Synthesis, Crystal Structure, and Spectroscopic and Magnetic Properties of a New [Co4O(OOCNC9H18)6] Cluster

The synthesis, X-ray structure, and NMR ( 1 H, 13 C, 17 O) and magnetic characterization of the complexes [Co(CO) 2 (tmpo)] ( 1 ) and [Co 4 O(OOCNC 9 H 18 ) 6 ] ( 2 ) are reported. Reaction of Co 2 (CO) 8 in the presence of a 4-fold excess of tmpo yields in a few minutes the blue carbamato complex 2 in >80% yield. The reaction possibly takes place by a cascade mechanism with the complex [Co(CO) 2 tmpo] ( 1 ) as an intermediate and the nitroxyl radical acting as an oxidizing agent.