A reader sends this new literature citation along, from Organometallics. He directed my attention to the Supplementary Information file, page 12. And what do we find there?
. . .Solvent was then removed to leave a yellow residue in the vial, the remaining clear, yellow solution was concentrated to a volume of about 1ml, and diethyl ether was added in a dropwise manner to the stirred solution to precipitate a yellow solid. The vial was centrifuged so the supernatant solvent could be decanted off by Pasteur pipette. The yellow solid was washed twice more with ether and the dried completely under high vacuum to give 99mg (93% yield) of product.
Emma, please insert NMR data here! where are they? and for this compound, just make up an elemental analysis…
And don’t forget to proofread the manuscript, either, while you’re at it. Oops.
Update: I see that Chembark is on this one, and has gone as far as contacting the corresponding author, whose day has gotten quite a bit longer. . .