Soxhlet success!

The extractor did wonderfully. The green substance from a couple posts ago was much less pure than I had hoped, consisting mostly of a blue substance (identity yet unknown, but not starting material.) There are three pretty distinct colors here, the yellow substance in the top sample tube is the desired product. The bottom tube is the mystery blue compound. I feel like I should spend a little time figuring out what this is so that I can avoid making it in the future. The middle tube is the original sample from the crude mix, composed of both compounds. I forget whether or not I had claimed the green compound in my color checklist, but if I did, it was unwarranted. Instead, I have made a yellow compound (which I can claim) and a blue compound (which I am not claiming yet as it is not properly identified.)

colors and technological needs

My chemistry has turned away from iridium towards cobalt. This means cheaper starting materials and harder characterizations, but it also means a whole new spectrum of colors. I've been getting some really nice blues and greens, some of which are even new products. I made a pretty wierd two coordinate cobalt bis-amide complex which was initially a dark black mess. A little sublimation however, cleaned that right up to a bright green color.

Usually I would have a photo here so that you could enjoy this coloration with me, but I haven't been able to fanagle the camera from home. I think I could benifit greatly from a cheap used camera bought off ebay which I could keep in the lab. Unfortunately I haven't been able to locate a camera as cheaply as I'd like which will still take decent quality pictures.

I guess for now you'll just have to trust me that the colors are as nice as I say they are.

Structure! and pretty pretty pictures.

Bingo! The crystals worked. I got a full structure with excellent probability ellipsoids. There is a little disorder in one of the tert-butyl groups, but that's almost to be expected, and certainly won't keep this from being a publishable structure. Fantastic!

In other good news I was reading up on how to take pictures of crystals with a regular camera on the internet. The only thing that I found was that people would focus one ocular of the microscope, shine a really really bright light on the crystals and then take the picture just by holding the lens of the camera up to the lens of the microscope. I was exteremly skeptical that this would produce anything worthwhile, but for lack of better ideas (and a little spare time on my hands in between reactions) thought I would give it a try. Eureka! It works! I used my labmates xenon bulb mega flashlight for the light source (it hurts your eyes to look at what the flashlight is shining on at close range, but works well under the microscope) and the crappy lab microscope with a regular digital camera. The crystals shown are the same batch I just got the crystal structure of.

I'm also including this on my colors checklist. Yellow. Check. These crystals are of a cobalt complex, which is were the color comes from.

color

As promised in an earlier post. Steps are being taken to document the pretty colors. What we have here is a basic iridium starting material. Iridium will be the metal atom of choice for most of the non-blue or green colors, which will be filled in with cobalt probably.


Coincidentally, my mother-in-law has towels that are this exact same color. Is this orange or yellow? Perhaps it shouldn't count for either. If I were going to be particularly rigorous about this I would take a UV-Vis spectrum, but lets not get hasty.

In other research news, I have a new compound which has been characterized by NMR. The next step is to try to get some crystals. Two initial attempts, one by reacting in THF and slowly evaporating the solution, the other by reacting in a concentrated heptane solution and cooling in the box freezer. Hopefully good news soon to follow.