Four CuI(ett) coordination polymorphs and changes in XRD upon hydrothermal condition optimization

Four [Cu-I(ett)](n) coordination polymorphs (1-alpha, 1-beta, 1-gamma and 1-delta), based on 5-(ethylthio)-1H-tetrazole (Hett), have been prepared successfully. By regulating the reaction time and reaction temperature, the rich coordination mode of the ett ligands can be regulated. Consequently, 1-alpha, 1-beta and 1-gamma show 2D wave-like layers, while 1-delta shows a 3D network. Powder X-ray diffraction (PXRD) analysis of the bulk sample of 1 prepared through a hydrothermal procedure revealed that 1-alpha and 1-delta can be isolated through temperature-dependent and time-dependent experiments, respectively. Starting from an as-prepared sample of 1-alpha in aqueous solution, the conversion from 1-alpha to 1-delta has been tracked over time by PXRD, with observations of the intermediate phases of 1-beta and/or 1-gamma in the hydrothermal re-crystallization process.