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Analysis of Very Small Organic Crystals with the XtaLAB Synergy-S

AppNote SMX016 Analysis of Very Small Organic Crystals with the XtaLAB Synergy-S

Background

As research projects multiply and diversify, and chemists attempt the synthesis of ever more exotic molecules, the isolation and crystallization of these molecules for subsequent characterization often represents the bottleneck for advancement of the project. So when crystallographers are presented with a batch of tiny crystals, they must be able to rely on a powerful X-ray diffractometer to collect the data required to elucidate the structure of these new compounds and characterize them without any ambiguity. To address such difficult applications, the Rigaku Oxford Diffraction XtaLAB Synergy-S diffractometer features a powerful 50 watt microfocus sealed tube with a small FWHM beam size of 110 µm, ensuring that most of the X-ray photons are concentrated on the important area, the crystal. In addition, the Rigaku Oxford Diffraction XtaLAB Synergy-S is configured with a HyPix-6000HE hybrid photon counting (HPC) detector. HPC detectors have been used at most synchrotron beamlines around the World because of their high sensitivity and very low electronic noise. These features are also critical to collect precise and accurate data on weakly diffracting crystals on home diffractometers. Here, we demonstrate the performance of the XtaLAB Synergy-S on a tiny organic crystal of benzophenone.

A very small crystal of benzophenone, with dimensions 0.015 x 0.018 x 0.027 mm³, was captured on a MiTeGen Kapton loop mounted on a magnetic base, using paratone oil. The crystal was mounted on the goniometer, centered in the beam using a video camera and data were collected at 100 K with the Rigaku Oxford Diffraction program CrysAlisPro.