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Complexes of the types R 3 Pb-Fe(CO) 2 Cp [R=Me (a). Et (1b),  i Pr (lc),  i Bu (Id)]. R 2 Pb[Fe(CO) 2 Cp] 2  [R=Me (2a), Et (2b)],  i Pr 2 (Br)Pb-Fe(CO) 2 Cp (3c) and [R 2 PbFe(CO) 4 ] 2  [R=Me (4a), Et (4b).  i Pr (4c)], as well as the spiro-complexes Pb[Fe(CO) 4 PbR 2 ] 2  [R = Me (5a). Et (5b).  i Pr (5c)] and Pb[Fe(CO) 4 ] 4  (6) were studied by multinuclear magnetic resonance spectroscopy ( 1 H.  13 C,  207 Pb NMR). For the first time, coupling constants  1 J( 207 Pb 57 Fe) were determined, covering a range between 33.5 (6) and 117 Hz (4a). The magnitude of the geminal coupling constants ∣ 2 J( 207 Pb 207 Pb) ∣ in the spiro-compounds 5 decreases from 1090.0 Hz (5a) to 377.0 Hz (5c). The signs of the coupling constants  n J( 207 Pb 13 C (R) ) (n = 1, 2) and  n J( 207 Pb 1 H (R) ) (n = 2, 3) were determined by various 2D NMR experiments. Among all known Pb(IV) compounds the lowest  207 Pb nuclear magnetic shielding was found in Pb[Fe(CO) 4 ] 4  (6): δ 207 Pb +3586.6. According to the single crystal X-ray structure determination of 4b (orthorhombic; space group Pbca; a = 967.4, b = 1367.7, c = 1772.4 pm), the Pb 2 Fe 2  ring is planar with bond angles FePbFe = 102.8° and PbFePb = 77.2°, and there is a relatively short transannular distance of 340.8 pm between the two lead atoms.

Carbonyliron-Lead Complexes: Multinuclear Magnetic Resonance Study in Solution and X-Ray Structure Determination of [Et 2 PbFe(CO) 4 ] 2