94792-87-7Relevant academic research and scientific papers
Ferrocenyl sulfides. Preparation and reactivity as bidentate chelating ligands
McCulloch, Beth,Ward, Donald L.,Woolins, J. Derek,Brubaker Jr., Carl H.
, p. 1425 - 1432 (1985)
A series of ferrocenyl sulfide derivatives, Fe(C5H4SR)2, where R = Me, i-Pr, I-Bu, Ph, and PhCH2, have been prepared by lithiation of ferrocene followed by reaction with the appropriate disulfide. The complexes were characterized by 1H and 13C NMR, mass spectra, and infrared spectroscopy. The ferrocenyl sulfide derivatives readily chelate palladium and platinum halides to form [3]ferrocenophane complexes Fe-(C5H4SR)2MX2 (R = Me, i-Pr, i-Bu, Ph, PhCH2; M = Pd, Pt; X = Cl, Br). 1H, 13C, and 195Pt NMR spectra were obtained where possible, and infrared, ultraviolet-visible and cyclic voltammetry data of the complexes are presented. The structure of Fe(C5H4S-i-Bu)2PdCl2 (6) was determined by single-crystal X-ray diffraction measurements. Compound 6 crystallizes in the orthorhombic space group Pbca with lattice parameters a = 22.168 (11) ?, b = 11.855 (7) ?, c = 16.131 (6) ?, Mr = 539.69, ρ(calcd) = 1.691 cm-3, and Z = 8. Least-squares refinement gave a final R value of 0.046 for 3689 observed reflections. The dihedral angle between the Fe-S1-S2 plane and the S1-Pd-S2 plane is 104.6°. The molecule 6 is fluxional in solution where the palladium atom flips from one side of the Fe-S1-S2 plane to the other.
