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Final Report

NATO Advanced Study Institute Erice, Sicily, June 2013.

Title: The Future of Dynamical Structural Science - links to Energy and Environmental Security and Early Detection of CBRN Agents

The NATO supported ASI entitled "he Future of Dynamic Structural Science - links to Energy and Environmental Security and Early Detection of CBRN Agents"
was held from the 30 th May 2013 to the 8 th of June 2013 at the Ettore Majorana Foundation in Erice, Sicily.

 

The course programme consisted of a mixture of lectures, some software demonstrations by the teaching staff, followed by hands-on workshops for participants. There were also poster presentations and talks by the participants on the course. In total 43 lectures were given by the teaching staff and these comprised a combination of various crystallographic and spectroscopic techniques with some cutting edge research results, to show the strength and breadth of the subjects under discussion. Ten international students were selected to give 25 minutes talks based on their submitted abstracts and these were chosen to represent the breadth of subject areas within the overall course. The participants presenting posters did so in two separate evening sessions and previously they gave a short [2 minutes] overview of their presentation and thus invited the audience to discuss their science at these two evening poster sessions.

Objective

The main objective of the course was to increase the knowledge of younger scientists in the required modern crystallographic and spectroscopic techniques that are essential for them to work successfully in the field of dynamical structural science, bridging the traditional scientific disciplines of chemistry, biology, physics, mathematics and engineering.

Lecturers

The program included presentations by world leaders in the fields of time-resolved crystallography and spectroscopy. Since time-resolved diffraction relies heavily on the results of time-resolved spectroscopic studies to inform the detailed experimental conditions, this multi-disciplinary programme which we had created, was felt to be essential to provide the next generation of scientists with the skills to work in this emerging field. The feedback from the students on this aspect of the program was that it had been hugely beneficial to them and represented an exciting challenge for the future. Most of the speakers gave two full lectures, which were a carefully balanced combination of introducing techniques from a theoretical perspective, through discussing current experimental methodologies and data processing to a presentation of recent results to illustrate the application of their technique. Approximately a third of the lecturers were also involved in giving demonstrations and workshops on appropriate software related to and essential for each technique. Many speakers also acted as Chairpersons for the sessions throughout the week.

Programme

The course was designed to provide an introduction to each technique with the lectures presenting both reactions from the slower (micro/milli) second timescales up to very fast (femtosec) studies and covering investigations into both chemical and biological species.

On the first evening, Martin Schmidt also gave a brief introduction to some of the historical sites within Erice and the associated long history of the town, in order to inform and also to orientate the students who had just arrived and who had had no time to explore the complex layout and narrow streets of Erice.

Paul Raithby presented the first lecture of the week, based on time resolved chemical crystallography, but he also gave a brief overview of the course. There followed an introduction into the study of metastable chemical species, discussing some of the experimental approaches they have used to study linkage isomerism of M-NO 2 complexes and how to maximise the conversion from one stable state to another. Paul struck the right note in balancing teaching content with research results and choosing a speed of delivery that we hoped all of our speakers would follow. Elena Boldyreva presented a very interesting background to the dynamics of structures studied by diffraction techniques under pressure and with appropriate historical notes to capture the recent background for the students and a clear overview of the technique and its importance as a modern sample environment. Paul McMillan's presentations were complementary to Elena's, since the applications themselves differed, the pressures were in general higher and in addition he showed his latest work in the biological areas and discussed their future development with some excitement for future challenges. Menahem Kaftory presented some elegant and careful studies on single crystal to single crystal transformations under the influence of different light sources. Martin Meedom Nielsen presented a rigorous introduction to the X-ray scattering from liquids, describing the molecular form factors derived and how much can be extracted from these advanced, time resolved experiments. Eric Collet described the study of photo-excited chemical species by X-ray diffraction and showed how the optical and magnetic properties for example can be related to these results and described some results of interesting phase changes. Yuji Ohashi gave very careful and detailed presentations of some of his early work in this area but with detailed descriptions of how the results relate to the properties with some fascinating new results. Simone Techert was able to discuss the importance of understanding the broad range of time scales that we are hoping to study in these time resolved experiments and how these relate to the chemical reactions we observe. Yasushi Koyama had volunteered a talk in a closely related area and he was selected from the participants to discuss his science and Marco Cammarata is a young scientist working in an exciting new area - the XFEL - whom we promoted to a longer talk, when a senior colleague was unable to attend at the last minute. The majority of the lecturers, in these predominantly crystallographic talks, emphasised the need for very accurate time-resolved spectroscopic data to understand the moderated molecular properties driven by changing sample environments. These data together with careful kinetic measurements inform the specific experimental conditions and are thus required prior to undertaking any high resolution crystallography studies.

As well as the various dynamical diffraction methods, a range of spectroscopic techniques were the subject of several of our speakers, including time-resolved absorption and Raman spectroscopy, XAFS and fluorescence spectroscopy. Siva Umapathy presented an introduction to time-resolved absorption and Raman spectroscopy linking the techniques into results obtained within his group. One approach discussed was stimulated Raman spectroscopy which can increase the intensity of the weak Raman signal and improve the spatial resolution of the technique. However, probing on the Stokes side is often not possible for highly fluorescent samples but such samples can be effectively studied by ultrafast Raman loss spectroscopy probing on the anti-stokes side. Paul Carey also spoke about Time-resolved Raman spectroscopy but at the interface of chemistry and biology, explaining extremely well for the novice students how the transition of applying techniques in a new area can be made successfully and also the challenging use of the Raman microscope. Ken Ghiggino introduced time resolved emission and absorption spectroscopy in his first talk, reminding the students of the underlying theory in a very accessible manner, moving on in his 2 nd talk to time resolved fluorescence microscopy, super resolution microscopy and single molecule spectroscopy Matteo Rocco, one of the participants, kindly stepped in to provide and introduction to XAFS when Moniek Tromp was unable to attend at the very last minute due to sickness. He also discussed some of their recently obtained experimental results on fibrinogens and was able to demonstrate some new software, SOMO, to small groups of students after his lecture, which was very well received.

In the lectures that were predominantly concerned with biochemical and biological studies, students were exposed to the details of the technique, where these might differ and why different aspects of the experiments were important compared to time resolved work on chemical compounds. Arwen Pearson presented two very accessible lectures on the ‘how to do' real experiments at the synchrotron, with particular reference to biological samples, but with obvious overlap with chemical applications. She took this into the future with her 2 nd talk explaining what we should be able to do in the very short time scale regime using new methods and in particular new ways of analysing the vast amounts of data recorded. Vukica Srajer was able to show how to plan and execute time resolved synchrotron experiments for macromolecular crystallography and from these how to determine the structures of important biological intermediates. Michael Wulff presented ways to look at capturing time resolved scattering (liquids) and diffraction (crystals) using a pulsed X-ray beam, created by the use of mechanical choppers, linked with a pulsed laser system, leading to the ‘finger printing' of reaction intermediates. Pierre Thibault introduced the background theory to a subject which was new to many of the students, of X-ray Coherent Diffraction Imaging and showed where this was taking us as XFEL sources increasingly come on line. Marvin Seibert described methods being developed to overcome radiation damage, which can be significant for biological samples and the application of very fast diffraction experiments in the study of liquids, or a liquid jet that contains very small crystalline particles at the new XFEL sources. He explained how these advanced experiments are still under development and how important is the fine tuning of the technical details together with very fast mega-data acquisition software, in order to obtain meaningful results.

Student presentations, selected from the submitted abstracts, were given by 10 of the participants on a range of topics and were all of a really high standard. Jose Trincao discussed the work of the dynamic structural science consortium in the UK, including the use of statistical methods to tackle combining data from multiple crystals after photo-activation. Anton Targonsky described a method for ultrasonic modification to explore crystal defects; Matthew Robinson discussed the table top time resolved electron diffraction equipment that had just been built in his home laboratory. Davide Altamura showed how you can use grazing incidence SAXS to explore nanostructured materials; Surajit Kayal presented some of his Raman studies including the results of Raman loss spectroscopy. Jonathan Hanson explored the simultaneous use of diffraction and IR spectroscopy to study catalytic reactions in situ and Matteo Levantino presented the results of time-resolved X-ray scattering into protein structural dynamics. Hideyuki Miyataku talked about the development of a dynamic light scattering based protein crystallisation equipment and early successful results. Eleonora Conterosito discussed her work using fast in-situ powder X-ray diffraction examining layered double hydroxides and Gyula Faigel took us into the world of XFEL showing models of how ultimately we should be able to study the dynamics of single molecules using intense, short, X-ray pulses. As mentioned above, poster presenters gave very brief oral overview of their science to the rest of the participants to encourage people to visit their poster for further discussion. Indeed the two poster sessions provided an excellent opportunity for the students to interact both scientifically and socially. Prizes were awarded to Maike Joester (Germany) and Ahmed Mabied (Egypt) for the best two posters presented during the meeting and we commended three others Joshua Hill (UK), Nikita Marchenkov (Russia) and Franziska Pinker (France) as the standards were really excellent. The Lodovico prize was shared this year between Eleonora Conterosito (Italy), Matt Robinson (UK) and Alexander Theodossis (Australia).

Judith Howard, Hazel Sparkes

A complete survey of the questionnaire can be found here.

Awards

Participants awarded during the closing ceremony: (from left to right) Hazel Sparkes, Alexander Theodossis, Matthew Robinson, Maike Joester,
Joshua Hill, Franziska Pinker, Ahmed Farghaly, Judith Howard, Nikita Marchenkov, Annalisa Guerri, Paola Spadon and Eleonora Conterosito.