Three-dimensional Structural Analysis of a Trace Sample: Example of Measurement of an Ultra-small Crystal (less than 3 μm) using XtaLAB SynergyCustom

Introduction

Single crystal X-ray structure analysis is a powerful structure determination method that can directly determine the three-dimensional molecular structure of an unknown compound. Using Rigaku's latest single-crystal X-ray diffractometer, XtaLAB SynergyCustom, equipped with a FR-X ultrabright X-ray generator and a Hypix-Arc 150° ultra-sensitive curved hybrid photon counting detector, ultra-small crystals with a minimum size of less than 3 μm can be easily measured in the laboratory.

Crystalline phase analysis

Acetaminophen ultramicrocrystal (1 μm x 2 μm x 3 μm = 6 μm³)	Automatic structure analysis result Measurement time: 34 min 20 sec R₁: 7.36%

Figure 1: Automated structure analysis using "What is this?" mode

Table 1: Result of full dataset collection

Conclusion

An ultrasmall crystal (3 μm × 2 μm × 1 μm) taken from a commercial capsule drug were used. The structure of acetaminophen was obtained in about 30 minutes after measurement and automatic analysis using “What is this?” mode (Figure. 1). In addition, full dataset collection using the same crystal yielded a good-quality structural analysis result that are ready for submission for publication (Table 1).

The XtaLAB SynergyCustom system enables the structure determination of trace samples that have been difficult to measure in the past, such as natural active ingredients, impurities, and pharmaceutical metabolites.