The synthesis of five-membered P-heterocyclic iron(0) complexes possessing a P–H unit and two heteroatoms (E = O, N), directly bound to phosphorus, is described. Initial problems to achieve access via “classical” reduction of P–Cl bonds of P-heterocycle complexes, e.g., leading to P–P coupling, could be solved by a “combined two-step” reduction/complexation. The use of K[Fe(CO)4H] not only opened access to such heterocyclic phosphane Fe(CO)4 complexes but also allowed the synthesis of sterically non-shielded ‘secondary’ heterocyclic phosphane complexes. Spectroscopic and structural parameters are discussed.
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