X-ray crystallography is used to measure the bond distances between the metal and the ligands, which give insight into the spin state of the complex.
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Due to the changes in magnetic properties that occur from a spin transition - the complex being more diamagnetic in a LS state and more paramagnetic in a HS state - magnetic susceptibility measurements as a function of temperature are most commonly used in addition to optical spectroscopy and X-ray crystallography.
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Typically, bond lengths determined by X-ray crystallography show a small decrease at increasing temperatures due to an increase in the amplitude of atom vibrations, which is the case seen here above 110 K for the average Co-N bond lengths (1.90 Å at 200 K and 1.89 Å at 298 K for the top axial CoIII ion and 1.88 Å at 200 K and 1.84 Å at 298 K for the bottom axial CoIII ion, Figure 11).
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