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Treatment of Co₃(μ₃-CC≡CR)(μ-dppm)(CO)₇ with O₂ (air) in the presence of [FcH]PF₆ afforded Co₃{μ₃-CC(O)R}(μ-dppm)(CO)₇ by the formal conversion –C≡C– + O–O → >C–O + C≡O. In this way, complexes with R = Ph, Fc, and W(CO)₃Cp, bis-clusters {Co₃(μ-dppm)(CO)₇}₂{μ₃:μ₃-[≡C(O)(C≡C)C≡]}, {Co₃(μ-dppm)(CO)₇}₂{μ₃:μ₃-[≡C(O)(C≡C)xC(O)C≡]} (x = 1, 2), and {Co₃(μ-dppm)(CO)₇}₂{μ₃:μ₃-[≡CC(O)C≡CC₆H4C≡CC(O)C≡]}, and heterometallic bis-clusters {Co₃(μ-dppm)(CO)₇}{μ₃:μ₃-[≡CC(O)C≡CC≡]}{M₃(μ-H)₃(CO)₉} (M = Ru, Os) have been prepared. Single-crystal XRD structure determinations of several products are reported together with that of precursor {Co₃(μ-dppm)(CO)₇}₂{μ₃:μ₃-[≡C(C≡C)₂C₆H₄(C≡C)₂C≡]}.
A series of alkynyl-tricobalt carbonyl clusters, Co₃(μ₃-CnR)(μ-dppm)(CO)₇ [R = But, Ph, C₆H₄I, C₆H₄C≡CPh, SiMe₃, Fc, Au(PPh₃)] containing three, five or seven carbons in the chain, have been prepared by elimination of phosphine–gold(I) halides in reactions between Co₃(μ₃-CBr)(μ-dppm)(CO)₇ and Au(C≡CR)(PPh₃) or between Co₃{μ₃-CC≡CAu(PR₃)} (μ-dppm)(CO)₇ (R = Ph, tol) and IC≡CR′ (R′ = SiMe₃, Fc). The use of poly-substituted arenes or ferrocenes has enabled preparation of the complexes 1,4-{(OC)₇(μ-dppm)Co₃ (μ₃-CC≡C)}₂C₆H₃X-5 (X = H, Br), 1,3,5-{(OC)₇(μ-dppm)Co₃(μ₃-CC≡C)}₃C₆H₃ and 1,1′-{(OC)₇(μ-dppm)Co₃ (μ₃-CC≡C)}₂Fc′ [Fc′ = Fe(η-C₅H₄-)₂]. The X-ray determined molecular structures of 12 of the complexes are reported.
The syntheses and characterizations of several complexes containing ferrocenylethynyl and ferrocene-1,1'-bis(ethynyl) groups attached to M(PP)Cp'[M = Fe, Ru, PP = dppe, Cp'= Cp*; M = Ru, Os, PP = (PPh3)(2), dppe, Cp' = Cp] are described. Reactions with tetracyanoethene have given either tetracyanobuta-1,3-dienyl or eta(3)-allylic derivatives, while addition of Me+ afforded the corresponding vinylidene derivatives. Some electrochemical measurements are discussed in terms of electronic communication between the redox-active M(PP)Cp' groups through the ferrocene nucleus. The molecular structures of 14 of these complexes have been determined by crystallographic methods.
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