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.