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Syntheses and crystal structures of novel chalcogenido-bridged niobium copper clusters
In the presence of tertiary phosphines, the reaction of NbCl5 and Copper(I) salts with Se(SiMe3)2 (E = S, Se) affords the new chalcogenido-bridged niobium-copper cluster compounds x 1[NbCu3Se4(PiPr2Me) 3] (1) and [NbCu4Se4Cl (PPh3) 4] (2). Using E(R)SiMe3 (E = S, Se, R = Ph, nPr) instead of the bisilylated selenium species leads to the compounds [NbCu2(SPh)6(PMe3)2] (3), [NbCu2(SPh)6(PnPr3)2] (4), [NbCu2(SePh)6(PMe3)2] (5), [NbCu2(SePh)6(PnPr3)2] (6), [NbCu2(SePh)6(PiPr3) 2] (7), [NbCu2(SePh)6(PtBu 3)2] (8), [NbCu2(SePh)6(P iPr2Me)2] (9), [NbCu2(SePh) 6(PPhEt2)2] (10), [Nb2Cu 2(SnPr)8(PnPr3) 2Cl2] (11) and [Nb2Cu6(S nPr)12(PiPr3)2Cl 4]¡¤2 CH3CN (12¡¤1 CH3CN). By reacting CuI salts and NbCl5 with the monosilylated selenides Se(tBu)SiMe3 and Se(iPr)SiMe 3 which have a weak Se-C bond the products [Nb2Cu 6Se6(PiPr3)6Cl 4] (13), [Nb2Cu4Se2(Se iPr)6-(PnPr3)4Cl 2] (14) and [Nb2Cu6Se2(Se iPr)10(PEt2Me)2Cl 2]¡¤DME (15) are formed which contain selenide as well as alkylselenolate ligands. The molecular structures of all of these new compounds were determined by single crystal X-ray diffraction measurements.
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Reference£º
Copper catalysis in organic synthesis – NCBI,
Special Issue “Fundamentals and Applications of Copper-Based Catalysts”