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Lanthanide elements have a stable oxidation state of (+3) and are limited in their reactivity with small molecules due to the relative redox inertness of the metals. To overcome this, redox active ligands can be used to temporarily store electrons, which can then be used for small molecule activation. The purpose of this research was to first synthesize and characterize both bis and tris redox active ligand complexes with neodymium, gadolinium, and ytterbium. Next, we explored their reactivity towards sulfur and oxygen with these redox-active complexes in the hopes of finding a pathway to stable terminal chalcogens. The Bart group has previously published the Neodymium bis ligated system as well as its reactivity towards S8. Extending this work, the successful synthesis of the Neodymium tris ligated system, as well as the bis and tris system for Ytterbium and Gadolinium were completed and characterized with x-ray crystallography. Reactivity of the early chalcogens, sulfur and oxygen, was explored and yielded a repeatable creation of the 6-member sulfur- metal metallocycle in a twist boat formation with both Yb and Gd. Along with the metallocycle, an unexpected and repeatable 7-member sulfur chain was observed and characterized by x-ray crystallography. Exploration of oxygens reactivity with the bis ligated systems yielded change in spectroscopic data but proved difficult to produce single crystals suitable for x-ray crystallography. This twist boat conformation is contrasted with the transition metals preference towards chair conformations. Keywords: Inorganic; Redox; Lanthanide; Chalcogen

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Purdue University / 2025

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