2016Final ReportReaction of 44Thiobisbenzenethiol with Fe3CO12Principal Investigator CHARLES A MEBIDepartment of Physical SciencesStatement of ProblemThis project wasaimed at studying thereaction of ID: 877384
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1 Faculty Research Grant 201 6 Final Re
Faculty Research Grant 201 6 Final Report Reaction of 4,4 ꞌ - Thiobisbenzenethiol with Fe 3 (CO) 12 Principal Investigator CHARLES A. MEBI Department of Physical Sciences Statement of Problem This project was aimed at studying the reaction of 4,4 ` - t hiobisbenzenethiol with t riirondodecacarbonyl. The expected product(s), iron - ca r bonyl cluster (s), are of interest as catalyst s for the production of hydrogen, an environmentally benign alternative to fossil fuels. The development of efficient catalysts for hydrogen generation is an important step towards achieving the hydrogen economy. Brief Review of Research Procedure Utilized Triirondodecarbonyl (2.28 g, 4.53 mmol) and 4,4’ - thiobisbenzenethiol (0.85g, 3.39 mmol ) were mixed in a 100 mL flask and purged with nitrogen for 30 minutes. Toluene (70 mL) was then added to the flask and stirred under reflux conditions for 30 minutes. The solution changed color from dark green to red. The solvent of the solution was remo ved by rotary evaporation affording an orange solid. Silica gel chromatographic separation of the residue using hexanes -
2 dichloromethane (50:50) solvent mixtu
dichloromethane (50:50) solvent mixture as eluent gave a c yclic tetranuclear iron - carbonyl complex in 41.3 % yield . This new compound h as been characterized using IR and UV - vis spectroscopy (Figure 1) . Electrochemical properties of the compound has been investigated by cyclic voltammetry ( Figure 2) . Single crystals of the compound were obtained and analyzed by X - ray crystallography. Summary of F indings The reaction of 4,4` - t hiobisbenzenethiol with t riirondodecacarbonyl a fforded a cyclic tetranuclear iron - carbonyl cluster . Conclusions and R ecommendations The project was successful and a manuscript describing results from this study has been prepared for publication. Figure 2. Cyclic voltammograms of product in the presence of increasing amounts of acetic acid. Figure 1 . UV - visible spectra of product recorded in DCM ( 1.0 mM )