title: Probing crystal packing of uniformly (13)C-enriched powder samples using homonuclear dipolar coupling measurements.
abstract: The relationship between the crystal packing of powder samples and long-range (13)C-(13)C homonuclear dipolar couplings is presented and illustrated for the case of uniformly (13)C-enriched L-alanine and L-histidine·HCl·H2O. Dipolar coupling measurement is based on the partial reintroduction of dipolar interactions by spinning the sample slightly off-magic-angle, while the coupling of interest for a given spin pair is isolated with a frequency-selective pulse. A cost function is used to correlate the so-derived dipolar couplings to trial crystal structures of the samples under study. This procedure allowed for the investigation of the l-alanine space group and L-histidine·HCl·H2O space group and unit-cell parameters.
authors.affiliation: Aix-Marseille Université, CNRS, ICR UMR 7273, 13397 Marseille, France.
authors.forename: Giulia
authors.initials: G
authors.lastname: Mollica
authors.affiliation: Aix-Marseille Université, CNRS, ICR UMR 7273, 13397 Marseille, France.
authors.forename: Myriam
authors.initials: M
authors.lastname: Dekhil
authors.affiliation: Aix-Marseille Université, Centrale Marseille, CNRS, Fédération des sciences chimiques de Marseille FR 1739, 13397 Marseille, France.
authors.forename: Fabio
authors.initials: F
authors.lastname: Ziarelli
authors.affiliation: Aix-Marseille Université, CNRS, ICR UMR 7273, 13397 Marseille, France. Electronic address: pierre.thureau@univ-amu.fr.
authors.forename: Pierre
authors.initials: P
authors.lastname: Thureau
authors.affiliation: Aix-Marseille Université, CNRS, ICR UMR 7273, 13397 Marseille, France.
authors.forename: Stéphane
authors.initials: S
authors.lastname: Viel
mesh_terms: D000409:Alanine / Q000737:chemistry; D002247:Carbon Isotopes / Q000737:chemistry; D018360:Crystallography, X-Ray; D006639:Histidine / Q000737:chemistry; D006851:Hydrochloric Acid / Q000737:chemistry; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D011208:Powders; D014867:Water / Q000737:chemistry
chemical_list: D002247:Carbon Isotopes; D011208:Powders; D014867:Water; D006639:Histidine; D000409:Alanine; D006851:Hydrochloric Acid
keywords: Crystal structure determination; Internuclear distances; NMR crystallography; Solid-state NMR; Space group; Spin network