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The reaction of [Cp′Mn(CO) 2 NO]X (Cp = C 5 H 5 , C 5 H 4 Me = Cp′; X =BF 4 , PF 6 ) with PPh 2 H leads to the formation of the diphenylmanganiophosphonium salts [{CpMn(CO)NO}PPh 2 H]X, which can be deprotonated by DABCO to give the not isolable manganiophosphane {CpMn(CO)NO}PPh 2 . This reactive intermediate, however, can be methylated by MeI and CF 3 SO 3 Me or organometallated by C 5 H 5 Fe(CO) 2 Cl to yield the phosphonium salts [{Cp′Mn(CO)NO}PPh 2 Me]PF 6  and [{Cp′Mn(CO)NO}PPh 2 {C 5 H 5 Fe(CO) 2 }]PF 6 , respectively. The methyl derivative is deprotonated by  π BuLi to give the unstable methylene phosphorane {Cp′Mn(CO)NO}PPh 2 =CH 2 , an organometallated phosphorus ylide. The in situ from [{Cp′Mn(CO)NO}PPh 2 H]BF 4  generated phosphane {Cp′Mn(CO)NO}PPh 2  is oxidized by epoxycyclohexane to give the intermediate oxophosphorane {Cp′Mn(CO)NO}P(O)Ph 2 , which reacts with the still available starting material to yield the first dimanganiodiphenylphosphonium salt [{Cp′Mn(CO)NO} 2 PPh 2 ]BF 4 . The compounds have been characterized by spectroscopic (IR, NMR, MS), analytical (C, H, N) and X-ray diffraction investigations ([{C 5 H 5 Mn(CO)NO}PPh 2 H]BF 4 , [{Cp′Mn(CO)NO}PPh 2 Me]BF 6 , [{Cp′Mn(CO)NO} 2 PPh 2 ]-BF 4 ).

zeitschrift für naturforschung b

Manganiophosphonium-Salze: Synthese, Eigenschaften und Struktur von Komplexen des Typs [CpMn(CO)(NO)PPh 2 H]BF 4  und [Cp′Mn(CO)(NO)PPh 2 R]X (R = H, CH 3 , {CpMn(CO)(NO)}; X = BF 4 , PF 6 )