Summary Post

I have learned so much over the course of my summer research project! My project was based around learning a skill, rather than answering a research question, so I am not in a position to elaborate on any groundbreaking conclusions, unfortunately. I became as much of a crystallographer as I could have hoped. At first, it seemed like an impossible task to mount crystals, but after 8 weeks, I could mount and run 10 unit cells in a day. By the end of my research, I had helped my lab (as well as three others) find unit cells, solve structures, and produce crystallographic information files for important chemical compounds. Some we were familiar with, and others were entirely new to research literature. I worked on 21 structures, with 2/3 of them being from our own lab. I also spent a week of my research proofing .cif files with a website called checkcif.iucr.org. There were about a dozen structures that needed to be proofed for any errors before being published, and I spent the majority of that week going through alert messages and doing my best to either fix them, or be able to explain why they cannot be fixed. It was a great deal of focus on a piece of the x-ray crystallographer’s tool kit that I would not have become adept at otherwise. The last portion of my research was a transition from being the student into being the teacher. I spent some of my time explaining (or attempting to explain) to a peer in my lab the techniques that are needed to use the x-ray diffractometer. I also tried to explain what to look for in SHELXLE to help solve disordered structures. This role reversal was part of a friendly trade because that peer took time away from his work to teach me about the pure chemistry that goes on in a lab. Crystallography requires chemistry knowledge, but wet chemistry is a whole different ball game!

[Read more…]

Summary – Synthesizing and Testing Complexes as Electrocatalysts

Entering this project, I set a goal of synthesizing a few specific complexes and testing them through electrochemistry to see if they could reduce protons to hydrogen gas.  Hydrogen gas is a source of clean energy, as hydrogen fuel cells produce only electricity, heat, and water.  Having the luxury of being on campus for a full ten weeks instead of just three, I was able to successfully synthesize five complexes.  Each of these required many calculations and multi-step reactions to produce the ligand.  I had to utilize the NMR instrument to generate spectra so that I could analyze the chemical makeup of my products and verify that I had produced the desired molecules.  Then, I took the ligand molecules and complexed them with a metal to form the final product.

[Read more…]

Update #3: Crystallizing the Complexes

Recently, I have spent a significant amount of time attempting to crystallize my complexes.  This is an important step because crystals are a purer form of the complex and will allow us to analyze the structure and verify that we have synthesized the desired complex.  However, I have only been able to get crystals of one out of my three complexes so far.  The technique I am currently using involves liquid diffusion.  The complex is dissolved in a solvent, then slowly layered on top of a denser solvent in which the complex is not very soluble.  The idea is that as the top layer slowly diffuses into the bottom layer, the complex will become less soluble and come out of solution in crystals.

[Read more…]

Update #2: New Complexes and Electrochemical Analysis

To recap, I am attempting to synthesize and test transition metal complexes which can act as electrocatalysts that reduce protons.  This reduction of protons generates hydrogen gas, which is a clean source of energy.

[Read more…]