Single-crystal neutron Laue diffraction dataset for L-tyrosine at 100 K and 157 K

This submission contains the results of crystal structure refinements against experimental single-crystal neutron Laue data for L-tyrosine crystal collected at 100K and 157K. The results were used to validate multipole model refinement from experimental high-resolution single-crystal three-dimensional electron diffraction data (3DED) for L-tyrosine data set deposited here: https://zenodo.org/records/13359514. The dataset includes:Raw experimental data collected at 100K and data reduction results (L-Tyr_2026_02_16_100K.zip)Raw experimental data collected at 157K and data reduction results (L-Tyr_2026_02_25_157K.zip)Final CIF files documenting the whole process (L-Tyr_CIFs.zip)To obtain crystals of L-tyrosine, first the L-tyrosine was dissolved in 2M potassium hydroxide (KOH) until a saturated solution was obtained. After that the saturated solution was diluted 1.5× by adding water. The good quality crystals were obtained by slow evaporation of the diluted solution at room temperature.The neutron diffraction experiments were performed at the OPAL Research Reactor of the Australian Nuclear Science and Technology Organization using the single-crystal Laue diffractometer (KOALA2 )[Edwards, A. J. Neutron Diffraction-Recent Applications to Chemical Structure Determination Aust. J. Chem. 2011, 64, 869– 872 DOI: 10.1071/CH11234], in its latest iteration KOALA2, stands at the end guide position of thermal neutron guide TG3 and utilizes the full wavelength range available therein. The lower wavelength cutoff varies for the different compounds according to the resolving power of the crystal. Single crystal of L-tyrosine was accordingly affixed on an aluminum hook with a small amount of Paratone-N oil. The crystal was in all instances flash-cooled on mounting to the φ axis of the Laue diffractometer into the nitrogen stream from an Oxford Cryosystems COBRA™ cryostream preset to a prescribed temperature. Laue patterns were recorded from the stationary crystal with a large cylindrical imaging plate detector. For L-tyrosine, a total of 12 diffraction images separated by sequential φ rotations of 17° has been collected from two orientations of a single crystal specimen of 0.8x0.4x0.2mm with exposure times of 14600s / image at 100K and 15000s / image at 157K. Indexing, integration, normalization, and data reduction were performed via the program LaueG, [Piltz, R. O. Accurate data processing for neutron Laue diffractometers. J. Appl. Crystallogr. 2018, 51, 635– 645, DOI: 10.1107/S1600576718005058, Piltz, R. O. LaueG software for displaying and processing neutron Laue images J. Appl. Crystallogr. 2018, 51, 963-965, DOI: 10.1107/S1600576718005046] with the integration being based on the Argonne boxes procedure [Wilkinson, C.; Khamis, H. W.; Stansfield, R.; McIntyre, G. Integration of single-crystal reflections using area multidetectors J. Appl. Crystallogr. 1988, 21, 471– 478 DOI: 10.1107/S0021889888005400].Crystal structures were refined using SHELXL 2019/3 [Sheldrick, G. M. SHELXT - integrated space-group and crystal-structure determination. Acta Crystallogr. A 2015, 71, 3–8. DOI: 10.1107/S2053273314026370] in Olex2 1.5-alpha [Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. OLEX2 : a complete structure solution, refinement and analysis program. J. Appl. Crystallogr. 2009, 42, 339–341. DOI: 10.1107/S0021889808042726] without restraints, with H-atoms located directly from the difference Fourier map and their atomic displacement parameters (ADPs) refined anisotropically in harmonic approximation. No extinction correction was required.