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Photolysis of the manganese half‐sandwich complex (η5‐C5Me5)Mn(CO)3 (1) in tetrahydrofuran (thf) cleanly yields the solvent complex (η5‐C5Me5)Mn(CO)2(thf) (2). Compound 2 is stable as solid at temperatures well below 0°C but undergoes spontaneous elimination of carbon monoxide at ambient temperature with concomitant formation of the novel dinuclear complex (η5‐C5Me5)2‐Mn2(μ‐CO)3 (3). While elemental analysis, infrared and mass spectroscopy as well as the 1H NMR and 13C NMR spectra unequivocally demonstrate this compound to adopt a highly symmetrical triply carbonyl‐bridged structure, a single‐crystal X‐ray diffraction study supports the presence of the first triple bond between manganese atoms (dMn – Mn 217.0(1) pm). An improved synthesis of tricarbonyl(η5‐pentamethylclopentadienyl)manganese (1) is also described.

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