✍ Scribed by Sergei I. Kozhushkov; Jan Foerstner; Alf Kakoschke; Dirk Stellfeldt; Li Yong; Rudolf Wartchow; Armin de Meijere; Holger Butenschön
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Treatment of {η^5^:η^1^[2‐(di‐tert‐butylphosphanyl‐P)ethyl]cyclopentadienyl}cobalt(I) chloride (5) with methylenecyclopropane (3) or bicyclopropylidene (4), as well as with their spirocyclopropanated analogues methylenespiropentane (7), cyclopropylidenespiropentane (10), or 7,7′‐bi(dispiro[2.0.2.1]heptylidene) (15) in the presence of sodium amalgam at −50 °C, furnished the stable cobalt complexes 6, 9, 8, 11, and 16, respectively, in 72, 83, 84, 86, and 54 % isolated yield, respectively. The complexes 14 and 16 were also obtained by ligand exchange of the ethene complex {η^5^:η^1^[2‐(di‐tert‐butylphosphanyl‐P)ethyl]cyclopentadienyl}(η^2^‐ethene)cobalt(I) (12) with 13 and 15 in 79 and 52 % yield, respectively. The X‐ray crystal‐structure analyses of complexes 9, 14, and 16, as well as the NMR‐spectroscopic data of all complexes, reveal that they can be regarded as linear and branched cobalta[n]triangulanes. The thermal stability of complexes 6, 8, and 9 up to 109, 145, and 160 °C was determined by differential thermal analysis‐thermogravimetry (DTA‐TG) analysis.
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