Mechanochemical synthesis and characterisation of cocrystals and metal organic compounds

Abstract

The mechanochemical synthesis of two model compounds, a metal organic framework (H₂Im)[Bi(1,4-bdc)₂] (bdc = benzene dicarboxylate, H₂Im = imidazole cation)) and a cocrystal (carbamazepine : indometacin 1 : 1) were followed ex situ using a combination of two analytical methods. Powder X-ray diffraction (XRD) and Raman spectroscopy data were evaluated for the synthesis of the metal organic framework. The XRD measurements and REM images were analysed for the synthesis of the cocrystal. The measurements revealed that both model compounds were synthesised within minutes. The metal organic framework (H₂Im)[Bi(1,4-bdc)₂] is synthesised via an intermediate structure. The cocrystal carbamazepine : indometacin 1 : 1 is formed within a few seconds. The crystallite size decreases during the further milling treatment.