The structural characterization of powder materials often remains challenging due to the lack of single crystals suitable for X-ray diffraction. Here, the authors present a workflow that integrates microcrystal electron diffraction with high-resolution mass spectrometry, database mining, solution and solid-state NMR, and DFT-D/GIPAW calculations to resolve atomic structures of complex powders, demonstrating the approach on a pyridoxine-N-acetyl-L-cysteine salt, a mechanochemically synthesized adduct for which large single crystals could not be obtained, and on N-formyl-methionyl-leucylphenylalanine, a bacterial chemoattractant peptide.
- Chiara Sabena
- Federica Bravetti
- Michele R. Chierotti
