complexes (R = t Bu, Me, Ph) as bright red-orange solids in 71%, 86% and 76% yields, respectively. Reactions with AgSbF6, previously used for the in-situ generation of active catalysts for allylic substitution reactions, 14 yielded complex mixtures. We attempted to determine the identity of these reaction byproducts in the case of R = t Bu, revealing the occurrence of ligand scrambling and oxidation of the metal center (Fig. ). The solid state structures of R Mo IV Cl2 (R = Me, t Bu, Ph) and R Mo IV (OTf)2 (R = Me, t Bu) complexes were characterized by single crystal XRD (Fig. ). We did not succeed in growing a crystal of sufficient quality for single crystal XRD structural determination of the complex Ph Mo IV (OTf)2 , despite being able to isolate it in pure form. All compounds were found to crystallize as mononuclear coordination complexes, enabling to unambiguously disclose the in-