The reaction of Fe2(CO)4(h5-C5H5)2 with 4-N-methylpiperidine-disulphide affords [Fe(h5-C5H5)(μ-SC5H9NCH3]2, the crystal structure of which has been determined. The crystals are monoclinic, space group C2/c with a 18.761(3), b 14.543(2), c 9.556(1) Å, β 103.67(2)°. With Z = 4 the calculated density is 1.46 g cm cm-3; the final weighted R factor was 0.047 for 1645 independent reflections. The two carbonyl groups and the two sulphur-attached piperidine groups in the dimeric structure are both cisoid. Reaction with CH3I leads to methylation that with aqueous HClO4 to protonation of the nitrogen atoms of the piperidine rings, giving formation of the [Fe(h5- C5H5)(CO)(μ-SC5H9N(CH3)2]2I2 · 2H2O salt and [Fe(h5-C5H5)(CO)(μ-SC5- H9NHCH3)]22+ cation, respectively. © 1986.
|Journal||Journal of Organometallic Chemistry|
|Publication status||Published - 25 Nov 1986|