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By reacting [{Cp‴Fe(CO) 2 } 2 (µ,η 1:1 -P 4 )] ( 1 ) with in situ generated phosphenium ions [Ph 2 P][A] ([A] - = [OTf] - = [O 3 SCF 3 ] - , [PF 6 ] - ), a mixture of two main products of the composition [{Cp‴Fe(CO) 2 } 2 (µ,η 1:1 -P 5 (C 6 H 5 ) 2 )][PF 6 ] ( 2a and 3a ) could be identified by extensive 31 P NMR spectroscopic studies at 193 K. Compound 3a was also characterized by X-ray diffraction analysis, showing the rarely observed bicyclo[2.1.0]pentaphosphapentane unit. At room temperature, the novel compound [{Cp‴Fe}(µ,η 4:1 -P 5 Ph 2 ){Cp‴(CO) 2 Fe}][PF 6 ] ( 4 ) is formed by decarbonylation. Reacting 1 with in situ generated diphenyl arsenium ions gives short-lived intermediates at 193 K which disproportionate at room temperature into tetraphenyldiarsine and [{Cp‴Fe(CO) 2 } 4 (µ 4 ,η 1:1:1:1 -P 8 )][OTf] 2 ( 5 ) containing a tetracyclo[3.3.0.0 2,7 .0 3,6 ]octaphosphaoctane ligand.

Insertion of Phosphenium Ions into a Bicyclo[1.1.0]Tetraphosphabutane Iron Complex