The crystallisation of copper(II) phenylphosphonates

摘要

The crystal structures and syntheses of four different copper(II) phenylphosphonates, the monophenyl-phosphonates alpha-, beta-, and gamma-Cu(O3PC6H5)center dot H2O (alpha-CuPhPmH (1) beta-CuPhPmH (2) and gamma-CuPhPmH (3)), and the diphosphonate Cu(HO3PC6H5)(2)center dot H2O (CuPhP2mH (4)), are presented. The compounds were synthesized from solution at room temperature, at elevated temperature, under hydrothermal conditions, and mechanochemical conditions. The structures of alpha-CuPhPmH (1) and CuPhP2mH (4) were solved from powder X-ray diffraction data. The structure of beta-CuPhPmH (2) was solved by single crystal X-ray analysis. The structures were validated by extended X-ray absorption fine structure (EXAFS) and DTA analyses. Disorder of the crystal structure was elucidated by electron diffraction. The relationship between the compounds and their reaction pathways were investigated by in situ synchrotron measurements.