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The photo-induced substitution of carbonyl ligands in the binuclear cyclopentadienyl-type complexes (CO) 3 M[C 5 H 4 (CH 2 ) n C 5 H 4 ]M(CO) 3  (n = 0 (fulvalene), M = Mn (1) and Re (2); n = 1 (bis(cyclopentadienyl)methane), M = Mn (3) and Re (4)) has been studied in the presence of tetrahydrothiophene, SC 4 H 8  (tht). Photodecarbonylation of 1 - 4 in tetrahydrofuran solution leads to solvent-stabilized intermediates which react with tht in the dark to give monosubstituted derivatives (CO) 3 M[C 5 H 4 (CH 2 ) n C 5 H 4 ]M(CO) 2 (tht) (1a - 4a). In the case of M = Mn, thtbridged compounds {(CO) 2 Mn[C 5 H 4 (CH 2 ) n C 5 H 4 ]Mn(CO) 2 }(μ-tht) (n = 0 (1b) and n = 1 (3b)) are also obtained which are the exclusive products of the photolysis of 1 and 3 in benzene in the presence of tht. Photodecarbonylation of 1 - 4 in neat tetrahydrothiophene produces disubstituted derivatives in the case of manganese, (tht)(CO) 2 Mn[C 5 H 4 (CH 2 ) n C 5 H 4 ]Mn(CO) 2 (tht) (n = 0 (1c) and n = 1 (3c)), whereas only the monosubstituted complexes 2a and 4a could be isolated in the case of rhenium. The molecular structure of the tht-bridged fulvalene complex 1b has been determined by an X-ray structure analysis. A special reaction of dimethyl disulfane with the photolyzed tetrahydrofuran solution of 2 leads to the bis(methylthiolato) compound (CO) 3 Re[C 5 H 4 - C 5 H 4 ]Re(CO)(SMe) 2  (5). The new complexes were characterized by their IR spectra v(CO) and their  1 H and  13 C NMR spectra.

zeitschrift für naturforschung b

Binuclear Fulvalene and Bis(cyclopentadienyl)methane Halfsandwich Complexes of Manganese and Rhenium Containing Tetrahydrothiophene Ligands. X-Ray Structure Analysis of {(CO) 2 Mn[C 5 H 4 -C 5 H 4 ]Mn(CO) 2 }(μ-SC 4 H 8 )