DOI: 10.18150/vtbpgp
title: High-resolution single-crystal X-ray diffraction dataset and complementary data for L-tyrosine crystal charge density analysis

description: This submission contains the charge density analysis data for L-tyrosine crystal from:1. Theoretical electron static structure factors obtained from the periodic DFT calculations (DFT)2. Experimental high-resolution single-crystal X-ray diffraction data (XRD) 1. Theoretical electron static structure factors obtained from the periodic DFT calculations (DFT)This submission contains the results of multipole model refinement against theoretical electron static structure factors obtained from the periodic DFT calculation for L-tyrosine crystal. 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:a.     Geometry optimization results from Crystal (DFT_GeomOptimization.zip)Periodic crystal geometry optimization was carried out in Crystalb.     Refinement files from JANA2020 (DFT_refinement.zip)Multipole model refinement against theoretical electron static structure factor obtained from the periodic DFT calculation was conducted in a stepwise fashion, beginning with transferred multipole parameters from the MATTS database and followed by iterative refinement of electron population, κ/κ′, and multipole parameters. Atoms coordinates and ADPs were not refined. 2. Experimental high-resolution single-crystal X-ray diffraction data (XRD)This submission contains the results of multipole model refinement against experimental high-resolution single-crystal X-ray data (XRD) for L-tyrosine crystal. 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:a.     Raw experimental data, data reduction and IAM refinements from CrysAlis and Olex2 (XRD_RAWExpData_DataReduction_RefinementsIAM.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 by adding the water to achieve 1.5x dilution. The good quality crystals were obtained by slow evaporation of the diluted solution at room temperature.A high-quality single crystal of the investigated compound was selected for diffraction experiments conducted at T = 100(2) K. High-resolution X-ray diffraction data were collected using an Agilent Technologies SuperNova Dual Source diffractometer, equipped with a micro-focused Mo X-ray tube and a HyPix 6000HE hybrid pixel array detector. The crystal-to-detector distance was maintained at 55 mm. Data collection up to a resolution of 0.43 Å (with an omega scan width of 0.5 °) required 77 hours, 33 minutes, and 38 seconds. The data reduction was performed using CrysAlisPro. The reflections were merged using SORTAV implemented in the WINGX program. The structure solution and structure refinement were performed using SHELXT and Olex2 programs implemented in the OLEX2 suite. All the non-hydrogen atoms were refined anisotropically, and hydrogens were fixed using the riding model.b.     CIF file documenting the whole process. (XRD_CIFfile.zip)c.     Refinement files from JANA2020 (XRD_Refinement.zip)Multipole model refinement against experimental high-resolution single-crystal X-ray data (XRD) was conducted in a stepwise fashion, beginning with transferred multipole parameters from the MATTS database and followed by iterative refinement of electron population, κ/κ′, and multipole parameters. Only non-hydrogen atom positions and anisotropic displacement parameters were refined freely.