In the past, we have adapted labs from Girolami, Rauchfuss, and Angelici’s “Synthesis and Technique in Inorganic Chemistry” book – specifically, we have done the YBa2Cu3Ox superconductor lab (and we didn’t have a diffractometer), the Mo-Mo quadruple bonds lab (#11), and the nickelocene lab (#20, though we start with commercially available nickelocene).  I like the nickelocene lab because it gives them glove box and Schlenk line experience.  I’ve also adapted a porphyrin lab I found in the Chemical Educator (2005, vol 10, p. 120-125).  Everyone synthesizes the porphyrin ligand, but then each student makes their own complex with a different transition metal ion.   Finally, a good lab to introduce nanoscience (as well as to emphasize absorption vs fluorescence spectroscopy) can be found in J Chem Ed – 2005, vol 82, p. 1697.

I hope this helps get you started.  

My course is also a separate course; one 4-hour laboratory session per week.Many (not all, maybe half) of my experiments are from (loosely or tightly) these two references:

Szafran, Z; Pike, R. M.; Singh, M. M.  Microscale Inorganic Chemistry

Girolami, G. S.; Rauchfuss, T. B.; Angelici, R. J.  Synthesis and Technique in Inorganic Chemistry,3rd Ed.

 with a smattering of input from

Woolins, J. D.  Inorganic Experiments

The rest are cobbled together from stuff I made up over the years, pre-existing labs, and stuff from the literature.

here is what we make {and the major take homes}

a series of MnBr(CO)2(dppm)(PR3) complexes, {IR/³¹P NMR}

Co(salen) {IR and O2 absorptio}

Pd-coupling (Buchwald/Hartwig) of an aryl bromide and an amine {organometallics and catalysis}

YBCO superconductor {non-stoichiometric compounds}

Co(en)₃ {chirality, UV-Vis}

phosphazene {³¹P NMR, IR, main group compounds}

 M(acac) complexes {paramagnetic NMR, Evans method, UV-Vis}

(arene)Cr(CO)₃ {IR,¹³C NMR}

Ru=C complexes {¹³C NMR, catalytic ring closing metathesis}

Not all students make all the compounds; its "choose your own adventure."  I am happy to share most of my materials, just ask.  Some of it is here on ViPEr (the manganese carbonyl experiment and the Pd coupling, for example).

I am teaching inorganic this fall and decided to try the project laid out in this J. Chem. Educ. article (2003, 80 (3), p 307) where the author describes adapting published research into lab experiments.  I am having trouble synthesizing the Mn^III(salpn)(acac) complex which is the first part of week 2.  The "detailed" synthesis laid out in the supplementary information to the J. Chem. Educ. paper is significantly different than that described in the research article with no explanation why.  I am just wondering if anyone currently uses this project or has in the past where the synthesis worked.

Edward,

Since I worked on Mn chemistry (and used the H2Salpn ligand even) I am trying to track down a copy of the Larsen paper from 1991.

My best guess is that you may be making Mn(III)(salpn)(CH3OH)+ which is readily being oxidized to the mu-oxo dimer, complex 3 in Michael Baldwin's JCE paper...what exactly is the color of your product(s)? If you have some of the green (complex 1) it might be possible to isolate pure compounds using chromatography.

I'm getting kinda rusty on the Mn chemistry as its now been over 4.5 years since I worked on any of it...but I hope maybe this helps.

Let me know how it works out, because I agree this is a great set of labs that I'd love to use if and when we ever have a semester-long inorganic lab course.

Best wishes!

:) Chris

Chris,

Thanks for the response.  The student-made sample was a dark tar that did dry to a mixture of green and black solid after washing with ether, so it might be complex #1.  It just took a long time to isolate and was not pure.  I tried the synthesis myself and let it reflux longer, but I got  black crystals which seemed identical to Mn(acac)3 or recovered starting material.  I just thought that if this has been used in lab classes before (i.e. 3-4 hour periods), the synthesis should be relatively hassle free so that students have time to make complex #2 from #1 in the same period as suggested.  Therefore I must be missing some pertinent information.  If I find out any more, I will post it here.

Ed