| The unique physical and chemical properties of macrocyclic molecules have made them a synthetic target for decades. Research concerning macrocyclic complexes has increased the knowledge pool of the scientific community, and has opened the door for the discovery of vital applications ranging from powerful reaction catalysts to biological oxidation agents. However, synthesis of such complexes has proven to be challenging, time consuming, and costly, due to the vast number of possible conformations these systems can adopt.;Our research is in preparation for the synthesis of a 20-membered macromonocyclic ring structure utilizing iron centers and rhodium centers linked with bis(diphenylphosphino)ethane (dppe) ligands. The macrocyclic complex, [Fe(CO)3(mu-dppe) 2]2[Rh(CO)Cl]2, has to be synthesized in a stepwise fashion, optimizing each intermediate reaction along the way. The synthesis of [Fe(CO)3(mu-dppe)2]2[Rh(CO)Cl] 2 has to be achieved in three steps. The first step was synthesis of the iron complex trans-Fe(CO)3(Ph2PCH=CH2) 2 from iron pentacarbonyl and diphenyl vinyl phosphine. This reaction was optimized with 85.9% yield, and characterized via FTIR, {1H} 31P NMR, {1H} 13C NMR, 1H NMR, X-ray crystallography, and melting point. In the second step, Fe(CO) 3(mu-dppe)2 was synthesized from the product of the first reaction and diphenylphosphine with a yield of 72%, and characterized via FTIR, {1H}31P NMR, 1H NMR, melting point, and X-ray crystallography. Finally, [Fe(CO)3(mu-dppe) 2]2[Rh(CO)Cl]2 can be synthesized using the product of the preceding synthesis. This novel compound has excellent application regarding hydrogenation and/or oxidation catalysis, due to the nature of iron phosphine complexes in the presence of rhodium or palladium. Computational data on the nature of the carbonyl bonding interactions are explored, and an original teaching adaptation of the synthesis of Fe(CO)3(PPh 3)2 is presented as well. |
