Dear Andreas, It's a closely guarded secret that the data collection for small molecules is not that different from that for macromolecular crystallography. (Otherwise there's the risk that more macromolecular folks might get hooked to the addictive charm of the small-molecule world!)
Just mount the crystals (various oils typically work) and test them for diffraction. Usual tests: easily indexable, Bravais lattice, Laue group, integration stats? It helps if the compound is stable (which seems to be the case here?). Switch on the liquid nitrogen stream on the diffractometer, as usual. You may need to go down with the wattage, especially for a large crystal like you describe, and if a heavy metal is present. Try to measure data to at least 0.83 A if you can (requirement for Acta Cryst.; should be doable even on a Cu source), though that is not necessarily required for structure solution (better than 1.1 A should be fine for that). Programs after integration, through refinement: This is a matter of personal choice. There are many excellent software packages. Here's a list that does not claim to be exhaustive (in alphabetical order), as I hardly know all of the possibilities (others should be able to add to this list): CRYSTALS, D. Watkin group, Oxford: <http://www.xtl.ox.ac.uk/crystals.1.html> JANA, V. Petricek group, Prague: <http://www-xray.fzu.cz/jana/jana.html> SADABS, XPREP, SHELXT/SHELXS, SHELXL, G. Sheldrick, Goettingen: <http://shelx.uni-ac.gwdg.de/SHELX/> SIR, C. Giacovazzo group, Bari: <http://www.ic.cnr.it/icnew/site/index.php> SUPERFLIP, L. Palatinus, Prague: <http://superflip.fzu.cz/>. For visualization, you could use ShelXle or Olex2 (on an occasion or two, I've even used Coot!). For validation, you would need PLATON and CHECKCIF, <http://checkcif.iucr.org/>. A disadvantage of small molecule crystallography is that structure solution now typically takes only a few seconds. So no time for coffee there! Wish you lots of fun nevertheless. Best regards, Navdeep --- On Mon, Mar 24, 2014 at 06:04:25PM +0000, Andreas Förster wrote: > Dear all, > > I've been approached by a materials student with a petri dish full > of big, sturdy, salty, yellow crystals. He claims I have the best > kit for single-crystal diffraction on campus. > > I would very much appreciate advice on how to deal with this, > anything in the range from "won't work" to "use software X to > analyze data in space group P-43N" would be welcome. > > Thanks. > > > Andreas --- Navdeep Sidhu Departments of Structural Chemistry & Pediatrics II University of Goettingen Office Address: Institute of Inorganic Chemistry Tammannstrasse 4 37077 Goettingen Germany Email: nsi...@shelx.uni-ac.gwdg.de Phone: +49 551 39 33059 Fax: +49 551 39 22582 Homepage: http://shelx.uni-ac.gwdg.de/~nsidhu/crystals_in_flatland.html ---
