MS20-P02 Low-Cost Portable Devices for Inert Low-Temperature Sample Manipulation Nils Trapp (Small Molecule Crystallography Center, ETH Zürich, Zürich, Switzerland) Michael Solar (Small Molecule Crystallography Center, ETH Zürich, Zürich, Switzerland) Michael Wörle (Small Molecule Crystallography Center, ETH Zürich, Zürich, Switzerland)email: nils.trapp@org.chem.ethz.ch
Sample cooling has become widely implemented in crystal structure determination, due to the broad array of advantages it offers (Goeta & Howard, 2004). In particular, measurement at reduced temperatures can severely improve data accuracy and resolution for small molecule crystals, due to reduced and more isotropic atomic vibration (Brock & Dunitz, 1990). In addition, it can reduce radiation damage in protein crystals, enable variable temperature or phase transition studies and allow measurements of samples that are not stable or solid under ambient conditions. Low temperature can also prevent crystal damage due to the escape of co-crystallized solvent, which often retains a relatively high vapor pressure. Because the cooling medium used in open-flow sample cryostats is either nitrogen or helium gas, air-sensitive and even pyrophoric crystals can be measured using standard equipment. However, transferring sensitive samples from storage vessel to diffractometer, without compromising crystal and data quality, remains a challenge in many cases.
 
A straightforward procedure for preparing and mounting crystals under inert conditions is demonstrated, using a specialized apparatus (μCHILL). The technique is extremely flexible, requiring only a single operator, little practice and almost no preparation time. The device enables a wide temperature range (at least –60 °C to room temperature), providing temperature control and very stable conditions with no ice formation over extended time periods. The flexible, modular and low-cost design is based on 3D printed parts and readily available standard components, potentially making the device available to a wide range of users and applications not limited to single crystal studies.
References:

Trapp, N, & Solar, M. (2018). Journal of Applied Crystallography, accepted.

Goeta, A. E. & Howard, J. A. K. (2004). Chemical Society Reviews 33, 490–500.

Brock, C. P. & Dunitz, J. D. (1990). Acta Cryst. B. 46, 795–806.

Keywords: crystal mounting, instrumentation, cryocrystallography