crystals and dissapointment

Well, a picture of the crystals just to show you how big they were. Unfortunately the camera I was using does not take very good close-up shots. There are two whole crystals shown in the J. Young tube, with a penny for size comparison. These were blocky, and I could actually tell you the space group just by looking at the facets on the crystals if I were to take the time to look them up. Unfortunately careful 11B and 13C NMR analysis indicates almost certainly that these are not what I thought they were, and to boot, they are pretty common and easy to obtain, which explains why I got such huge crystals.

some crystals

Finally a break. The liquid pearl mentioned in the previous blog was painstakingly filtered (4 hours on a Buechner) and a quick 13C NMR said the prize was in the filtrate. Weird because the pearly part stayed on the filter, but I think there was just a wee bit of pearl in a bulk of dull white crap. Cooling the filtrate overnight in the fridge gave some nice flakey crystals, clear but with a significant iridescence, kind of like mica. While this is well and good, they aren't really X-ray quality crystals because they are just thin plates, nor are they worth getting a structure of anyway.

And in better news, a vial that's been in the box freezer for almost a month now (haven't looked at it in a few weeks) has yielded big fat blocks of clear crystals. Theres one thats nearly 3 mm square, almost neutron diffractable. Almost. More to the point, these are definitely X-ray quality, and they're of an unreported complex, so they might be worth collecting data on. I doubt it though, but we'll see what Prof. Heller thinks.

X-ray quality crystals were grown from a solution of THF over several weeks in a -40 C freezer.

Liquid pearl

For reasons I may explain later (or not, it doesn't matter) I was converting some phloroglucinol to 3,5-dihydroxybenzenesulfonate. The prep calls for diluting the aqueous solution with ethanol in order for the product to crystallize overnight. Whatever, this didn't happen. After a few other attempts I evaporated all of the solvent and then tried to dissolve it into a minimum of water, which didn't work at all for some unknown reason (it was soluble in water to start out with - maybe a pH issue). It did give a suspension which looked remarkably like liquid pearl. Pretty as it is, this stuff turns out to be nearly impossible to filter because the particles are so fine. These particles are however, soluble in neat ethanol, and hopefully some crystals can be coaxed out of solution this way.

Long time, no work

Sorry to disappoint the many many fans who I know attentively watch this blog on a daily basis. The promising reaction I spoke of nearly a month ago now? No crystals, just some gummy crap at the bottom of the vial. Where has our fearless author been this past month? Well, for the first part of it I was feverishly working on a research proposal project as a requirement for staying in the graduate program. The proposal outlines the synthetic plan necessary to synthesize Moebius molecules. I rendered a computer simulation of the molecule for the conclusion, and I've included it here. Obviously its not going to really look red and blue, thats just the coloring used to define the rails and rungs of the Moebius strip. I haven't gotten much feedback on the proposal yet from my committee, but I figure that no news is good news in this particular case. Professor Heller did at least acknowledge it and said he liked the proposal. Good enough for me.

So that covers the first two weeks of my absence, the last two weeks have been spent feverishly preparing for group meeting which I gave yesterday. Mostly this was spent trying to scrape together some results in the wee bit of time I had left in between finishing the proposal and giving the group meeting presentation. All in all I thought it went rather well, and now its time to settle back into some solid, non-feverishly done research.