x-ray-powder-diffraction-conservation-science-towards-routine-crystal

X-ray Powder Diffraction in Conservation Science: Towards Routine Crystal Structure Determination of Corrosion Products on Heritage Art Objects

The crystal structure determination and refinement process of corrosion products on historic art objects using laboratory high-resolution X-ray powder ...

State Academy of Art and Design Stuttgart

In the course of the investigation of glass-induced metal corrosion processes, a microcrystalline sodium copper formate hydroxide oxide hydrate, Cu4Na4O(HCOO)8(H2O)4(OH)2, was detected on a series of antique works of art, and its crystal structure was determined ab initio from high-resolution laboratory X-ray powder diffraction data using the method of charge flipping, simulated annealing, and difference-Fourier analysis (P42/n, a = 8.425 109(97) Å, c = 17.479 62(29) Å, V = 1240.747(35) Å(3), Z = 8). In the crystal structure, the metal cations are interconnected in a two-dimensional metal-organic framework via the oxygen atoms of the formate, hydroxide, and oxide anions. Doublets of face-sharing square pyramidal Cu(2+) polyhedra are linked via a single, central oxide oxygen atom to give a paddle-wheel arrangement, while the Na(+) cations are organized in Na2O11 moieties with highly disordered, edge-sharing octahedral coordination. In addition, hydrogen bonding plays an important role in stabilizing the crystal structure.

Gerhard Eggert

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