Abstract:

The porous Hoffman-type 3D lattice, (Fe(pz)2Ni(CN)4 exhibits thermally induced spin-crossover (SCO) behavior that is dependent on the solvent guest species occupying the pores. In situ Fe K-edge X-ray absorption spectroscopy (XAS) and both non-resonant and resonant KβX-ray emission spectroscopy methods (XES) are used to probe this framework under two solvent environments that yield different extremes of spin crossover temperature. Resonant XES measurements produced high resolution XAS spectra with distinct pre-edge and edge features, whose assignment was established using both simple ligand field theory and TD-DFT calculations. Furthermore, multiple X-ray emission spectrometers were developed at APS 20-ID under SCGSR fellowship and Lab Directed Research and Development (LDRD). One based on existing miniXES design, with improvements in resolution, sample area size and versatility. The second is an X-ray emission spectrometer is capable of simultaneous measurements of up to 7 kβ emission lines consisting of variety of transition metal elements. The designs are based on purely dispersive flat crystals at fixed distance and positions from the emission source, with emission selection dependent solely on the crystal material, and is capable of single scan X-ray emission measurements, making it usable for resonant and non-resonant emission measurements.

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