Abstract
The cluster cis-[Re6Se8(PEt3)4I2] undergoes substitution reactions with neutral ligands L in the presence of AgSbF6 to afford the cis-disubstituted clusters [Re6Se8(PEt3)4L2]2+ (L = MeCN (6), t-BuCN, DMF, Me2SO (9)). Cluster 6 reacts with pyridine to give [Re6Se8(PEt3)4(py)2]2+. Retention of stereochemistry was demonstrated from 31P NMR spectra and the crystal structure of [9](SbF6)2, which revealed the two Me2SO ligands to be O-bonded at adjacent Re sites of the face-capped octahedral [Re6(μ3-Se)8]2+ core. The clusters cis-[Re6Se8(PEt3)4L2]2+ are of interest as possible precursors to oligomeric clusters under thermolysis conditions where one or both ligands L are removed. Thermolysis of orange-red [6](SbF6)2 (180 °C, 24 h) afforded a brown-green crystalline product identified by an X-ray structure determination to contain the dicluster [Re12Se16(PEt3)8(MeCN)2]4+ (11). Two [Re6Se8]2+ cluster units are bridged by a Re2Se2 rhomb to afford the centrosymmetric core [Re12(μ3-Se)14(μ4-Se)2]4+, established recen...
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