Six new crystal structures were determined using a Rigaku Mercurcy 375/MCCD(XtaLab mini) diffractometer. The structure of a molybdenum cofactor was solved resulting in an R1 (R1 = Σ ||Fo| - |Fc|| / Σ |Fo|) of 3.61% despite the presence of a disordered DMSO molecule. New Tetrakis(N-phenylacetamidato) Dirhodium(II) complexes were synthesized and characterized. Two 2,2-cis-[Rh2(NPhCOCH3)4]•(C3H4N2)x where x= 1 or 2 were successfully crystallized and solved with R1 values below 5%. Additional studies were conducted via NMR to observe formation of both products. Three potential catalysts were synthesized starting with 3,1-[Rh2(NPhCOCH3)4]. The resulting compounds were a mono adduct 3,1-[Rh2(NPhCOCH3)4]•(C3H4N2), and two dimer of dimers complexes with amine bridges 3,1-[Rh2(NPhCOCH3)4]2•(C8H6N2) and 3,1-[Rh2(NPhCOCH3)4]2•(C10H8N2). All three complexes were crystallized and solved with R1 values less than 10%. Additional NMR studies were conducted to elucidate solid and solution phase structures and to determine the possibility of additional amine bonds forming.