title: De novo determination of the crystal structure of a large drug molecule by crystal structure prediction-based powder NMR crystallography.
abstract: The crystal structure of form 4 of the drug 4-[4-(2-adamantylcarbamoyl)-5-tert-butyl-pyrazol-1-yl]benzoic acid is determined using a protocol for NMR powder crystallography at natural isotopic abundance combining solid-state (1)H NMR spectroscopy, crystal structure prediction, and density functional theory chemical shift calculations. This is the first example of NMR crystal structure determination for a molecular compound of previously unknown structure, and at 422 g/mol this is the largest compound to which this method has been applied so far.
authors.affiliation: Centre de RMN à Très Hauts Champs, CNRS/ENS-Lyon/UCB Lyon 1, Université de Lyon , 5 rue de la Doua, 69100 Villeurbanne, France.
authors.forename: Maria
authors.initials: M
authors.lastname: Baias
authors.forename: Jean-Nicolas
authors.initials: JN
authors.lastname: Dumez
authors.forename: Per H
authors.initials: PH
authors.lastname: Svensson
authors.forename: Staffan
authors.initials: S
authors.lastname: Schantz
authors.forename: Graeme M
authors.initials: GM
authors.lastname: Day
authors.forename: Lyndon
authors.initials: L
authors.lastname: Emsley
mesh_terms: D001565:Benzoates / Q000737:chemistry*; D009682:Magnetic Resonance Spectroscopy; D008958:Models, Molecular; D015394:Molecular Structure; D004364:Pharmaceutical Preparations / Q000737:chemistry*; D011720:Pyrazoles / Q000737:chemistry*
chemical_list: C000589241:4-(4-(2-adamantylcarbamoyl)-5-tert-butyl-pyrazol-1-yl)benzoic acid; D001565:Benzoates; D004364:Pharmaceutical Preparations; D011720:Pyrazoles