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

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High-Temperature X-Ray Crystal Structure Analysis of Schiff Base Cu(II) and Ni(II) Complexes and Data Statistics.

Anna Okui¹, Rin Tsuchiya¹, Daisuke Nakane¹

¹Department of Chemistry, Faculty of Science, Tokyo University of Science, 1-3 Kagurazaka, Shinjuku-ku, Tokyo 162-8601, Japan.

Molecules (Basel, Switzerland)

|March 27, 2025

Summary

High-temperature X-ray analysis reveals atomic movement details in copper (II) and nickel (II) complexes. Temperature affects electron density and intermolecular interactions, providing insights into material behavior.

Keywords:

Schiff base copper displacement parameters high temperature nickel

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Area of Science:

Materials Science
Crystallography
Inorganic Chemistry

Background:

Schiff base copper (II) (Cu) and nickel (II) (Ni) complexes are known compounds.
Understanding atomic behavior at varying temperatures is crucial for materials development.

Purpose of the Study:

To assess the accuracy of high-temperature X-ray crystal structure analyses.
To investigate atomic movement and its impact on crystal structures.
To compare structural data at room temperature (298 K) and elevated temperatures (410 K).

Main Methods:

Synthesis of Schiff base copper (II) and nickel (II) complexes.
High-temperature X-ray crystal structure analysis.
Comparison of lattice constants, temperature factors, and electron density maps.
Hirshfeld surface analysis to examine intermolecular interactions.

Main Results:

Electron density maps showed a decrease in electron density at higher temperatures.
Intermolecular interactions, particularly between chlorine and hydrogen atoms in the Cu complex, changed significantly with temperature.
Anisotropic temperature factors, especially for chlorine, exhibited significant changes.
Differences in analytical data between room and high temperatures were observed.

Conclusions:

High-temperature X-ray analysis provides valuable data on atomic movement and structural changes.
Temperature significantly influences electron density and intermolecular interactions in these metal complexes.
The findings are useful for developing models of temperature-dependent material properties.