April 15, 2009

more crystals!!!


Like I said, with the ligand on the metal the rest of the chemistry will follow fast. I've got 4 different crystal attempts going on several derivatives. Derivative number 1 was accomplished in no time at all. I chilled a hexane solution in the argon box over the weekend and got tiny blocks of crystals. The crystallographer swooned about these crystals. They looked a little small to me, but he seemed to think they were of the perfect size. In the picture these crystals look black, however if you break them up the fractured crystals look deep purple. The solution of these crystals is also a deep intense purple; I'll try to get a decent picture of the color later. The diffraction pattern is weak, but lets hope a structure can be coaxed out of the data.

April 10, 2009

xtls

The crystals were exceptional. Observe the sweet diffraction...


I got the structure back at 6% R factor, which the crystallographer claims is of "better than average quality". I tend to think that the average is 5%, so this would be slightly worse than average quality, but I suppose the crystallographer should know better than I do.

This is the product I have been seeking for so long via the magnesium ligand activation. As mentioned in a previous post I had given up on the magnesium and switched to lithium. This worked like a charm and now that the ligand and metal have come together the fun of derivatizing can begin.

X-ray quality crystals were grown from a slowly evaporated methylene chloride solution.