title: X-ray and 13C solid-state NMR studies of N-benzoyl-phenylalanine.
abstract: A crystalline sample of N-benzoyl-DL-phenylalanine 1 and a polycrystalline sample of N-benzoyl-L-phenylalanine 2 were studied using 13C high-resolution solid-state NMR spectroscopy. The X-ray structure of the DL form was established. Sample 1 crystallizes in a monoclinic form with a P21/c space group, a=11.338(1) A, b=9.185(1) A, c=14.096(2) A, beta=107.53(3) degrees, V=1400(3) A3, Z=4 and R=0.053. The principal elements of the 13C chemical shift tensors deltaii for 1 and 2, selectively 13C (99%) labeled at the carboxyl groups were calculated. On the basis of 13C (delta)ii analysis the hydrogen bonding pattern for sample 2 was deduced. Enriched samples were used to establish the intermolecular distance between chemically equivalent nuclei for 1 and spatial proximity in heterogeneous domain for 2, employing the ODESSA pulse sequence. The consistence of the complementary approach covering X-ray data, analysis of the 13C (delta)ii parameters and ODESSA results is revealed.
authors.affiliation: Polish Academy of Sciences, Centre of Molecular and Macromolecular Studies, Sienkiewicza, Lódź, Poland. marekpot@bilbo.cbmm.lodz.pl
authors.forename: M J
authors.initials: MJ
authors.lastname: Potrzebowski
authors.forename: P
authors.initials: P
authors.lastname: Tekely
authors.forename: J
authors.initials: J
authors.lastname: Błaszczyk
authors.forename: M W
authors.initials: MW
authors.lastname: Wieczorek
mesh_terms: D002247:Carbon Isotopes; D003460:Crystallization; D018360:Crystallography, X-Ray; D019281:Dimerization; D006860:Hydrogen Bonding; D009682:Magnetic Resonance Spectroscopy; D008958:Models, Molecular; D010649:Phenylalanine / Q000031:analogs & derivatives* / Q000737:chemistry
chemical_list: D002247:Carbon Isotopes; D010649:Phenylalanine; C053764:benzoylphenylalanine