Three different Ge environments in a new Sr5CuGe9O24 phase synthesized at high pressure and high temperature

Acta Crystallogr B Struct Sci Cryst Eng Mater. 2020 Oct 1;76(Pt 5):727-732. doi: 10.1107/S2052520620008914. Epub 2020 Aug 12.

Abstract

In the framework of expanding the range of copper-based compounds in the pyroxene family, we have synthesized at high pressure and high temperature a powder containing a mixture of a new phase with stoichiometry Sr5CuGe9O24 having two identified impurity phases. Electron crystallography showed that the new phase crystallizes in the monoclinic space group P2/c, with unit-cell parameters a = 11.8 Å, b = 8.1 Å, c = 10.3 Å and β = 101.3°. We applied the recently developed low-dose electron diffraction tomography method to solve the structure by direct methods. The obtained structure model contains all 9 independent cation positions and all 13 oxygen positions. A subsequent refinement against powder X-ray diffraction data ascertained the high quality of the structure solution, in particular, the unusual structural arrangement that there are three different environments for Ge in this phase.

Keywords: electron crystallography; high pressure; high temperature; pyroxene; structure determination.