Submitted by Julia C. / University of California Davis on Sat, 09/20/2008 - 20:38
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I am looking for a straightforward synthesis of good single crystals for our Inorganic Chemistry students (juniors and seniors) to make in lab and then use to learn about collecting structural data and solving the single crystal structure using our software. The compound should be safe, stable, and easy to handle. It can be (but doesn't need to be) a molecular compound, and should be more complex than a simple salt. If anyone has ideas, suggestions, or recommendations, I would love to hear them. Thank you!
Nancy Williams / Scripps College, Pitzer College, Claremont McKenna College

Alas, I'm a platinum chemist, so most of the compounds I work with are sorta ho-hum in the color department, but Pt(SEt2)2Cl2 crystalizes beautifully from CH2Cl2 and hexanes, and is a beautiful yellow.

 K2PtCl4 + SEt2 (3 eq or so) in water....run overnight (or at 100C for an hour). Subsequently, extract yellow product with CH2Cl2 thrice, remove solvent in vacuo. Recrystalize (layered) from CH2Cl2/hexanes (ca. 1:5 ratio) in a -20 freezer for a week. Presto. Xtals!


Sat, 09/20/2008 - 21:01 Permalink
Adam Johnson / Harvey Mudd College

In reply to by Nancy Williams / Scripps College, Pitzer College, Claremont McKenna College

Metal acac complexes are notoriously colorful and crystalline.  There are a bunch of preps out there but Woolins' book "Inorganic experiments" has good preps and solvents for recrystallization.  We have made Cu, Fe, Co... maybe Ni?

Adam

Mon, 09/22/2008 - 15:22 Permalink
Kurt Birdwhistell / Loyola University New Orleans

In reply to by Adam Johnson / Harvey Mudd College

I would make one of the Cobalt ammine complexes such as hexammine Cobalt(III)chloride.  Plenty of preparations out there for this one.  If interested I can send you one.  Also Angelici's book has a preparation. 

Kurt

Sun, 10/05/2008 - 22:28 Permalink
Hilary Eppley / DePauw University

In reply to by Adam Johnson / Harvey Mudd College

We do this in our intro class, and while we don't actually solve the crystal structures, I do have a crystal growing contest. We do Co (dark green), Fe (red), Mn (dark brown), and Cr (the Cr is a particularly nice purple color!). I give them a range of solvents and techniques to choose from for the recrystallization--If you contact me, I'd be happy to share the write up on the crystallization part. --Hilary heppley@depauw.edu
Sun, 10/12/2008 - 20:08 Permalink