Abstract

The trirhenium complex Re 3(CO) 10[μ- SCH 2CH 2CH 2](μ-H) 3 ( 1) was found to produce an oligomerization of thietane at 25° C over 18 h to yield the new complex Re 3(CO) 10[μ-SCH 2CH 2CH 2 SCH 2CH 2-CH 2SCH 2CH 2CH 2SCH 2CH 2CH 2](μ-H) 3 ( 2), in 47% yield. Details of the structure of compound 2 were obtained rom a single crystal X-ray diffraction analysis of its PMe 2Ph derivative 3. It was found to contain a bridging thiolate group SCH 2CH 2CH 2 that is terminated with a SCH 2CH 2CH 2SCH 2CH 2CH 2SCH 2CH 2CH 2 macrocycle. The macrocycle was cleaved from the cluster by treatment with NaOEt and the free molecule trithiacyclodecane was isolated in 32% yield. Crystal data for 3: space group = P2 1/ n, a = 8.637(2) Å, b = 41.80(1) Å, c = 15.418(2) Å, β = 111.79 (2)°, Z = 4, 2836 reflections, R = 0.036.

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