Synthesis and Spectroscopic Characterization of Diosmium Carbonyl Clusters with Ferrocenedicarboxylato Ligands
The microwave-assisted reaction of Os3(CO)12 and 1,1’-ferrocenedicarboxylic acid has resulted in the formation of a new diosmium carbonyl sawhorse complex with a chelating 1,1’-ferrocenedicarboxylato ligand, Os2(μ4-1,1’-ferrocenedicarboxylato)(CO)6. The optimization of this synthesis was atypical, requiring a decrease in the concentration of reactants used to achieve the optimal yield, 63.3%. Despite the compound readily crystallizing, crystallographic analysis of the compound has not yet been successful due to an abnormal diffraction pattern similar to, but not identical to, crystal twinning. Crystals have been successfully grown of a derivative of this compound, Os2(μ4-1,1’- ferrocenedicarboxylato)(CO)4[P(p-tolyl)3]2, which was synthesized through replacement of axial CO ligands on Os2(μ4-1,1’-ferrocenedicarboxylato)(CO)6. The X-ray crystal structure of this latter compound has been determined.