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η 3 -Allylhydrogensulfidonickel (2) reacts with n-butyllithium with elimination of lithium sulfide and formation of the ionic η 3 -allylnickel-sulfur-cluster [(η 3 -C 3 H 5 Ni) 3 S 2 ] + [Li(THF) 2 ] -  (4). The crystal structure of the analogous THF-TMEDA-adduct (4′) indicates that the nickel and sulfur atoms of the anion adopt a trigonal bipyramidal arrangement, in which the sulfur atoms are at the apices of the bipyramid. The Li(THF) 2+  cation in 4 can be replaced by the (n-C 4 H 9 ) 4 N +  cation (5). The  1 H NMR spectra suggest the presence of two stereoisomers of the anionic clusters in 4 and 5 having C 3h  and C s  symmetry. In the reaction of η 3 -allyl- or η 3 -methallylhydrogensulfidopalladium (6, 6 a) with n-butyl-lithium crystalline compounds having the composition RC 3 H 4 PdSLi(THF)≈ 4 , R = H, CH 3  (7, 7 a) are obtained; their  1 H NMR spectra also reveal the existence of the two stereoisomers having C 3h  and C s  symmetry. The same type of stereoisomerism is observed with the crystalline [(n-C 4 H 9 ) 4 N] + [(η 3 -C 3 H 5 Pd) 3 S 2 ] -  (8) obtained from 7 and (n-C 4 H 9 ) 4 N+ClO 4  - . For 7 and 7 a an ionic structure consisting of trigonal bipyramidal (η 3 -RC 3 H 4 Pd) 3 S 2 - anions and Li 3 S(THF) 4 + cations is proposed.

zeitschrift für naturforschung b

η 3 -Allylmeta]l-Schwefel-Komplexe, VI. Anionische η 3 -Allylnickel- und -palladium-Schwefel-Cluster/ η 3 -Allylmetal-Sulfur-Complexes, VI.  Anionic η 3 -Allylnickel- and -palladium-Sulfur-Clusters