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Researchers demonstrated atomic-resolution structure determination of small organic molecules from nanocrystals present in ordinary powders, using minimal specimen preparation. The study included pharmaceutical and natural-product examples and showed that individual compounds could be analyzed from a mixed specimen. It established a practical route around the need to grow crystals large enough for conventional single-crystal X-ray diffraction.
A prototype electron diffractometer combined a transmission electron microscope with a hybrid pixel detector. Researchers determined a methylene blue derivative and identified the crystal structure of paracetamol within a commercial medicine containing crystalline and noncrystalline components. The work demonstrated chemical crystallography from crystals too small for standard X-ray workflows, while emphasizing the need for appropriate structural validation.
Researchers determined crystal structures of ramelteon and tolvaptan using three-dimensional precession electron diffraction tomography on approximately 500-nanometer crystals. Structures from subsequently grown, much larger crystals were measured by single-crystal X-ray diffraction for comparison. Agreement in molecular conformation, packing, and unit-cell parameters supported the electron-diffraction workflow for these two pharmaceutical materials.
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