Abstract
Reactions of Cu(I) salts with KS2COR (R = iPr, nPr) and NaBH4 in 7:6:1 ratio in acetone at room temperature yield xanthate ligated heptanuclear copper (I) hydride clusters [Cu7(H)(S2COR)6] [R = iPr (1H), nPr (2H)]. Their deuteride analogs [Cu7(D)(S2COR)6] [R = iPr (1D), nPr (2D)] have been obtained from NaBD4. The clusters are structurally characterized by using electrospray ionization mass spectrometry (ESI-MS), NMR, and X-ray crystallography (1H, 2H). Structural elucidations reveal that clusters 1H and 2H feature a tricapped triangular pyramid copper arrangement with an interstitial hydride. To the best of our knowledge 1H and 2H are the largest Cu(I) clusters stabilized by xanthate ligands. Similarly the 1:1 ratio reaction of Cu(I) salts with KS2COR in the absence of hydride sources results in [Cu3(S2COiPr)3]∞ (3), a linear chain coordination polymer. Interestingly a new coordination mode (κ4: μ3-S, μ1-S) has been observed in 3 for the first time in xanthate chemistry.
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