Multimetallic Polymerization Catalysis Research in the Agapie laboratory is targeted toward developing new, practical catalysts by using inspiration from biological systems.
This suggests addition of the metal complex to mesitylene causes downfield shifting of the signal for protons attached directly to the ring as they are unshielded from the backbonding of carbonyl groups.
The reaction specifically takes place in the following manner: Scheme 1 This is compound of interest because it a metal-arene complex and can be considered to be an octahedral rather than tetrahedral complex.
The IR spectrum of [1,3,5-C6H3 CH3 3]Mo CO 3 can be analyzed for peaks indicative of symmetrical and antisymmetrical carbonyl stretching, whose areas can be used to calculate the bond angle between the carbonyl groups attached the to metal. Experimental All syntheses were carried out in nitrogen and the reagents and solvents were purchased from commercial sources and used as received unless otherwise noted.
A greased sidearm, stopcock, and 30 Arene molybdenum lab cold water condenser were attached to the round-bottom flask. A greased gas inlet Arene molybdenum lab then attached to the condenser and connected to a bubbler.
The condenser was not connected to a cold water source; it was used only to allow air to circulate. The sidearm was connected to a nitrogen source, and the system was allowed to degas for 5 minutes. The system was then put on the sand bath and the stir bar was spun at a moderate speed via a magnetic stirring instrument.
After a total of 0. The remaining solution cooled to a blackish yellow color. The following and final procedures took place in the presence of air. Once cool, the solution was washed with 15 mL of hexane via suction filtration in a 15 mL frit.
The solution was then washed with another 5 mL of hexane. About 10 mL CH2Cl2 was added to the blackish yellow powder precipitate remaining in the frit. The powder was washed with 25 to 30 mL of hexane and vacuum dried.
This powder was discarded and the collected yellowish washings were rotovapped for about 0.
The product was vacuum filtered, as it would not completely dry under the rotovap. The resulting yellowish powder was determined to be 1 0.
The 1H NMR spectrum of 2 was extrapolated from the literature. Results The reaction of Mo CO 6 with mesitylene yielded 0. This translated to 0. Mo CO 6 reacted to form the product in a 1: Proton NMR spectroscopy yielded a two peaks of interest.
Much of this quantitative shortcoming can be attributed to clumsiness, as much of the solution containing future product was lost when the reaction vessel was dropped. This not only resulted in a direct loss of solution, but also exposed the solution to air.
The solution had been kept under nitrogen as to prevent decomposition of the products. This exposure to air undoubtedly had a contribution to the poor percent yield. The solution was also not heated as desired because it was difficult to control the sand bath.
The solution was to be brought to a moderate boil, but could not be controlled to do so. It would not boil, then boiled rigorously a moment later. Attempts were made to subdue the boiling, but were unsuccessful. This overheating was probably not favorable for the reaction. More adept control of the sand bath would have resulted in a better yield of product.
Washing the product with excess amounts of hexane and CH2Cl2 also may have added to the loss of product. Excess washing would make it difficult to extract the product from the solution, as there would have been a relatively small amount of product compared to the amount of solution it was dissolved in.
Vacuum filtration then had to be used to collect the product, which was not ideal. Best case scenario, the rotovap would have completely dried the product and it would have been scraped out of the flask.
Vacuum filtration gives a better chance for loss of product. This seems to confirm the structure and addition of the metal complex, as only the C-H peak was shifted downfield.Synthesis, electrochemistry, and crystal and molecular structures of some molybdenum(0) arene derivatives with fluorinated and phenyl-substituted arene .
Inorganic Chemistry Laboratory fall 3 Experimental Procedures Part 1. Synthesis of η6-cycloheptatriene molybdenum tricarbonyl [(η6-C 7H8)Mo(CO)3] 8 Our first synthetic goal is to convert Mo(CO)6 into a moderately air-sensitive organometallic arene .
Ergonomically chemistry is the study of chemical compounds that contain carbon atoms bound to a metal atom. Ergonomically compounds can contain main group elements, or more metallic elements such as zinc or carbon. Research in the Agapie laboratory is targeted toward developing new, practical catalysts by using inspiration from biological systems.
Some of the most fascinating catalysts in Nature display complex inorganic cofactors, sometimes in combination with organic cofactors, and perform chemical transformations (water reduction and oxidation, . The arene−metal bond in tricarbonyl(η 6-arene)molybdenum complexes is labile, and the complexes readily undergo arene exchange at ambient temperature.
Equilibria are reached when [Mo(η 6 -C 6 H 6)(CO) 3 ] is reacted in the presence of THF with arenes bearing functional groups. The Le Bail method is quite a small little thing, a tiny detail in the way to apply the Rietveld decomposition formula.
But that tiny detail changes the horizon.