The 2010 Spring meeting of the BCA was held at Warwick University and brought together over 270 delegates from across academia and industry for three days of thought and talk on the subject “data matters.” The conference was organized with three simultaneous programs covering biological, chemical, physical, and industrial crystallography. A young crystallographer (YC) satellite meeting was held prior to the main meeting, and 14 or so YCs gave talks on their research projects across a wide range of disciplines. The following summarizes the sessions organized by the Industrial Group (IG).

The IG organized four lecture sessions on the subjects of data—what goes in; data—what comes out, complementary and nonambient techniques, and unpublished data and almighty blunders. The IG also held an Alun Bowen memorial lecture, given by Dave Taylor, and a teaching plenary lecture, given by Simon Billinge. The IG session organizers would like to thank all our organizers for their contributions.

David Taylor [ICDD and Pilkingotns (retired)] gave the Alun Bowen lecture, titled “Phase Identification—How it’s Changed Over the Years.” Taylor first paid tribute to Alun Bowen who, as Chair of the Industrial Group, encouraged the Taylor involvement in the BCA. In this fascinating talk, Taylor described his career in industrial crystallography with Pilkington’s glass and the application of new crystallographic techniques, such as hot-stage XRD and X-ray reflectivity in the glass industry. In keeping with the conference theme, most of Taylor’s talk described how the collection and sharing of data have developed over the years, from Roentgen’s discovery of X-rays and the first commercially available Debye-Scherrer cameras (1918). Taylor described the developments of the “Hanawalt” search based on the three most intense d spacings using data stored as a card index (initially handwritten!) through to today’s ICDD database which contains over 700 000 data sets, includes organic and calculated powder data, and is expected to increase at 30 000 entries per annum. Following Taylor’s lecture, the ICDD held a hands-on workshop in which participants were introduced to phase identification of single components and complex mixtures using PDF-4.

Taylor’s contribution to industrial crystallography and commitment to the BCA (including serving as Treasurer of the BCA and Chairman of the Industrial Group) have been recognized by the award of Honorary Membership of the BCA, which was presented to Taylor by Elspeth Garman, President of the BCA, at the conference dinner.

Elspeth Garman, President of the BCA, awarded Honorary membership to Dave Taylor.

Simon Billinge (Michigan State University) gave the teaching plenary, “Structure at the Nanoscale: Atomic Pair Distribution Function Analysis of Nanostructured Materials.” The teaching plenary is always an excellent opportunity to learn about new techniques, and this year was no exception. Billinge explained how the Bragg peaks are blind to order on the nanoscale but that diffuse scatter can be used to probe the nanoscale. In a delightful look back to some of the first diffraction data ever collected, Billinge showed a page from the Bragg notebook (available on the website of Leeds University: http://www.leeds.ac.uk/library/spcoll/bragg-notebook/pdf.htm). The information on short range structural order of a variety of materials was extracted using the pair distribution function (PDF), providing enough information to fingerprint and in some cases determining the local structure. PDF has been applied to crystalline materials but also promises to be an invaluable tool for understanding the local structure of “X-ray amorphous” structures. Case studies included characterizing stacking faults and stress within CdSe “quantum dots,” structure determination of buckyball (C60), and domain size and characterization of amorphous carbamazepine. PDF is a technique that can be run on synchrotron or laboratory sources and is steadily moving from its academic origins into industrial applications.

Matt Johnson (GSK) chaired the session “Data: What goes in” in which three speakers shared their wealth of knowledge on the collection of high quality diffraction data. Ross Harrington (Newcastle University) spoke on “Getting the Best Possible Data from Your Crystals,” giving a guide on what to look for in crystals before, during, and after X-ray analysis. The basic subjects, such as what a suitable crystal looks like, choice of radiation, and dealing with twinned data sets and other common problems, were covered. Harrington gave many tips on single crystal analysis, such as leave your solution NMR samples at the back of the fume hood and see if anything crystallizes, keep single crystals in the growth medium until just before mounting, trust the data not the molecular structure supplied with the sample, sanity check the unit cell against known structures, and use your chemical knowledge as well as crystallography. Finally, a tip echoed by a later speaker: maintain your diffractometer well!

Sarah Barnett (Diamond Light Source) then gave a “Rough Guide to Synchrotron Diffraction,” explaining the advantages of using the I19 beamline rather than a laboratory diffractometer for small molecule single crystal diffraction. The synchrotron’s higher flux and tunable energies make for high speed data collection even when the crystals are small or of poor quality. The impact on the data is higher resolution combined with rapid data collection. A further benefit of the synchrotron is the robots that can be used to mount and align crystals efficiently. Barnett advised future users of Diamond on how to make the best use of their beam time by preparation beforehand (possibly in consultation with Diamond staff) and monitoring the storage ring status during data collection.

The final speaker in this session was Alastair Florence (University of Strathclyde) who spoke about “XRPD Data in Physical Form Identification and Structure Determination.” Florence began by discussing the importance of physical forms to the pharmaceutical industry and the role XRPD plays in this. He set out his thoughts on maximizing the chances of success when using XRPD for fingerprinting, phase identification, and structure determination. He recommended checking the calibration of the diffractometer using an in-house standard over a variety of angles, as well as the common industry standards, grinding the sample lightly before analysis (a drawback of high throughput screens being the lack of opportunity to grind the samples), and careful sample mounting and alignment in order to get the best possible data. Florence explained the data collection process for structure determination and presented examples of solving structures using the DASH software. His results showed that although the crystal structure obtained was often close to the actual structure, it was not always as accurate as we would like. He then demonstrated how software tools such as Mogul can improve the accuracy by using CSD data to generate probability distributions for bond angles, lengths, and torsion angles and applying constraints based on these distributions.

Brett Cooper (MSD) and Cheryl Doherty (Pfizer) were cochairs of the next session, Data: What Comes Out. Trevor Rayment (Diamond) gave an overview of the capabilities of the Diamond synchrotron, “Food, Formulation, Foams and Fabrication—Modern Applications of Synchrotron Radiation for Industry.” Rayment introduced synchrotron radiation as an essential tool for scientific research in the 21st century. He gave as an example the massive increase in the number of biological structures deposited in the databases, thanks to the use of synchrotron radiation. Rayment is keen to enable industrial use of the synchrotron and emphasized that the synchrotron is ready to use, which waiting times are short, data acquisition is rapid, and technical support and advice are available. Rayment also described some recent developments at Diamond including real-time analysis of samples using the Pilatus detector and the use of remote control operation.

The second talk of the session was presented by Robert Hammond (University of Leeds). His talk was entitled “A Molecular-Scale Perspective: New Insights into the Assembly of Crystalline Particles.” Hammond started by discussing the drive to understand materials properties and that it is possible to apply molecular modelling techniques with inputs from crystallography to achieve this. He introduced the use of a molecular mechanics approach to model the critical clusters of the growth phase in nucleation. He then showed that it is possible to use these techniques to further explore the intermolecular interactions of prenucleation clusters with a variety of different solvents.

The third and forth talks of the session were the winner and the runner up of the Industrial Group Prize awarded to the best Industrial Relevant Presentations from the Young Crystallographers Meeting held prior to the main meeting.

The winner of the prize was Mark Eddlestone (University of Cambridge) for his talk “Analysing Pharmaceutical Materials by Transmission Electron Microscopy (TEM).” Eddlestone introduced the technique of TEM and highlighted some of the issues including the difficulties involved in sample preparation and stability in the electron beam. He went on to describe how the technique could be applied to the analysis of pharmaceuticals including obtaining information on morphology, phase ID, as well as crystal structure and defects. He described how individual crystals could be examined and phase determined with a possible application to patent infringement cases.

The runner up of the Industrial Group prize was Jonathan Foster (University of Durham) with his talk “Supramolecular Gels: A New Medium for Crystal Growth.” Foster described a new range of bisurea gel forming agents that could be used as a medium to grow crystals. He described the advantages conferred by growing crystals in the gels: by slowing down crystal growth it may be possible to form the thermodynamically stable form, in contrast to rapid growth in other media, in which a thermodynamically metastable form may predominate. The gel structures can easily be broken up by the addition of a gel disrupting agent such as a simple anion. Once disrupted the crystals could then easily be recovered by filtration and could be used for single crystal studies. By varying the type of gel formers and the solvents it may be possible to grow a variety of crystalline phases.

The session on “Complementary and Non-Ambient Techniques” was chaired by David Beveridge (Harman Ltd.). Tim Hyde (Johnson Matthey) opened the session with a talk called “Catalysis Studies using Complementary Techniques at Johnson Matthey.” Hyde highlighted that his company’s approach is to collect data under conditions as close to those under which the catalyst operates as possible; these conditions can be as extreme as 1400 °C and 100 bar; and data need to be collected with appropriate time resolution and to give information over relevant length scales. The techniques used include high temperature and pressure XRPD, XRPD with evolved gas analysis by mass spectrometry, TEM, photoelectron spectroscopy for depth profiling, and solid state NMR. Synchrotron-based techniques such as SAXS, XAS, and total scattering are also used.

Axel Zeitler (University of Cambridge) gave the second talk of the session: “Terahertz Spectroscopy of Structure and Dynamics in Organic Molecular Crystals.” Zeitler introduced the technique, which is a vibrational spectroscopy in the far IR region, between IR and microwaves. At these frequencies the vibrational spectrum is dominated by intermolecular lattice modes and hydrogen-bonding modes, so that terahertz spectroscopy is a tool to study the interactions between a molecule and its crystal structure. Zeitler described how terahertz spectroscopy could be used in polymorphism and solvation studies and illustrated his talk with several case studies. Terahertz spectroscopy was used to monitor the phase transition of carbamazepine form III to form I at 433 K and to quantify the phases present. In another case, terahertz spectroscopy was able to detect differences between structures where XRPD could not and was used to understand the formation of cocrystals of theophylline with malic acid, as either the racemate or the L-enanatiomer.

The final talk of this session was given by Simon Watson (GSK) and called “Running Hot and Cold—Understanding Crystal Structure Phenomena with Variable Temperature Solid State NMR.” Watso introduced the technique of ssNMR and explained how data could be collected over the temperature range of 153 to 400 K, which allows some phase transitions to be studied. He showed how ssNMR can readily distinguish different polymorphs, hydrates, and solvates and complementary to XRPD in that forms which may be difficult to distinguish by XRPD can be very readily distinguished by ssNMR. A further use of ssNMR is to give the number of molecules in the asymmetric unit cell, again a complementary use to XRPD. Watso gave three case studies of the application of ssNMR in the pharmaceutical industry, including one in which ssNMR was used to determine whether extra peaks seen in the XRPD pattern were due to the presence of a second polymorph or deviations in the crystal packing caused by changes in molecular orientation.

The final IG session was run jointly between the IG and the Chemical Crystallography Group and was chaired by Richard Morris (Morris analytical X-ray) and Luca Russo (University of Newcastle). The meeting ended with this light-hearted but nevertheless highly informative set of talks. Bill Clegg (University of Newcastle) started the session with a talk entitled “Reasons Good and Bad for Not Publishing Crystal Structures.” He examined the barriers to sharing crystal structures despite the fact that publication is not the only route; simple deposition in a suitable database can be enough to share the data. Sometimes good quality data are lost to the wider community because of commercial or confidentiality constraints. However, many crystal structures are not and should not get into the public domain because they are not fit for purpose: reasons for this range from poor quality data, incompetence, and misinterpretation of the data.

The second talk in this session was given by Simon Coles (University of Southampton) on “eCRYSTALS: Management and Publication of Small Molecule Data.” Coles described the Southampton eCRYSTALS repository for crystal structures. This is a response to the need for rapid dissemination of new crystal structures in an age when a student can solve about five structures in one day, as opposed to the whole of their PhD, as was the case 30 years ago. The eCrystals repository allows rapid access to the data in a form in which it is possible to directly check the correctness and validity of the structure. It is hoped that a network of these repositories can be established across international boundaries.

The final speaker was Colin Groom (CCDC) who gave an amusing account of some of the errors he had encountered in structures submitted to the CCDC. At the same time, he assured the audience that all mistakes would be kept anonymous and encouraged us to submit structures whenever possible. Among the errors mentioned were S and P atoms swapped, too few or too many atoms in a molecule, a CN group that should be CO, and confusion between the use of °C and Kelvin (the CCDC default is to use K). Groom concluded by describing the perils of unexpected discovery of a new polymorph, particularly in the pharmaceutical industry.