The new European X-ray Free-Electron Laser is the first X-ray free-electron laser capable of delivering X-ray pulses with a megahertz inter-pulse spacing, more than four orders of magnitude higher than previously possible. However, to date, it has been unclear whether it would indeed be possible to measure high-quality diffraction data at megahertz pulse repetition rates. Here, we show that high-quality structures can indeed be obtained using currently available operating conditions at the European XFEL. We present two complete data sets, one from the well-known model system lysozyme and the other from a so far unknown complex of a β-lactamase from K. pneumoniae involved in antibiotic resistance. This result opens up megahertz serial femtosecond crystallography (SFX) as a tool for reliable structure determination, substrate screening and the efficient measurement of the evolution and dynamics of molecular structures using megahertz repetition rate pulses available at this new class of X-ray laser source.

A description of the 1 million pixel AGIPD system in use at the SPB beamline of the European XFEL is given.

Serial femtosecond crystallography (SFX) with X-ray free electron lasers (XFELs) allows structure determination of membrane proteins and time-resolved crystallography. Common liquid sample delivery continuously jets the protein crystal suspension into the path of the XFEL, wasting a vast amount of sample due to the pulsed nature of all current XFEL sources. The European XFEL (EuXFEL) delivers femtosecond (fs) X-ray pulses in trains spaced 100 ms apart whereas pulses within trains are currently separated by 889 ns. Therefore, continuous sample delivery via fast jets wastes >99% of sample. Here, we introduce a microfluidic device delivering crystal laden droplets segmented with an immiscible oil reducing sample waste and demonstrate droplet injection at the EuXFEL compatible with high pressure liquid delivery of an SFX experiment. While achieving ~60% reduction in sample waste, we determine the structure of the enzyme 3-deoxy-D-manno-octulosonate-8-phosphate synthase from microcrystals delivered in droplets revealing distinct structural features not previously reported.

Flame spray pyrolysis (FSP) is a novel technique for the fabrication of nanostructured catalysts with farreaching options to control structure and composition even in cases where complex composites need to be prepared. In this study, we took advantage of this technique to synthesize highly dispersed pure and Pddoped iron oxide nanoparticles and investigated them as Fischer-Tropsch (FT) catalysts. By systematically varying the Pd content over a large range from 0.1 to 10 wt %, we were able to directly analyze the influence of the Pd content on activity and selectivity. In addition to catalytic measurements, the structure and composition of the particles were characterized before and after these measurements, using transmission electron microscopy, adsorption measurements, X-ray diffraction, and EXAFS. The comparison revealed on the one hand that small Pd clusters (diameter: 1-2 nm) evolve from initially homogeneously distributed Pd and on the other hand that the iron oxide transforms into iron carbides depending on the Pd content. The presence of Pd influences the particle size in the pristine samples (8-11 nm) resulting in specific surface areas that increase as the Pd content increases. However, after activation and reaction the specific surface areas become similar due to partial agglomeration and sintering. In a fixed bed FT reaction test, enhanced FT activity was observed with increasing Pd content while the selectivity shifts to longer chain hydrocarbons, mainly paraffins. Mechanistic implications regarding the role of Pd for the performance of the catalysts are discussed.