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The crystallisation of copper(II) phenylphosphonates

Research paper by Manuel Wilke, Anke Kabelitz, Tatiana E. Gorelik, Ana Guilherme Buzanich, Uwe Reinholz, Ute Kolb, Klaus Rademann, Franziska Emmerling

Indexed on: 14 Oct '16Published on: 06 Oct '16Published in: Dalton Transactions



Abstract

The crystal structures and syntheses of four different copper(II) phenylphosphonates, the monophenylphosphonates α-, β-, and γ-Cu(O3PC6H5)·H2O (α-CuPhPmH (1) β-CuPhPmH (2) and γ-CuPhPmH (3)), and the diphosphonate Cu(HO3PC6H5)2·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 α-CuPhPmH (1) and CuPhP2mH (4) were solved from powder X-ray diffraction data. The structure of β-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.

Graphical abstract 10.1039/C6DT02904C.gif