Abstract
Reaction of Fe3(CO)12 and Ph2PH in the presence of Et3N in THF at 0 °C immediately forms Fe2(CO)6(μ-PPh2)(μ-OH) (1), Fe2(CO)6(μ-PPh2)(μ-k2O,P-OPPh2) (2), and Fe2(CO)6(μ-PPh2)2 (3) in yields of 25, 14, and 19%, respectively. Experiments confirm that Et3N shortens the reaction time. The absence of O2 hinders the formation of 2. The presence of H2O can increase the yield of 1. Their structures have been determined by X-ray crystallography and the complexes have been completely characterized by EA, IR, and 1H, 13C, 31P NMR. Electrochemical studies reveal that they exhibit catalytic H2-producing activities.
Graphical Abstract
![](/cms/asset/73a41064-57a9-44aa-a05e-f0318da6b33d/gcoo_a_940925_uf0001_oc.jpg)