Photolysis of Cp′(CO) 2FeSiMe2O (2-C5H4N)(1a: Cp′= η5-C5H5 (Cp), 1b: Cp′= η5- C5Me5 (Cp*)) afforded Cp′(CO) Fe [κ2 (Si, N)-SiMe2O (2-C5H4N)](2a: Cp′= Cp, 2b: Cp′= Cp*) in good yield each. These cyclic compounds also formed in moderate yields through photoreaction of Cp′(CO) 2FeSiMe3 with HSiMe2O (2-C5H4N)(3). Single-crystal X- ray diffraction study confirmed the structure of 2b containing a five-membered chelate ring ...