CHE 450G: Practical Inorganic Chemistry

U of KY Dept of Chemistry

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CHE 450G Independent Experiments

[Premise]   [Suggested Topics]   [Topics Already Taken]

Premise

Independent Experiments can be selected from virtually any area of Inorganic Chemistry. By now you have had some experience reading or searching the Inorganic literature and have performed a variety of different techniques. This is your opportunity to explore areas of Inorganic Chemistry that you find interesting as well as to learn new techniques or principles. This is what research is all about! In addition, each team will give a joint oral presentation on their project .

These experiments will require very careful planning and a greater ability to handle unforeseen problems in the laboratory. Consequently, this final experiment is worth a considerably larger part of your grade than your previous experiments. Your grade will be based in part on effort, insight, degree of difficulty etc. Every experiment you have done so far this semester has been to prepare you for this moment -- going into the laboratory to plan an original experiment and execute it on your own.

There are a variety of sources from which to pick your independent experiment. The experiment should occupy the allotted laboratory time accordingly and should involve at least one synthetic step. You may choose to make a series of compounds and compare them or perhaps synthesize one compound and then prepare derivatives. Feel free to employ new techniques such as variable temperature NMR experiments, vapor phase transport synthesis, high pressure reactions etc. etc.

The hardest part in this assignment will appear to be finding a suitable topic. A few examples are given below as well as some starting points. In reality, there are thousands of papers that you could pick from the literature and repeat! Only one lab team may perform a particular experiment.

Your grade will be based on the following components:

• Research proposal, planning, preparedness etc.
• Execution of the experiment, lab technique, originality, degree of difficulty etc.
• Joint oral presentation.
• Final lab report, particularly the interpretation of the data and coherency of the project.

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Suggested Topics for Independent Experiments

Each lab team must pick a unique experiment and submit a one page white paper proposal by Wednesday, October 7th. A formal proposal is due soon thereafter.

Each topic must be approved by the instructor before you begin work. We will discuss the feasibility of the experiment as well as possible experiments/measurements to perform. Make sure you have a timetable for how you plan to use your laboratory time as well as a list of materials and supplies that you will require.

Below are some topics/techniques that you may want to explore or incorporate into your experiment (subject to equipment, cost and safety limitations). I haven't been very specific in too many of these cases. I will probably update this list as the semester progresses.

You must pick a topic from literature. I will not approve Experiment #x from a laboratory course book unless you can show me how you plan to expand and and improve it.

It is strongly recommended that at least part of your experiment involve a synthesis from Inorganic Syntheses, library call # 545.9 In7. Experiments in this series are reviewed and repeated by other researchers to confirm that they are actually reproducible. Most students discover that unchecked literature preps rarely work as advertised, and this delays or makes impossible completion of their projects.

Although Inorganic Syntheses is strongly recommended, any topic or preparation from a reasonably good journal can be fair game provided we discuss the work in detail. Here are a few ideas to get you going:

• Preparation of M-M quadruply-bonded complexes such as Cr₂(OAc)₄L₂ or similar Mo and W compounds.

• Intercalation compounds such as FeOCl or TaS₂ and their intercalation with organic guests such as amines.

• P₂I₄.

• Synthesis of a catalyst such as Wilkinson's catalyst followed by its use in hydrogenation of olefins etc.

• Synthesis of a chiral organometallic complex and its use in asymmetric synthesis.

• Preparation of polysilanes or silicones.

• Studies of dihydrogen complexes (versus dihydride complexes).

• Synthesis and characterization of dinitrogen complexes.

• Water soluble ligands for homogenous organometallic catalysis (see Angew. Chemie, Intl. Ed. Engl.1993, 11, 1524).

• Synthesis and characterization of zeolites.

• Synthesis and characterization of Group IV Ziegler-Natta olefin polymerization catalysts. Involves synthesis of catalyst, isolation and analysis of the polymer (look up papers by Tobin Marks for ideas).

• "Non-coordinating" anions (great topic). See Angew. Chemie, Intl. Ed. Engl., 1993, 32, 1025.

• Ferrocenophanes, "polymers of ferrocene" (look up papers by Ian Manners).

• Ring-opening metathesis polymerization of olefins (look up papers by Richard Schrock or Robert Grubbs).

• Multidecker sandwich compounds (like ferrocene but double decker).

[Premise]   [Suggested Topics]   [Topics Already Taken]

Topics Selected by Lab Teams

Team #	Team Members	Topic or Title
1	Dudley and Landis	Cobalt-catalyzed cyclotrimerization of triply unsaturated organics
2	Lott and Barney	Synthesis and characterization of a ruthenium olefin metathesis catalyst
3	Palmejar and Perkins	Solid state syntheses and characterization of BaMO3 (M = Ni, Bi, Ti)
4	Wurth and Rozenzhak	Determination of binding constants of Cs(crown ether) complexes using Cs NMR
5	Chen	Synthesis and characterization of zeolites
7	Darnall and Thoma	Synthesis and characterization of CpRu(PPh3)2 carbenes and vinylidenes

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