title: Fine refinement of solid state structure of racemic form of phospho-tyrosine employing NMR Crystallography approach.
abstract: 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.
authors.affiliation: Polish Academy of Sciences, Centre of Molecular and Macromolecular Studies, Sienkiewicza 112, PL-90-363 Lodz, Poland.
authors.forename: Piotr
authors.initials: P
authors.lastname: Paluch
authors.affiliation: Polish Academy of Sciences, Centre of Molecular and Macromolecular Studies, Sienkiewicza 112, PL-90-363 Lodz, Poland.
authors.forename: Tomasz
authors.initials: T
authors.lastname: Pawlak
authors.affiliation: Jerzy Haber Institute of Catalysis and Surface Chemistry, PAS, Niezapominajek 8, 30-239 Krakow, Poland.
authors.forename: Marcin
authors.initials: M
authors.lastname: Oszajca
authors.affiliation: Jerzy Haber Institute of Catalysis and Surface Chemistry, PAS, Niezapominajek 8, 30-239 Krakow, Poland; Faculty of Chemistry, Jagiellonian University, Ingardena 3, 30-060 Krakow, Poland.
authors.forename: Wieslaw
authors.initials: W
authors.lastname: Lasocha
authors.affiliation: Polish Academy of Sciences, Centre of Molecular and Macromolecular Studies, Sienkiewicza 112, PL-90-363 Lodz, Poland. Electronic address: marekpot@cbmm.lodz.pl.
authors.forename: Marek J
authors.initials: MJ
authors.lastname: Potrzebowski
mesh_terms: D018360:Crystallography, X-Ray / Q000379:methods*; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008958:Models, Molecular; D008968:Molecular Conformation; D019000:Phosphotyrosine / Q000737:chemistry*; D013237:Stereoisomerism
chemical_list: D019000:Phosphotyrosine
keywords: 2D HETCOR correlations; GIPAW calculations; Hydrogen bonding; Inverse detection; Molecular motions; Powder X-ray diffraction; Solid state NMR; Very fast MAS