takes pride in her "In this building from 1956-1994 achievements which have and at other times in the Oxford contributed to the success of the Science Area, Professor Dorothy Chemistry Department in Oxford, Crowfoot Hodgkin (1910-1994) the largest in the country. He was OM, FRS, Nobel Laureate, led sure that Dorothy would have pioneering work on the structures been proud of the fact that some of antibiotics, vitamins and 40% of today's students are proteins, including penicillin, Acknowledgements women. Vitamin B12 and insulin using X- BCA Sponsors ray diffraction techniques. Many One of Dorothy's students, methods for solving crystal The British Crystallographic Professor Sir Tom Blundell, FRS, structures were developed taking Association is grateful to then spoke on "Structural Biology advantage of digital computers Birkbeck College, and Crystallography today: the from the very earliest days. The University of London, influence of Dorothy Hodgkin on work provided a basis for much of who host and manage current developments". present day molecular structure the server for our (Reported later in this article) In driven molecular biology and Website. introducing the speaker, Graham medicinal chemistry." Richards reminisced that he and 14 May 2001

6 Royal Scoiety of Chemistry Landmark September 2001

to retain their order. The study of proteins in water has been immensely important over the years. The final paragraph of the paper in Nature which she and Bernal published demonstrates remarkable foresight.

"At this stage such ideas are merely speculative, but now that a crystalline protein has been made to give X-Ray photographs, it is clear that we have the means of checking them by examining the structures of all crystalline proteins, arriving at far more Outside the Museum with the plaque detailed conclusions about Left to right Dr C R Lucas, Vice Chancellor, Oxford University, Professor Graham Richards, protein structure than previous Chairman of Chemistry, Oxford, Professor Tony Ledworth, Immediate Past President, Royal Society of Chemistry, Professor Sir Tony Blundell physical or chemical methods have been able to give."

Pepsin proved to be a member of a large family of proteolytic enzymes called the aspartic proteinases which have been extensively studied since then. They have about 320 amino acids and 2 motifs of Asp-Thr-Cly at the active site. Charles Bunn was one of the first to work on rennin which was also found to be an aspartic proteinase containing this same motif; it is involved in the inhibition of angiotensin II synthesis, and may be a possible target for better drugs to reduce A drinks reception followed courtesy of GlaxoSmithKline. Left to right - Dr David Giachardi, General Secretary, Royal Society of Chemistry, Elizabeth high blood pressure. Pepsin has Hodgkin, Professor Keith Prout an extended deep active site and drug companies began to think "Structural Biology and Professor Blundell began by about discovering drugs to fit it. Crystallography today: describing Dorothy Hodgkin's In the 1980s chemistry dominated the influence of Dorothy early work in Cambridge with her drug design, X-ray crystallography Hodgkin on current Ph.D supervisor, J.D.Bernal, was traditionally used to model determining the structure of the 3D structures. Knowledge of developments" protein crystals using X-rays. In the structure allows the design of Professor Sir Tom Blundell FRS 1934 she took high quality X-ray structure based inhibitors but (Sir William Dunn Professor of photographs of the crystalline more recently it has proved Biochemistry at the University of protein pepsin, having realised cheaper to generate anti- Cambridge) that the crystals had to be kept in hypertensive drugs using their mother liquor if they were genomics.

7 Royal Scoiety of Chemistry Landmark Fibre Diffraction

The pepsin motif, Asp-Thr-Cly, still cannot answer Dorothy's was also identified in 1985 in the simple question. Traditionally, Fibre Diffraction: retroviral genomes of RSV and laboratory X-rays were used to highlights for X- HIV, published by Toh H et al. in determine the structure of Nature 315, 691 (1985). Studies of proteins and their 3D structures rays, neutrons and the life cycle of HIV and the modelled. Today more powerful structure of HIV proteinase led to synchrotron radiation sources are CCP13 the production of the drug mostly used. Structural biology is 'Indinavar', an HIV proteinase now being applied to aid pre- inhibitor. The 3D structure of the clinical drug discovery to find Fibre Diffraction with X- HIV proteinases was discovered in cures for diseases caused by stray rays and neutrons 1989 but later mutations were mitogenic activity, and those found to have occurred, so involved in cell development, As with many other fields, the cocktails of inhibitors had to be proliferation and differentiation. scope of fibre diffraction is now used to improve the treatment of Modern computers and new changing very rapidly. Major AIDS. Pre-clinical Drug design algorithms using a drug like developments in molecular now has a new paradigm since virtual library now speed up the biology/biochemistry mean that the publication of Complete process of screening new drugs new biological systems are Genomes in the public databases more effectively. Dorothy would becoming available and that in December 2000. (Details can be have enjoyed using these; she totally new approaches exist for found on the Internet at always tried to use the latest sample preparation. There are http://igweb.integratedgenomics. equipment in her research. parallels with this in com/GOLD/) material/polymer science. Perhaps Dorothy Hodgkin's most Exciting opportunities for the Dorothy's interest in people led important influence was the way study of these systems are arising her to work on the structure of she worked and interacted with at X-ray and neutron beam insulin, she felt she had to find people. Although she sources. New facilities planned the structure of insulin before a collaborated with many who such as the DIAMOND cure could be found to save worked in industry, she never synchrotron and the second children dying from early onset thought of this as collaborating target station at ISIS will be of diabetes. This structure was with a faceless industry, but major importance. Equally published by Adams, M.J., rather as working with her friends important will be the upgrade of Blundell, T.L, Dodson, G.G, who happened to be employed existing facilities to exploit their Dodson,E, Vijau, M, and Hodgkin by an industrial company. Her full potential. At the Daresbury D.C et al. in Nature 224, 491-495 students learnt the importance of SRS, a purpose designed high- (1969). Just knowing the structure a large network of contacts to angle fibre diffraction camera has did not satisfy Dorothy, she successful research. been constructed by Dr. R. wanted to know how the insulin Keyhoe for use on beamline 14.1 carried out its function in the Kate Crennell (see http:// www.dl.ac.uk/ SRS/ PX/ body. Fred Sanger showed her a July 2001 line14/ 14_1/fibre_camera.html). model of the insulin receptor At the Institut Laue Langevin (ILL) binding which she admired but Note: Information about Dorothy in Grenoble a major she had to understand how the Hodgkin can be found on the BCA refurbishment of instrumentation insulin behaved in the body. She web site, at in under way as part of the ILL asked 'How does it work?' No one http://bca.cryst.bbk.ac.uk/BCA/obits Millennium Programme: perhaps could answer that question then /CVS/DCH.html the most important development and despite more recent work by and there is an excellent life here for the fibre diffraction Hubbard and Hendrickson in 1995 history at: community is the planned and work by Louise Johnson on http://www.engr.psu.edu/wep/Eng upgrade of the D19 the structure of phosphorylase we CompSp98/Aclausi/HodgkinD.html diffractometer – the new detector

8 Fibre Diffraction September 2001

on this instrument will give a gain Recent results from beamline 2.1 Neutron fibre diffraction in detecting solid angle of at the Daresbury SRS suggest at the Institut Laue approximately 25 and open up that X-ray fibre diffraction can Langevin - hydrogen entirely new possibilities for fibre be used as a diagnostic method bonding in cellulose diffraction (as well as single for the investigation of cancer crystal) work (see http:// tumours in breast tissue. The In the neutron arena, one of the www.ill.fr/ YellowBook/ D19/ study, which was published by most striking results in fibre help/ dev/ development.html). Lewis, Rogers, Hall, Towns- diffraction is the work of Langan, Andrews, Slawson, Evans, Pinder, Nishiyama & Chanzy (J. Am. Chem. Fibre diffraction has made critical Ellis, Boggis, Hufton & Dance (J. Soc. 121 (43), 9940) who are using contributions to our Synch. Rad. 7, 348), shows clear unique facilities available for understanding of biological and differences between fibre neutron fibre diffraction on synthetic polymer systems in the diffraction patterns recorded instrument D19 at the Institut Laue past. The following highlights from healthy and diseased breast Langevin (ILL) in Grenoble to study hydrogen bonding in various forms from recent X-ray and neutron tissue (see Figure 1). These of cellulose. Cellulose is often said fibre diffraction work illustrate differences are believed to occur to be one of the most abundant the importance of the technique as a result of changes in the polymers on Earth. These workers for the future. structural ordering of the are interested in the structural collagen within breast basis of the biological, chemical carcinomas. Collagen is a major and physical properties of X-ray fibre diffraction – component of the extracelluar cellulose. Central to this is the new insight to breast matrix (ECM) in breast tissue; its hydrogen bonding network of the tumour tissue from the degradation is known to be of hydroxyl groups of the polymer. Neutron diffraction provides the Daresbury SRS major importance in the most powerful method that can morbidity and mortality of offer a detailed visualisation of this cancer. Furthermore, extensive hydrogen bonding network in alteration of the ECM has been cellulose fibres. Figure 2 shows a observed in other forms of 2Fo-Fc map derived from data cancer – collagen derangement recorded from cellulose II samples has been attributed to enzymatic that have been deuterated by degradation and altered mercerisation in NaOD. The maps neosynthesis. Since the fibre- clearly show the labile hydrogen forming collagen molecules atoms involved in the hydrogen bonding and allowed the authors produce well-defined diffraction to distinguish between two data, changes in the structural Figure 1. (a) Apparently normal breast competing models for cellulose II. tissue ordering of the ECM can be studied by X-ray diffraction. This approach offers some advantages over standard histopathology in that it utilises untreated samples and takes an average over all tissues illuminated by the X-ray beam. It is therefore potentially much faster and also less prone to errors that can occur by simply Figure 2. 2Fo-Fc map calculated from Figure 1. (b) Tumour tissue. X-ray looking at the wrong part of a cellulose II. The neutron fibre diffraction diffraction images of 2 samples from the sample. data were recorded on instrument D19 at same breast. Most of the features present the Institut Laue Langevin, Grenoble (see arise from collagen in the sample (see Langan, Nishiyama, Chanzy, J. Am. Chem Lewis et al, J. Synch. Rad. 7, 348). Soc. 121(43), 9940)

9 Fibre Diffraction Crystallography and Antiquities

The CCP13 collaborative Crystallography and diffractometer. Samples are computing project for normally removed under a fibre diffraction Antiquities binocular microscope offering maximum precision and minimum damage in sampling. A casualty The unique experimental In the last issue of Crystallography opportunities available to the of this type of sampling, of News, David Rendle (2001) fibre diffraction community are of course, is any possibility of course being paralleled by introduced his article by saying meaningful quantitative analysis. seemingly relentless increases in that Crystallography in Forensic In a few case study ‘cameos’ I will computing power as well as major Science usually implies the use of try to provide some idea of the initiatives such as the X-ray powder methods (XRD). way XRD is used to help answer “computational GRID” which The same can be said really for the questions just set out. aims, within a relatively short Crystallography and Antiquities: Frequently, XRD provides only a time, to revolutionise distributed rarely are single crystal methods part of the answer and usually computing and data transparency. used, though there have been the investigation will be These massively enhanced exceptions, and the interest is collaborative, involving several facilities for computing now mean most often in the qualitative different analytical techniques that biological and synthetic identification of crystalline and perhaps several scientists. polymer questions can be phases. Another parallel with the addressed in a way that was quite use of XRD in forensic science is, Recently, we have been impossible even a few years ago. perhaps, the range of materials investigating the pigments used It is fortunate therefore that the encountered: we might be to decorate ancient Egyptian fibre diffraction community has a analysing Anglo-Saxon jewellery coffins and other artefacts well focused strategy for data one day and lumps of slag, sherds (Middleton and Humphrey in extraction and analysis in the form of pottery or Egyptian pigments press). Studies like this allow us of the CCP13 collaborative the next. The parallels do not to develop our knowledge of the computing project. The project, stop there either, for we too are ancient Egyptian artist’s palette which is now nearly 10 years old, interested in tracking materials and the ways in which it changed has been exceptionally successful. back to their source, much as the over time and in different parts of Heavily allied to the NCD forensic scientist might need to ancient Egypt. XRD is well-suited programme at Daresbury, it has determine the source of a flake of grown from a community that to this type of investigation, paint or a trace of soil. However, was initially centred on X-ray fibre allowing the identification of the diffraction studies of biological there are differences and most of pigment using only a minute molecules to one that now covers our XRD analyses are aimed at sample, which can be removed X-ray and neutron diffraction answering questions along the almost non-destructively from an concerns over the whole polymer lines: What was it made of?, How existing blemish on the community. It is perfectly poised was it made?, and Where was it ‘paintwork’. Indeed, X-ray to deliver the radical new made?, perhaps providing the powder photography was used approaches needed for data information to address questions more than sixty years ago, by extraction and modelling software like When was it made? and Is it a Jope and Huse (1940), to to its biology and materials fake?. characterise a series of samples of science communities. Egyptian Blue, the blue pigment A common factor that runs used on many artefacts from Trevor Forsyth (Chairman, CCP13) through nearly all analyses carried ancient Egypt (see, for example, Institut Laue Langevin & out in the museum is that we are the Middle Kingdom coffin shown Physics Department, Keele restricted in the size of sample in Figure 1). They were able to University that we use, so that for us XRD show that blue pigments from Tel: +33(0) 4 76207158 powder methods generally means several sites in England were the Fax: +33(0) 4 76207648 the use of Debye-Scherrer powder same as examples from Egypt, Email: [email protected] cameras, rather than a and subsequent research has

10 Crystallography and Antiquities September 2001

confirmed that this pigment was white pigment. Huntite was breaks or from an unglazed foot- used widely across the ancient recognised as a mineral species ring (Bimson 1969), provided a world from about 3100 BC only in 1953 (Faust 1953) and, means to characterise the nature through the Roman period until it because of its typically very fine of the paste mixtures used to ceased to be used around the 9th grain size, it can be very difficult make early English porcelain century AD. Egyptian Blue is a to identify either optically or by samples and compare them with copper calcium silicate, which is chemical analysis. However, the Chinese porcelain. The so-called identical to the mineral, XRD powder pattern is diagnostic. glassy-frit porcelains, which cuprorivaite. However, this is very typically have calcium-rich rare in Nature and there is no compositions, were found to doubt that the blue used in contain a calcium silicate mineral ancient Egypt and elsewhere was (typically wollastonite); those manufactured by heating based on the use of magnesium- together quartz, limestone or rich soapstone (talc) typically calcite and a source of copper contain enstatite, formed by the (such as copper alloy filings) to a transformation of the soapstone; temperature of about 850-1000o C. and bone-ash porcelains were It is the earliest synthetic found to be characterised by pigment. whitlockite, a calcium phosphate mineral formed by the transformation of bone. By Figure 2. Chinese underglaze-blue contrast, XRD showed that the porcelain dish, mid-14th century, Yuan Dynasty. Chinese hard paste porcelains are characterised by mullite, usually with some relict quartz and Chinese porcelain (Figure 2) cristobalite. became known in Europe from about the fifteenth century AD and almost immediately attempts Figure 1. Detail of Middle Kingdom coffin were made to emulate it by from El Bersheh. European manufacturers. Chinese porcelain was made from a mixture of kaolinite and a Natural minerals also formed an ‘porcelain stone’ or ‘petunze’. important element in the ancient This provided the essential Egyptian palette, including ingredient, a high proportion of commonly occurring minerals sericite mica, which acted as a such as hematite for red, limonite high temperature flux, vital to the for yellows, and calcite or gypsum successful manufacture of hard- Figure 3. Ninth century AD silver strap-end from Whitby with niello decoration. for white. However, XRD has paste porcelain. European revealed the use of some more manufacturers were unaware of unusual minerals. Jarosite, an this and used a variety of Niello, a black material used to iron sulphate, was used for a ‘recipes’, each with a different produce striking inlaid designs on distinctive pale lemon-yellow combination of raw materials. decorative metalwork, has a long paint on some Middle Kingdom The mineralogy of these ‘soft- history as a jeweller’s decorative coffins from Asyut in Middle paste’ porcelains reflects the raw technique, going back at least to Egypt, and there is increasing materials used by the various the Romans. It has been evidence that huntite, a factories. X-ray powder identified in Anglo-Saxon magnesium calcium carbonate photography, using minute jewellery (Figure 3) and its use was used extensively as a fine, samples removed from existing extended across Europe and into

11 Crystallography and Antiquities September 2001

Asia but by the sixteenth century fine example of Late Bronze Age, and some form of analysis is its popularity in Europe had Cretan craftsmanship, dating to c. essential to avoid misidentifications. waned. Nevertheless, some fine 1400 BC, suggesting, along with The two seals shown in Figure 5 examples were made in Russia other evidence, that the antiquity are very similar in appearance but during the 18th and 19th of this technique may be analysis by XRD showed that they centuries and the technique considerably greater than were made from two different enjoyed a brief 20th century previously thought (La Niece materials (Sax et al. 1993). The revival in England with the Arts 1998). larger, Akkadian period seal on and Crafts movement. Niello is the left (c. 2300 BC) was made made by melting metal filings from serpentinite, a stone well- with sulphur; various metals have suited to seal-making because it is been used in different places at fairly hard and takes a good different times, including silver, polish. The seal on the right, copper and lead, either singly or which dates to the later Ur III in combination. After cooling, period (c. 2100-2000 BC), was the resulting metal sulphide is made from chlorite, a softer and crushed, mixed with a flux, much inferior material. Why applied to the prepared area and change to an inferior material? then heated to soften (or melt) The change coincides with an the sulphide into place, rather invasion of the area by a people like an enamel. Figure 5. Mesopotamian cylinder seals of called the Guti and it seems that serpentinite (larger seal on left, Akkadian, c. 2300 BC) and chlorite (right, Ur III period, this disrupted the trade routes c. 2100-2000 BC). that supplied the serpentinite, obliging the seal-makers to Cylinder seals (Figure 5) substitute it with chlorite, which developed in Mesopotamia, was available more locally. alongside the cuneiform system of writing, beginning some time As noted at the beginning of this around 3500 BC. They have article, XRD may not always intricately carved designs on their provide the complete answer to curved surfaces and were usually the questions we ask of perforated along their length, so antiquities but I hope that this that they could be suspended on short note has illustrated that it

Figure 4. Inlaid silver cup from Enkomi, a thread and worn. When rolled may often contribute something Cyprus, c. 1400 BC. out in soft clay, the intaglio to our understanding of the designs (carved in reverse!) ancient world. Without some form of analysis, provided a mark of the owner’s niello is easily confused with authority, in much the same way Andrew Middleton other black inlays, especially on as sealing wax and seals are still Department of Scientific Research ancient artefacts that may have used on official documents. The The British Museum been buried and corroded. It is cylinder seals were made from here that XRD comes into its own, variety of materials, chiefly References providing an unequivocal means natural minerals and stones, but Bimson, M. 1969 The examination of by which the characteristic metal sometimes ivory, metals or ceramics by X-ray powder diffraction. Studies in Conservation 14 83-9. sulphides can be identified. For faience. Identification of the Faust, G.F. 1953 Huntite, Mg3Ca(CO3)4, example, it has been possible to materials of the seals can throw a new mineral. American Mineralogist identify a mixture of silver, light on the exploitation of raw 38 4-23.Jope, E.M. and Huse, G. 1940 copper and lead sulphides on a materials in antiquity but Examination of ‘Egyptian Blue’ by X-ray fragment of shiny black inlay identification is not always as powder photography. Nature 146 26. La Niece, S. 1998 Niello before the from the Enkomi cup (Figure 4), a straightforward as anticipated

12 Dehydration of α-lactose September 2001

Romans. Jewellery Studies 8 49-56. physical transformations of Comparison of Surfaces Middleton, A.P. and Humphrey, M.S. in lactose need to be characterised press Pigments on some Middle 020 and 100 in order that, when used in a Kingdom coffins. In W.V. Davies (ed.) Colour and Painting in Ancient Egypt, pharmaceutical formulation, it The water in face 020 is arranged London. will remain stable. A change in in layers between rows of lactose Rendle, D. 2001 Crystallography in form can lead to adverse changes molecules, whilst the water in forensic science. Crystallography News in the active component of a face 100 is arranged in channels No. 77 27-8. formulation. perpendicular to the face. The Sax, M., Collon, D. and Leese, M.N. 1993 The availability of raw materials for Near way in which the water molecules Eastern cylinder seals during the The object of this work was to are arranged affects the way in Akkadian, Post-Akkadian and Ur III investigate the dehydration of α- which they leave the structure of periods. Iraq LV 77-90. lactose monohydrate, using ALM when it is heated. Molecular Dynamics modelling. Differential Scanning Calorimetry The dehydration of and X-ray Diffractometry were Molecular Dynamics used during the course of the Simulations work, as characterisation tools. α -lactose The simulations were carried out monohydrate at 420K, using the Hoover DSC and XRD results thermostat and Dreiding IG Poster Prize Winner, potential set throughout. NVT Reading 2001 The samples of ALM used in this dynamics were done. The study were dried in an oven simulation of surface 020 α-Lactose monohydrate (ALM) is under a stream of dry nitrogen suggested that the face goes an extremely important gas, at various temperatures, through an amorphous face pharmaceutical excipient. It is before DSC and XRD traces were during the drying phase. This widely used because of its recorded. The DSC trace for a happens before the water availability in a highly pure sample of lactose heated to 120°C molecules move away from the crystalline form, and because of shows very little change from that surface. As the topmost layer of its low toxicity. Lactose (β-D- for unchanged ALM. A peak at this surface is composed of lactose galactopyranosyl(1,4)-C- 140°C is due to loss of water from molecules, with a layer of water glucopyranose) is the main sugar the crystal lattice. At beneath, this would seem to be of milk and other dairy products. temperatures up to 160°C, DSC necessary, in order for the water It appears as different forms, traces show no peak for the loss molecules to escape. The topmost depending on the α- or β- of water, but a peak around layer was first to become glucose isomerization in aqueous 170°C, suggesting a change to disordered, followed in turn by solution, and the association of another phase. Drying ALM at lower layers. Face 100 also water molecules in the solid form. 165°C results in a DSC trace with becomes disordered during the In aqueous solution, the two no peaks present, suggesting that drying process, but to a lesser forms (α - and β-) are balanced by this phase change takes place degree than face 020. This may mutarotation. The natural during the drying procedure at be due to the channels of water crystalline state is α-lactose 165°C. The XRD results confirm present in this face, which would monohydrate, but several other this, with the pattern for a sample appear to allow the water solid forms exist, such as, dried at 120°C being identical to molecules to leave this surface anhydrous β, and stable and standard ALM. According to the more readily than face 020. The unstable anhydrous α-lactose. XRD trace for a sample heated at molecules of lactose are more There is also an amorphous form 150°C, the unit cell for this sample likely to stay in their original of α-lactose monohydrate. The is similar to that for standard orientation in this face as well, different forms have different ALM, but the molecules are whilst in face 020 they tend to hydration properties, and the orientated differently. move through 90°, so that the

13 Dehydration of α-lactose Book Reviews

two rings of the sugar molecule done, in order to investigate the By comparison to the first edition, are arranged horizontally, rather kinetics underpinning the in the second edition Chapter 1 is than vertically. dehydration process. expanded to show how a variety of more complex crystal structures H.L.Williams1, G.B.Thomson1, can be explained in terms of Conclusions, Discussion P.C.Wright1, D.R.Merrifield2 different faulting sequences of and Future Work close-packed layers. In addition, 1. Dept of Mechanical and Chemical the structures of carbon including The results from DSC and XRD Engineering, Heriot-Watt University, fullerenes are discussed, and Edinburgh studies show that ALM related to the development of 2. SmithKline Beecham Pharmaceuticals, dehydrates at 140°C, to give an New Frontiers Science Park (South), Third symmetry ideas. In Chapter 2 the unstable product. This is an Avenue, Harlow, Essex figures have been updated and unstable anhydrous form of α- these facilitate a clearer lactose, which is very hygroscopic understanding of two- and converts readily to ALM. The dimensional and, consequently, peak seen on DSC traces for Book Reviews three-dimensional symmetry. samples dried at temperatures Non-periodic patterns are also lower than 165°C is caused by the The Basics of introduced. Chapter 3 now conversion of this unstable Crystallography and includes a short discussion on anhydrous product to stable Diffraction - 2nd Edition space-filling polyhedra and in anhydrous α-lactose. At By Christopher Hammond Chapter 4 the discussion of space dehydration temperatures greater groups is significantly expanded, than 165°C, the product of Publisher Oxford University Press and is a very helpful background dehydration is the stable to the understanding of the Space anhydrous form, so there is no May 2001 Group representations in Vol. A peak on the DSC trace Hardback ISBN 0-19-850553-1, of the International Tables for corresponding to the conversion £49.95 Crystallography. Chapters 5 and from unstable to stable Paperback ISBN 0-19-850552-3 6, covering lattice planes and anhydrous form. £22.95 Miller indices, and the reciprocal lattice, have been revised, and are The modelling results suggest This text book is aimed at now easier to read and that there may be an amorphous advanced undergraduates and understand. In Chapter 7 the phase involved in the dehydration post graduate students working human eye as an optical mechanism. This may be involved in the areas of solid-state instrument is discussed, and the in the formation of the unstable chemistry, physics, materials processes involved are related to anhydrous α-lactose. The science and earth science, and the situation in the diffraction samples used in this study were also contains information that process for other wavelengths of dried under nitrogen gas, in order will be of value to more electromagnetic radiation. In that the same conditions could be experienced research workers and Chapter 8 the contributions of maintained for all samples. lecturers. In this new edition the von Laue, the Braggs and Ewald Dehydration in a moist first edition has been significantly to X-ray diffraction are described. atmosphere may result in expanded (242 pp to 331) and Chapters 9 and 10 in the first different products at different much of the material has been edition have been expanded to temperatures. To model the revised and updated. In Chapters 9, 10 and 11 in the new effect of water on dehydration, particular, the reader is edition. The topics of X-ray and Molecular Dynamics simulations introduced to topics that are of neutron diffraction from ordered will be done with the surface of more general interest but that are crystals, preferred orientation and lactose in contact with water closely related to the basic its measurement are now covered molecules. On-line dehydration, concepts of crystallography and in detail, and the relevance of the using a heating cell, will also be diffraction. work on preferred orientation to

14 Book Reviews September 2001

materials and earth sciences to students and lecturers working First, they adored science, they emphasised. Chapter 12 contains in the area of crystallography and had many other activities but they an excellent discussion and diffraction. The textbook is one were all passionately determined explanation of stereographic in a series sponsored by the and in love with their work. projections, and the usefulness of International Union of the method explained. The book Crystallography and published by They had sympathetic parents and is completed with a series of Oxford University Press. influential relatives; most of them useful appendices including were from professional or details of crystallographic model Paul Raithby academic families; for example builders, crystallographic University of Bath we learn that Dorothy Hodgkin's software, biographical notes on July 2001 uncle asked a friend for advice as famous crystallographers and to how Dorothy could continue in other scientists working in the science after her first degree. The area of diffraction, useful Nobel Prize Women in friend replied she should try to crystallographic relationships, Science. Their Lives, become a student of J.D.Bernal. vectors and complex numbers, Struggles and and systematic absences. There Momentous Discoveries Religious values stressing are useful teaching exercises at by Sharon Bertsch McGrayne education were critical; some the end of each chapter with were Quakers and half were quite detailed answers at the end Publisher Carol Publishing Group Jewish. of the book. 1998 2nd Edition UK price £15 Behind many of these successful Overall, the second edition ISBN 0-9702256-0-1 450 pages, women stood a man; the Braggs represents a significant paperback with line diagrams and and J.D.Bernal encouraged a improvement on the already high photographs generation of English women quality first edition. The material crystallographers, including is clearly laid out and the subject This is a fascinating book for all Dorothy Hodgkin. Others were is developed logically. The those interested in the history of not so fortunate, on page 7 we fundamental importance of science, especially those who read 'Unfortunately for Jocelyn symmetry is made at an early wonder why some people Bell Burnell's career her thesis stage. While the subject matter is become great scientists and yet adviser failed to become her correctly described as ‘basic’ the others with apparently similar mentor and she received little or text can be read at several levels abilities leave science altogether. no career counselling.' and there are aspects that will be This book describes the lives of 15 of interest to undergraduate women who have either Good luck and timing were vitally students and others that are themselves won a Nobel prize or important; pioneers like Marie better suited to researchers with played a crucial role in a Nobel- Curie and Lise Meitner came of greater experience and expertise. prize winning project; it tries to age just as European Universities Throughout, the text is very answer the question: why have opened their doors to women; readable, and the level of only 10 of recipients of the Nobel eight of the fifteen women were mathematics is appropriate to the Prize in the sciences been women born within fifteen years of each subject matter covered. The when there have been over 300 other, eleven within a single additional material of preferred men since the Prizes were first generation between 1896 and orientation fibrous materials is awarded in 1901? 1921. Some, like Gertrude Elion, very interesting and useful, and is (prize winner in 1988) had the discussion of electron The first chapter, 'A Passion for worked for years without diffraction and its applications Discovery' analyses the qualities managing to get a 'scientific' job, given in Chapter 11. these women had in common but it was not until late in the which enabled them to overcome Second World War that the I strongly recommend this book the many obstacles in their way. shortage of industrial chemists

15 Book Reviews Meeting Reports

enabled her to get a research post to this promise. with Burroughs Wellcome. There Meeting Reports she worked on purines, studying Students came from a wide range not only their structures but also Eighth Intensive Course – of places, fields of study and their biochemical reactions, background – and had a similar in X-ray Structure searching for better drugs for range of experience of single diseases such as leukaemia and Analysis crystal structure determination. others to prevent rejection in The immense skill, effort and 30th March – 7th April 2001, transplanted kidneys. commitment by the group tutors Trevelyan College, Durham The book has 3 sections, 'First in engendering co-operation and generation pioneers', including collaborative working is an The Eighth Course was the third Marie Curie and Lise Meitner, essential part of the Course, and one to be held in Durham, the 'Second generation' which one which is very much courses having begun in Aston includes both Dorothy Hodgkin appreciated by the students. University, Birmingham, in 1987. and Rosalind Franklin, and 'The This course generally followed the New Generation', Jocelyn Bell The Course covered all aspects of successful format of its Burnell, an astronomer who structure determination, including predecessors, but it has evolved to discovered quasars as a graduate fundamental concepts of reflect changes which have student, and Christiane Nüsslein- symmetry, diffraction, Fourier occurred in structure analysis, a Volhard, a developmental synthesis and direct methods and process which will continue. David biologist who gained the Nobel their application to solving and Watkin, the director of the first prize for physiology and medicine interpreting structures. The five Courses, made a welcome in 1995. practical side also included a return in the role of lecturer, survey of crystal growth replacing Bob Gould who had Each woman's life is described in techniques, data collection, directed the previous two Courses a separate chapter using structure solution, refinement, in Durham. information from primary and interpretation and presentation. secondary sources and interviews The Course finished with lectures The Course is based on lectures with colleagues, students, family, and a practical session on given by a group of four lecturers, friends and experts in the field. databases given by staff of the interspersed with tutorials in small Bibliographic references for the Cambridge Crystallographic Data groups of eight students: this time sources are collected into a Centre. we had nine groups, a total of 72 section of 'Notes' at the end and students. All lecturers and tutors there is a comprehensive index. The evenings were given over not are present for the duration of the All scientific explanations are only to the Matrix Mixer, but also Course, and so are available for nontechnical and illustrated with to sessions on crystallisation, a informal questions or discussions: simple diagrams or photographs, crystallographic bar quiz, an it is common to see tutors sacrifice including some I had not seen expert panel and student at least part of their coffee breaks before for the crystallographers. presentations. The evening where to help students with particular the students were mandated to queries. The Course began on the I enjoyed this book; I learned work together to produce group first evening with a gentle new facts on the careers of some presentations was particularly reminder by David Watkin about people I thought I knew all about entertaining and informative. For essential mathematics in the so- and as a physicist I was surprised light relief one evening featured a called “Matrix Mixer”, and then to find I understood the more Ceilidh marked by great ran for a further seven days with biological and medical chapters. enthusiasm: if occasionally the just an afternoon off for dances went chaotically wrong recuperation. Students were Kate Crennell that was all part of the fun. The warned in advance that the Course July 2001 Course Dinner occupied the final would be intensive and it lived up evening, where those responsible

16 Meeting Reports September 2001

for making the Course a success – the opportunity of concentrated concluded by emphasising that a sponsors, organisers, lecturers, study and learning support which high quantity of data needs high tutors, students and local staff – is not available elsewhere. There is quality data management to were thanked for their much use of crystallographic black produce usable knowledge. contributions. boxes within computer programs, which invite the user to press a “Prediction, Morphology and The Course was clearly highly button or follow a script. In many Mechanical Properties of appreciated by the students, who cases this does work reasonably Paracetamol” was presented by provided valuable feedback which well but in difficult cases even the Sally Price of UCL. Sally’s will inform the content and best black boxes may eventually presentation demonstrated how structure of the next Course in say “Consult an experienced difficult polymorph prediction can 2003. There are particular crystallographer”. Only by be, but also highlighted some of challenges in the wide range of understanding how these boxes the ways that may make previous experience of work can difficult problems be polymorph prediction more mathematics and crystallography. solved, and developing this feasible in the future. She It is important to provide understanding is the prime highlighted how the use of global adequate support in these areas objective of the Course. minima in lattice energy would without detracting from the more always be necessary, but pointed advanced material, and this is one Sandy Blake out the high number of minima of several aspects of the Course University of Nottingham that normally occur within a which will be developed over the Course Director 2001 feasible range. She then went on next two years. A book based on to explain how you could the Course, written by one past eliminate unlikely structures based and three current lecturers and BCA Industrial Group on their morphologies. For entitled “Crystal Structure Analysis Pharmaceutical Special instance, crystal structures whose – Principles and Practice” is due to Interest Group Meeting elastic constants mean they would be published by OUP in January be too compressible to be realistic 2002. The Ninth Course in 2003 7th June 2001, GlaxoSmithKline are unlikely to form. In addition, will have five lecturers, with Simon crystal structures whose slowest Parsons changing role from tutor Paul Higginson of Pfizer opened growing face is too slow are also to lecturer. the meeting with the presentation unlikely to form. Sally concluded The venue was again a highly "Automated Solutions to High by suggesting that involving successful element of the Course. Throughput Crystal Screening". nucleation kinetics may be the The lecture facilities at Trevelyan Paul’s presentation highlighted way forward in this area. College have been upgraded since the cost that could occur in the the previous Course, and the close pharmaceutical industry should Our hostess Clare Anderton gave proximity to accommodation, the wrong solid form be taken the final talk of the morning catering and social amenities into development. He highlighted entitled “On-Line Monitoring of means that the different aspects the benefits of automated Solid-State Form during of the Course could be easily screening, not just to the Crystallisations by Raman integrated. researcher who is relieved of the Spectroscopy”. Clare explained monotony of repeated what Raman Spectroscopy is and The number of scientists involved experiments, but also to the how it works. She then in crystallographic structure company who can reduce the risk highlighted some of the determination continues to of an unwanted form appearing advantages over methods such as expand: it is an essential technique late in development. Paul XRPD, especially for online but one where they must acquire demonstrated the use of monitoring. These included: high expertise quickly and alongside automated screening, and the throughput, real time other methods. The Intensive instrumentation involved, with a investigation, multiplexing with Course is a vital resource, offering successful case study. He more than one probe, portability

17 Meeting Reports September 2001

of the instrument and the developed for the interpretation which enables the accurate sensitivity of Raman to solids of the XRPD patterns to allow for location of reflection positions forming in solution. Clare then fingerprint phase analysis through along with good angular took us through two case studies peak search and cross correlation. resolution and superior counting to show just how effective the Once identified, Crystallics can statistics. This specification method can be. The first case characterise these polymorphs, produces data with a quality that study showed how the crystalline off-line, by thermal analysis (DSC, maximises the chances of solving form could be monitored from the TGA) and by crystal structure the structure. It is vital that the mid-point to the end of a determination, typically using effects of preferred orientation on crystallisation procedure. The Single Crystal X-ray Diffraction. If intensities are removed from the second case study showed how the necessary, a ‘MultiMax’ reactor can measured patterns and this is form of a product varied during be used to optimise crystal growth achieved by collecting data using a the manufacturing procedure, conditions to produce suitable rotating capillary geometry. To previously unseen by off-line quality single crystals. If only small, reduce absorption effects measurements. Both case studies poorly diffracting crystals are borosilicate capillaries are used, allowing quantification of forms available the crystal structure can while data is improved still further to as little as 5-10% in situ. be determined from high- by using a 1mm slit which reduces resolution XRPD data. Ab initio the background at no cost to the The first presentation of the structure prediction is also offered measured intensities. Data analysis afternoon was by Dr. Arjen van as a means of structure with DASH begins with unit cell Langevelde of Crystallics on “High- determination. Finally, once and space group determination. Throughput XRPD in Polymorph polymorphs have been identified The peak positions of the first 20 Discovery”. Crystallics is a company and characterised, the reflections are located using DASH which specialises in the crystallisation conditions to and passed to an input file for a investigation of solid form optimise the production a specific third party indexing program such pharmaceutical materials, in polymorph on scale up can be as DICVOL-91. After indexing, a particular polymorph precisely determined using the careful process of unit cell and identification, characterisation and ‘MultiMax’ reactor in batches up space group verification takes production. Polymorph to 50 ml. This system is able to places by visual comparison of identification is achieved through automatically determine the meta- predicted ‘tick marks’ vs observed an automated high-throughput stable zone through solution peak positions. The next stage is to crystallisation screen. Here turbidity measurements. (Further perform a Pawley fit of the raw concentration, solvent information can be found at data which seeks to model the composition, temperature, cooling http://www.crystallics.nl/) pattern background, zero point, gradients and ripening time can intensities, peak widths and also be individually controlled to Dr. Alastair Florence of the refine the unit cell parameters. produce a wide range of University of Strathclyde Typically data is collected to 60° 2θ crystallisation condition thus continued the session with his but the high angle data is often maximising the chances of presentation entitled ‘DASHtastic omitted from the fit due to a high discovering polymorphs. More Adventures with the Bruker-D8’. degree of peak overlap and poor than 1000 different crystallisation Alastair related his recent success signal-to-noise in this region. After experiments can be undertaken at in using the DASH program to data processing, the business of one time, yet each crystallisation solve molecular crystal structures solving the structure can take takes place in 20ml wells, from Powder X-ray diffraction place and this was described using minimising the amount of material data collected on the Bruker-D8 Chlorpropamide as an example. required. The resultant solids are diffractometer. The diffractometer Initially a trial structure was screened for crystallinity by an in his laboratory is equipped with generated by placing the automated X-Ray Powder a primary monochromator to asymmetric unit at random within

Diffraction (XRPD) system, while provide Cu Kα1 radiation and a the unit cell. Comparison of the proprietary software has been Position Sensitive Detector (PSD) simulated XRD pattern with the

18 Meeting Reports September 2001

experimental one clearly under ambient conditions and can dimensional X-ray diffraction demonstrated that the structure transform to 4-epi-OTC. The level system designed for rapid was incorrect. A Simulated of the 4-epi-OTC impurity must be screening, D8 Discover GADDS for Annealing algorithm was then controlled to be less than 1% Combinatorial Screening, has been used to move the molecules about during production. HPLC is used to developed for this purpose. The the cell and vary torsion angles monitor the 4-epi-OTC level but system consists of a θ-θ vertical within the molecules to generate the system must first be calibrated goniometer on which are housed more trial structures and minimise against standards of accurately X-ray tube and optics, a two- the difference between simulated known 4-epi-OTC content. In order dimensional X-ray detector, and and experimental patterns. to reproducibly generate these an XYZ sample stage plus 300,000 structures were tested to standard samples, the laser/video for sample alignment find the one that gave an environmental conditions that and monitoring. This geometry excellent fit across the whole govern the formation of 4-epi-OTC allows the combinatorial library of pattern at which point the must be understood. Using the samples to be mounted with ease. structure was considered to be X’Pert Pro system, three crystalline The two-dimensional multiwire solved. The process took just 5 phases were found to be detector can collect a large area of minutes! associated with the formation of a diffraction pattern with high 4-epi-OTC and by recording PXRD speed, high sensitivity, low noise The third presentation of the patterns as a function of and derives intensities by afternoon was by Detlef Beckers temperature (5°C steps) and RH (5 integrating around the powder of Phillips Analytical and was % steps) it was possible to rings thus limiting the effects of entitled “Temperature and construct a phase diagram relating preferred orientation. The Humidity Controlled X-Ray all three of the phases. Using this laser/video system ensures that Diffraction Analysis on 4-Epi- information the conditions each sample is aligned accurately Oxytetracycline”. The ability to required to generate samples of on the instrument center. monitor structural changes of a precisely known 4-epi-OTC content Different areas of a sample can be material as a function of could be determined. probed by the system since the X- temperature and relative humidity ray beam can be collimated from is of great importance to Chris Weston of Bruker AXS 1000 to 50 µm. Once all the data pharmaceutical industry. An concluded the session with his has been collected the GADDS unexpected phase transition at presentation on “X-Ray Rapid software can be used to perform high temperature and high Screening System for the user specified screen. This humidity during storage or Combinatorial Chemistry”. could be phase identification transport can turn a powerful Combinatorial chemistry refers to (qualitative and quantitative) or medicine into a useless powder. techniques to fabricate, test and measurements such as degree of Phillips Analytical have developed store the resulting data for a crystallinity, particle size, texture a stage for the X’Pert Pro material library containing tens, or stress. To achieve this a wide Diffraction System where sample hundreds or even thousands selection of screening parameters chamber temperature and different materials or compounds. can be extracted from the patterns humidity can be independently Combinatorial investigations such as integrated intensity, controlled. Humidity levels of 5% require rapid screening techniques maximum intensity, peak width, to 95% can be achieved between to test and evaluate variations of peak 2θ position, crystallinity and room temperature and 50°C. An composition, structure and various stress components. The example of the use of the system property within a material library. screening results can be displayed was described by reference to X-ray diffraction is one of the most in colour coded map, 3D surface measurements on 4-epi- suitable screening techniques for plot, or pass/fail map with user oxytetracycline (OTC). OTC is a solids since it is fast and non- defined criteria. basic compound for the destructive and abundant production of various types of information can be revealed from Brett Cooper, Merck Sharpe & antibiotics, however it is unstable the diffraction pattern. A two- Dohme and Neil Feeder, Pfizer

19 Forthcoming BCA Meetings September 2001

Glass Content of Ground Dr Jonathan Steed (King's Forthcoming Granulated Blast Furnace Slag College, London) Ian Slipper, University of 'Crystal Frustration - and how to BCA Meetings Greenwich Avoid It'

Industrial Group: Standards for Line Profile Analysis Professor Richard Winpenny Steve Norval, ICI plc. (University of Manchester) Autumn Meeting - 'Studies of High Nuclearity 3d- Crystallography in Optional visit to the Pilkington Metal Cages with Unusual Industry Exhibition Area at 9.30 or during Magnetic Properties' Thursday 1st November 2001, lunch 10am- 4pm The Pilkington Exhibition area is A registration form is included with this newsletter. Full details Pilkington, Lathom, Lancashire well worth a visit. The 9:30 option including a registration form are will suit those people staying also on the CCG pages of the BCA Welcome and Introduction overnight in local hotels. The website. The local organiser is Jack Brettle, Head of Science exhibition covers glass Carl Schwalbe (e-mail: Support, Pilkington manufacture and the innovative [email protected]). use of glass in a diverse range of Parking on site is limited, and the Crystallography and X-ray products. A registration form is use of public transport or car- Reflectometry at Pilkington included with this newsletter. For sharing is encouraged. Mark Farnworth, Pilkington more information contact Judith Participants who need car parking Shackleton (e-mail: space should contact the GADD Sir! 21st Century Tools of [email protected]) local organizer directly. the Trade - Applications of XRPD in the Characterization of Offers of short presentations Pharmaceuticals Chemical Crystallography (particularly by post-graduates Anne Kavanagh, AstraZeneca, Group: Autumn Meeting and post-doctoral workers) at the Macclesfield Mesomolecular meeting should be sent to the crystallography scientific session organiser, XRD Studies on the Thermal Wednesday November 14 - 2001, Stability of Electrodeposited 10.35am - 4.15pm, Professor Paul R. Raithby, Nanocrystalline Nickel Aston University Department of Matthias Abraham, University of Chemistry, University of Bath, Oxford. The meeting will focus on Bath BA2 7AY, Tel: (01225) methods and experiences of 826444 Fax: (01225) 826231 Microstructure and Performance structure solution, refinement E-mail: [email protected] of Materials. and results for large small Keith Rogers, Cranfield University molecules. Invited speakers include; Presentation of an Industrial PCG Workshop Group Award to Ian Langford Introduction to the Dr Andrew Burrows (University of Principles and Practice of Bath) Rietveld Refinement Award Lecture - Zinc Oxide 'Co-ordination and Hydrogen Ian Langford, Honorary Senior Bond Interplay in Supramolecular IMPORTANT - CHANGE OF DATE Research Fellow, Birmingham Network Formation' University and VENUE Professor Martin Schroder Please note that this Workshop Applications of XRD in the (University of Nottingham) will now be held as a Satellite Imaging Industry 'Construction of Framework meeting to the BCA Spring David Beveridge, ILFORD Imaging Polymers: Catenates, Helicates Meeting 2002, at the University of UK Ltd and Porous Materials' Nottingham.

20 Forthcoming BCA Meetings September 2001

The workshop will take place • data collection strategies, covered will be: high-pressure immediately prior to the BCA including angle- and energy- single-crystal diffraction in the meeting, on Sunday 24 and dispersive techniques with both laboratory using point and area Monday 25 March, 2002. The X-ray and neutrons; detectors; developments in high- Workshop will conclude at the • basic refinement strategies - pressure single-crystal and powder start of the main BCA meeting at how to give yourself the best neutron diffraction; state-of-the- lunchtime on Monday 25 March. chance to get the right result; art high-pressure powder- Full details are still being finalised • an introduction to some of the diffraction at synchrotron sources; and will appear on the Workshop software suites available. high-pressure EXAFS; and WebPage: opportunities in high-pressure http://www.isis.rl.ac.uk/Crystallogra Speakers will include Bill David spectroscopy. phy/RietveldWorkshop.htm (ISIS/UCL), Jeremy Cockcroft (Birkbeck) and Kevin Knight (ISIS). Speakers will include: With this meeting the PCG will Further details will be announced • Andy Jephcoat (Oxford) - begin a series of tutorial on the meeting Web site as they Raman Studies of Bonding workshops on powder diffraction develop. Under Pressure profile refinement methods. This • Dave Keen (ISIS) - High-Pressure technique, much used and a vital Contact the organiser Chick Wilson Single-Crystal Neutron component of much of physical ([email protected]) for more Diffraction crystallography, is very powerful details. • Bill Marshall (ISIS) - Neutron but if improperly used can lead to Powder-Diffraction at High- problems both in the refinement Pressure process itself and in the resulting BCA Physical • Mohamed Mezouar (ESRF) - structural models. The aim of these Crystallography Group High-Pressure Powder- workshops is to provide a general and the IoP Structural Diffraction Using Synchrotron introduction to the method and its Condensed Matter Physics Radiation applications. They are aimed both Group • Simon Parsons (Edinburgh) - at those new to the technique, Uses of Area Detectors in Single- particularly research students and Autumn Meeting Crystal Diffraction at High post-docs, and those who feel the Applications of high pressure in Pressure need for a refresher. structural studies. Hosted and supported by the Registration will be free and local The first of these workshops will be Daresbury Laboratory. accommodation will be available if held on 24 & 25 March, 2002, at Daresbury Laboratory, required. The deadline for receipt the University of Nottingham, as a 5 December 2001 of registrations will be 16 Satellite meeting to the BCA 2002 November, but please register Spring Meeting. It will introduce This one-day meeting will cover earlier if you require the basics of profile refinement the wide-ranging applications of accommodation. using the Rietveld method. The high-pressure techniques in the workshop will include introductory study of crystal structure. The For more information on the lectures, demonstrations and meeting will include scientific meeting contact the organiser: hands-on examples. Topics will presentations, accounts of the Dave Allan (The University of include: latest technical advances in Edinburgh; [email protected]) or pressure techniques for both X-ray the PCG Secretary Chick Wilson • principles of Rietveld and neutron diffraction and also (C.C. [email protected]). Full details refinement, including spectroscopy, and the opportunity and an on-line registration form minimisation; to view some of the advanced are available on the meeting • crystal structure refinement and high-pressure kit currently being website: what it achieves, including the made available in laboratories and http://www.isis.rl.ac.uk/crystallogr use of constraints and restraints; central facilities. Among the topics aphy/HighPressureMeeting.htm

21 Corporate Membership September 2001

Other Meetings of Corporate Members Interest Astex Technology International Centre for If you have news of any meetings Diffraction Data Bede Scientific Instruments Ltd to add to list please send them to Molecular Structure the BCA Web Master Bruker/Nonius Corporation [email protected] or to the Editor, Cambridge Crystallographic Oxford Cryosystems [email protected] Data Centre Philips Analytical October 18 2001 Hampton Research Frontiers in Crystal Structure Analysis, (Annual Meeting of the Swiss Society for Crystallography), Yverdon, Switzerland, 18th October 2001 BCA Corporate Membership [Details via IUCr website] The BCA values its close ties with commercial companies involved October 22-26, 2001 with crystallography. To enhance these contacts, the BCA is pleased International Symposium on Crystal to announce that they are now offering Corporate Membership. Chemistry of Coordination, Organic and Supramolecular Compounds. Corporate Membership is available on an annual basis running from Moldova, 22-26 Oct 2001. [website 1 January to 31 December and includes the following benefits: http://phys.asm.md/ISCrChem] • Up to 10 free BCA memberships for your employees. October 25-27, 2001 Pittsburgh Diffraction Conference, • A 10% discount on exhibition stands at the annual Spring Cincinnati, Ohio, USA, 25th - 27th Meeting. October 2001[website http://www.che.uc.edu/Chemistry/PDC/ • Free insert in the annual Spring Meeting delegate bag. Pdc.htm] • Two free full registrations to the annual Spring Meeting. March 4-7, 2002 10th Annual Meeting of the German • Ten complimentary copies of the quarterly BCA Newsletter. Society for Crystallography (Deutsche Gesellschaft fuer Kristallographie / • Corporate Members will be listed in every BCA Newsletter and DGK) Kiel, Germany [Details from IUCr on the BCA Web Site with links to your corporate site. website] The cost of this membership is £600.00 per annum March 23-28, 2002 9th International Conference on the Crystallization of Biological To apply for Corporate Membership, or if you have any enquiries, Macromolecules, Jena, Germany, please contact: [website http://www.conventus.de/iccbm9/] BCA Administrative Office Northern Networking Ltd March 25 - 28, 2002 Bellway House BCA Annual Meeting, Nottingham 813 South Street University (Full details in December Glasgow issue) G14 0BX

August 6 - 15, 2002 Phone 0141 954 4441 XIX Congress of the International Fax 0141 954 2656 Union of Crystallography, Geneva, e-mail [email protected] Switzerland [email: [email protected]]

22 The 2001 Walter Hälg Prize PCG/SCMPG Bursaries

The 2001 PCG/SCMPG Bursaries Walter Hälg Prize The PCG welcomes bursary applications from BCA or IoP The recipient of the 2001 members who are affiliated to the ENSA/Hälg Prize will be Professor PCG or to the Structural Jane Brown of the Institut Laue Condensed Matter Physics Group Langevin, Grenoble, in of the IoP. These are intended recognition of her outstanding mainly to help young scientists contributions to the science of (students and post-docs) to attend neutron scattering over the last meetings and conferences four decades. The prize is to be relevant to PCG/SCMPG areas of presented at a special session of interest. Bursaries can be applied the International Conference on Professor Jane Brown for at any time, through the Neutron Scattering, to be held in PCG/SCMPG Secretary Munich between 9-13 September She first became interested in the ([email protected]) and will be application of polarised neutrons considered by the Group Professor Brown has made a in the early 1960s whilst spending Committee. However, each year significant impact upon our two years at Brookhaven National we expect to target selected understanding of the Laboratory in the US. Returning to meetings as highly relevant for fundamental magnetic properties Cambridge as a senior assistant in the award of bursaries. of materials through her research and subsequently contributions to both the assistant director of research in Applications for bursaries are development and exploitation of the Cavendish Laboratory and expected to be received by the polarised neutron diffraction and fellow and lecturer in Physics at PCG Secretary at least two weeks advanced spherical neutron Newnham College she forged prior to any early registration polarimetry techniques for the close links with Harwell, where deadline - more details of precise determination of complex she established a programme in deadlines will be publicised on the magnetic structures and spin neutron diffraction. In 1972 she PCG Website. Recipients of density distributions. She has was appointed as Senior Scientist bursaries are expected to write a played a key role in developing in charge of the Diffraction Group brief report on the relevant and establishing a computational at the Institut Laue Langevin, meeting, and may be asked to framework, namely the extremely Grenoble. She received a report on a particular session. powerful and extensively used Gulbenkian Visiting Professor Cambridge Crystallography Appointment to work at the PCG Website: Subroutine Libraries (CCSL), to University of Coimbra, Portugal, in http://bca.cryst.bbk.ac.uk/bca/PCG facilitate structure determination the early 1990s and has also been /pcg.html from crystalline diffraction. a Visiting Professor at Professor Brown is also very well Loughborough University in known to the European neutron England for several years. scattering community for the Although formally retiring from expert guidance, support and the Institut Laue Langevin in 1995, training in single crystal and she continues to run an extremely magnetic diffraction that she has active research programme, whilst tirelessly provided at the Institut also remaining a very popular Laue Langevin over the last thirty local contact for user experiments. years. Professor Bob Cywinski Professor Brown is a graduate of Chairman of ENSA Cambridge University, England. University of Leeds, UK

23 CLRC e-Science Centre Mineralogy Database

CLRC e-Science Centre to researchers in the UK who wish to Mineralogy Database run UK Grid Support Centre use the Grid in their work. The Centre will also be producing a This mineral database website The CLRC e-Science Centre has report consolidating the contains more than 5,000 web been invited by Tony Hey, the experience of all 3 partners with pages of mineral data. It includes Director of the e-Science Core the current generation of Grid selected mineral definitions and Programme, to set up and manage tools. mineral pictures. There are 4,205 the Grid Support Centre for the individual mineral species UK on behalf of the programme. For more information see website descriptions with links. Mineral The CLRC e-Science Centre has also http://www.e-science.clrc.ac.uk data on individual species are received funding from OST to linked to a mineral table by develop a Grid infrastructure for crystallography, X-Ray powder its own experimental, computing Size Strain – III diffraction, chemical composition, and data facilities in support of its Analysis of microstructure and physical and optical properties, user community. residual stress by diffraction Dana's new classification, Strunz CLRC has invited Edinburgh and methods classification, and alphabetical Manchester Universities to listings of mineral species. Links to participate in the Support Centre December 2-5, 2001, TRENTO - ITALY other sources of mineral data to ensure that the Centre has Information, on-line registration, available on the WWW are also access to the best experience on-line hotel reservation, included. Website address: currently available in the UK on instructions for authors, abstract http://webmineral.com Grid middleware and services. submission, programme and updates are available only When it is operational, the Centre through the conference web-site: will provide a range of services to http://bragg.ing.unitn.it/sizestrain

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