Abstract
The reactions of Re 2Cl 4(PEt 2Ph) 4, Et=ethyl and Ph=phenyl, with excess methyl disulfide (MeSSMe) and phenyl disulfide (PhSSPh) produce the compounds Re 2(μ-SMe) 3Cl 4(PEt 2Ph) 2 ( 1) and Re 2(μ-SPh) 3Cl 4(PEt 2Ph) 2·acetone ( 2), respectively. Similarly, Re 2Cl 5(PMePh 2) 3 reacts with PhSSPh to yield Re 2(μ-SPh) 3Cl 4(PMePh 2) 2 ( 3) and Re 2Br 4(PEt 2Ph) 4 reacts with either EtSSEt or PhSSPh to produce either Re 2(μ-SEt) 3Br 4(PEt 2Ph) 2 ( 4) or Re 2(μ-SPh) 3Cl 4(PEt 2Ph) 2 ( 5). All of these new Re 2 7+ complexes display one-electron paramagnetism. X-ray crystallographic studies of compounds 1– 4 reveal a common face-sharing bioctahedral structure with three bridging thiolate ligands. The ReRe bond distances (averaging 2.473 Å) are indicative of multiple metal–metal bonds. Compound 1 may also be prepared in low yield by the reaction of Re 2Cl 4(PEt 2Ph) 4 with 2,5-dithiahexane or the reaction of ( n-Bu 4N) 2Re 2Cl 8 with a mixture of MeSSMe and PEt 2Ph.
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