Fine refinement of solid state structure of racemic form of phospho-tyrosine employing NMR Crystallography approach
| Autor: | Tomasz Pawlak, Wieslaw Lasocha, Piotr Paluch, Marek J. Potrzebowski, Marcin Oszajca |
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| Rok vydání: | 2015 |
| Předmět: |
Diffraction
Models Molecular Nuclear and High Energy Physics Magnetic Resonance Spectroscopy very fast MAS molecular motions Molecular Conformation Nuclear magnetic resonance crystallography Crystal structure Crystallography X-Ray inverse detection GIPAW calculations Molecule Invariant (mathematics) Phosphotyrosine Instrumentation powder X-ray diffraction solid state NMR Radiation Hydrogen bond Chemistry 2D HETCOR correlations Stereoisomerism General Chemistry hydrogen bonding Crystallography Solid-state nuclear magnetic resonance Powder diffraction |
| Zdroj: | Solid State Nuclear Magnetic Resonance |
| ISSN: | 0926-2040 |
| DOI: | 10.1016/j.ssnmr.2014.08.002 |
| Popis: | We present step by step facets important in NMR Crystallography strategy employing O-phospho-dl-tyrosine as model sample. The significance of three major techniques being components of this approach: solid state NMR (SS NMR), X-ray diffraction of powdered sample (PXRD) and theoretical calculations (Gauge Invariant Projector Augmented Wave; GIPAW) is discussed. Each experimental technique provides different set of structural constraints. From the PXRD measurement the size of the unit cell, space group and roughly refined molecular structure are established. SS NMR provides information about content of crystallographic asymmetric unit, local geometry, molecular motion in the crystal lattice and hydrogen bonding pattern. GIPAW calculations are employed for validation of quality of elucidation and fine refinement of structure. Crystal and molecular structure of O-phospho-dl-tyrosine solved by NMR Crystallography is deposited at Cambridge Crystallographic Data Center under number CCDC 1005924. |
| Databáze: | OpenAIRE |
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