First Light: TBA (2024/2025)
Single crystal X-ray diffraction is the preferred technique to solve the atomic structure of a crystalline material. It is now a routine technique in many research laboratories, however, the limited flux, spectral purity and focusing ability of a lab-source severely limits the size and quality of the crystals that can be measured. Moreover, many materials do not grow crystals that are large enough to be studied in-house. Synchrotrons can close this gap; however, they are not commonly used for routine small molecule crystallography due to the additional technical expertise required and long lead times in the proposal-based access policy.
The SINCRYS project is funded by the Danish Ministry of Education and Research and was officially started on the 1st of January 2022, with the aim of building a simple small molecule single crystal diffractometer as a side branch to the DanMAX beamline at MAX IV. It is funded by ‘Nationalt Udvalg for Forskningsinfrastruktur’ (NUFI) under the Ministry of Higher Education and Science. SINCRYS is headed by Aarhus University and is performed in collaboration with MAX IV (Lund University). The project has a total budget of ~52 MDKK. The purpose of the instrument to acquire high resolution 3D atomic structure data of crystals with dimensions of just a few micrometres. Due to the fundamental nature of the derived structural information, the instrument will serve an extremely broad research community in academia as well as industry and spans from bioscience and pharmaceutical sciences across chemistry, materials and geoscience to solid state physics. Exploration of new materials is indispensable e.g., for attaining sustainability, and continuous materials development is essential for maintaining a competitive Scandinavian industry. The instrument will expand the available techniques at MAX IV and complement the BioMAX and MicroMAX beamlines where the focus is on high-throughput macromolecular crystallography. SINCRYS will be tailored for smaller unit cells commonly found in organic molecular crystals, inorganic materials and hybrid organic-inorganic compounds.
With help of a beam splitter, a small fraction of the synchrotron radiation (the 9th harmonic, ~21.0 keV) from the DanMAX undulator will be diverted to the SINCRYS experimental hutch. The beam splitter must not affect the main beam by either diverting a too large fraction of the radiation, by absorption, or by distorting it. Both the main- and the side-station will be operable in parallel. To facilitate this, a minimum distance of one metre between diverted and undiverted beam is required. A thin diamond crystal is employed as a diffractive beam splitter, using the 111 reflection in Bragg (or Laue) geometry. The C111 reflection diverts radiation within a narrow bandwidth to the SINCRYS side branch. Subsequent reflection from a second crystal (again C111 or Ge220) with equal/similar inter-planar spacing and diffracting planes parallel to the first is the golden standard in crystal monochromator design, which is followed here. This has the advantage to return the twice diffracted beam parallel to the direction of the incident, with an adjustable offset, such that downstream optical components and the sample do not have to follow the Bragg angle changes with selected photon energy. Over the full undulator gap the energy of the 9th harmonic ranges from 20.0 to 23.0 keV.
The focus in the development of the SINCRYS instrument is on high-throughput solutions, offering as much automation of the journey from crystalline sample to solved structure as possible. This high degree of automation ensures optimal conditions to setup the SCS, a portal for service crystallography inspired by the successful UK National Crystallography Service (www.ncs.ac.uk). Here, both academic and industrial researchers can order services that range from sample mounting and data collection to structure solution and refinement. Availability of a one-stop-shop akin to SCS will lower the threshold for accessing single crystal diffraction at a synchrotron and is expected to make the technique available to a much wider and more diverse community. It has the potential to eventually provide a home for Scandinavian research efforts.
