As an update to my research endeavors I built another batch of molecular ligands for the Iridium today. I used varying temperatures as a test set for degradation since we were having problems with the Iridium not bonding. After analysis via nuclear magnetic spectroscopy (NMR) I was able to deduce a good pincer structure, though some issues during synthesis caused it to be a bit dirty, but dirty POCOP’s aside, it was stable.
Once my initial readings were in I could add the iridium in the dry box under argon atmosphere and see which temperature proved most able to stimulate the iridium bonding whilst not degrading the R-groups on my ligand.
This was done using tetrahydrofuran (THF) and toluene solvents whilst in the dry box. I used two different solvents since toluene seemed to not work well. That being said, the toluene sample showed the most promising read outs from the NMR, of course. More analysis will be needed, but despite some sketchy print outs and some minor mishaps the iridium may yet have taken! Tomorrow I will dissolve the solid portion of my sample in methylene chloride since it proved insoluble in deuterated toluene and see if the NMR comes out cleaner or at least with some stronger peaks. Wish me luck! It’d be nice to get published!