Abstract
In the reaction of C5H5Fe(CO)2l and C5H5Fe(CO)2CH3, respectively, with S-(+)-(C6H5)2PN(CH3)CH(CH3)(C6H5) (abbreviated P∅2R*) the complexes C5H5Fe(CO)(P∅2R*)I (1), C5H5Fe(CO)(P∅2R*)COCH3 (2), and C5H5Fe(CO)(P∅2R*)CH3 (3) are formed as pairs of diastereoisomers the components of which differ only in the configu­ration at the iron atom. CsH5Fe(CO)(P∅2R*)CH3 (3) can be obtained in higher yield by photochemical decarbonylation of C5H5Fe(CO)(P∅2R*)COCH3 (2). The (+)365- and (-)365-diastereoisomers of each pair exhibit different chemical shifts in the 1H NMR spectra. Diastereoisomer separation can be achieved by fractional crystallization. Starting with 57Fe metal (-)365-C5H5 57Fe(CO)(P∅2R*)I was prepared via 57Fel2, 57Fe(CO)4l2, C5H557Fe(CO)2l, and C5H557Fe(CO)(P∅2R*)I in order to demonstrate optical activity of a 57Fe compound in the y region by Mössbauer polarimetry in later experiments to be reported elsewhere.

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