Fine refinement of solid state structure of racemic form of phospho-tyrosine employing NMR Crystallography approach

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 (...

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Bibliographic Details
Published in:Solid state nuclear magnetic resonance 2015-02, Vol.65, p.2-11
Main Authors: Paluch, Piotr, Pawlak, Tomasz, Oszajca, Marcin, Lasocha, Wieslaw, Potrzebowski, Marek J.
Format: Article
Language:English
Subjects:
2D HETCOR correlations
Crystallography, X-Ray - methods
GIPAW calculations
Hydrogen bonding
Inverse detection
Magnetic Resonance Spectroscopy - methods
Models, Molecular
Molecular Conformation
Molecular motions
Phosphotyrosine - chemistry
Powder X-ray diffraction
Solid state NMR
Stereoisomerism
Very fast MAS
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Summary: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. [Display omitted]
ISSN:0926-2040
1527-3326
DOI:10.1016/j.ssnmr.2014.08.002