Testimonial: Dr. Olivier Pérez, CRISMAT Laboratory
The arrival of the XtaLAB Synergy-S diffractometer: A turning point for our crystallography group
The arrival of our Synergy S diffractometer in September 2018 marked a pivotal moment for our crystallography group, ushering us into the modern era of single-crystal X-ray diffraction. Equipped with two microfocus sources (Copper and Molybdenum) and a photon-counting detector (Eiger 1M, DECTRIS), the instrument offers unprecedented versatility. Its broad operating temperature range — from 28 K to 1200 K — further expands its capabilities. All the ingredients were in place to profoundly reshape our experimental workflows.
So, what have been the most significant changes?
- Time efficiency: From crystals to structures in minutes
Today, a high-quality crystal can be measured in just 3 to 60 minutes. While time savings are not always critical for our research, they have transformed our teaching. We can now offer live demonstrations of single-crystal X-ray diffraction to Master’s students. Within an hour, they can select a crystal, collect data, process it, and obtain a full structure. This hands-on experience not only makes crystallography more tangible, but also helps ignite genuine interest in the field.
- Versatility through dual-source configuration
The dual-source system is a major asset: Copper for organic and organometallic compounds, Molybdenum for inorganic materials. For structures with large unit cells, the longer wavelength of the copper source helps reduce reflection overlap and improves data integration.
Beyond conventional single-crystal experiments, the Synergy S has also proven effective for non-standard and low-quantity samples — notably in cases where traditional X-ray powder diffraction is not viable due to insufficient material. In such situations, the Synergy S can serve as a powerful alternative, allowing structural insights to be obtained from just a few micrograms of sample.
This capability is exemplified by our successful diffraction studies on individual flax fibers, which cannot be ground or prepared for conventional powder analysis. Thanks to the copper source and its motorized divergence slits, combined with the detector's sensitivity, the system enables reliable measurements even on these challenging, limited-quantity samples — opening new avenues for materials characterization.
- Microcrystal capabilities: Measuring the nearly invisible
We are now able to analyze inorganic single crystals smaller than 5 µm in all dimensions. Thanks to the detector’s high sensitivity and zero electronic noise, the resulting data quality is remarkable. While such measurements can take up to 20 hours, they yield data of a quality that permits refinement using anharmonic thermal motion models — something previously unthinkable for such small volumes.
These advances allow us to offer precise structural characterization of minuscule samples — cases that, just a few years ago, would have been limited to powder X-ray diffraction only.
- Tackling the complexity of aperiodic materials
My own area of expertise — the study of aperiodic materials, including modulated and incommensurate composite crystals — presents several challenges: strong main reflections alongside extremely weak satellites, long exposure times, and the risk of detector saturation.
The Synergy S manages these demands with ease. Even long exposures do not lead to saturation. Additionally, satellite reflections often appear at irrational positions and may overlap with other signals. Here, the high-performance detector, combined with the reciprocal space tools and advanced integration options in CrysAlisPro, greatly improves reliability, even for the most complex datasets.
The synergy between hardware and software is what makes this system so powerful — even for the most unconventional cases. I would like to sincerely thank Dr. Mathias Meyer and his team for their outstanding responsiveness, support, and commitment to addressing the often-demanding needs of our user community.
- Thermo-Diffraction and Phase Transition Studies
Another major research direction enabled by the Synergy S is the study of phase transitions via thermo-diffraction. These investigations require the ability to detect subtle lattice distortions, slight variations in diffracted intensities, and extremely weak signals, such as pre-transitional diffuse scattering or satellite reflections.
The system’s precise goniometer and high-efficiency detector, together with CrysAlisPro, make it possible to collect data seamlessly across a wide temperature range — during both heating and cooling cycles. This allows for precise tracking of characteristic reflections, quantification of order parameters, and identification of hysteresis effects. This line of research naturally aligns with our ongoing work on aperiodic materials.
Conclusion
The Synergy S has profoundly reshaped both our research capabilities and our approach to teaching. It has opened doors to previously inaccessible samples and techniques, while making crystallography more accessible and inspiring for students and collaborators alike.