title: In Situ Investigation of a Self-Accelerated Cocrystal Formation by Grinding Pyrazinamide with Oxalic Acid.
abstract: A new cocrystal of pyrazinamide with oxalic acid was prepared mechanochemically and characterized by PXRD, Raman spectroscopy, solid-state NMR spectroscopy, DTA-TG, and SEM. Based on powder X-ray diffraction data the structure was solved. The formation pathway of the reaction was studied in situ using combined synchrotron PXRD and Raman spectroscopy. Using oxalic acid dihydrate the initially neat grinding turned into a rapid self-accelerated liquid-assisted grinding process by the release of crystallization water. Under these conditions, the cocrystal was formed directly within two minutes.
authors.affiliation: Federal Institute for Materials Research and Testing (BAM), Richard-Willstaetter-Str. 11, 12489 Berlin, Germany. hannes.kulla@bam.de.|Department of Chemistry, Humboldt-Universit&#228;t zu Berlin, Brook-Taylor-Str. 2, 12489 Berlin, Germany. hannes.kulla@bam.de.
authors.forename: Hannes
authors.initials: H
authors.lastname: Kulla
authors.affiliation: Federal Institute for Materials Research and Testing (BAM), Richard-Willstaetter-Str. 11, 12489 Berlin, Germany. sebastian.greiser@bam.de.
authors.forename: Sebastian
authors.initials: S
authors.lastname: Greiser
authors.affiliation: Federal Institute for Materials Research and Testing (BAM), Richard-Willstaetter-Str. 11, 12489 Berlin, Germany. sigrid.benemann@bam.de.
authors.forename: Sigrid
authors.initials: S
authors.lastname: Benemann
authors.affiliation: Department of Chemistry, Humboldt-Universit&#228;t zu Berlin, Brook-Taylor-Str. 2, 12489 Berlin, Germany. klaus.rademann@hu-berlin.de.
authors.forename: Klaus
authors.initials: K
authors.lastname: Rademann
authors.affiliation: Federal Institute for Materials Research and Testing (BAM), Richard-Willstaetter-Str. 11, 12489 Berlin, Germany. franziska.emmerling@bam.de.
authors.forename: Franziska
authors.initials: F
authors.lastname: Emmerling
mesh_terms: D003460:Crystallization; D006860:Hydrogen Bonding; D009682:Magnetic Resonance Spectroscopy; D008958:Models, Molecular; D019815:Oxalic Acid / Q000737:chemistry*; D011718:Pyrazinamide / Q000737:chemistry*; D014961:X-Ray Diffraction
chemical_list: D011718:Pyrazinamide; D019815:Oxalic Acid
keywords: cocrystal; hydrate; in situ; mechanochemistry; pyrazinamide