Synthesis and Characterization of Chalcogenolato-Bridged Allyl Palladium Complexes: Versatile Precursors for Palladium Chalcogenides
摘要:
The complexes [Pd(mu-ER)(eta(3)-allyl)](2) (ER = EMes; E = S, Se, allyl = C3H5, C4H7) have been isolated by the reaction of [Pb(ER)(2)](n) with [Pd-2(mu-Cl)(2)(eta(3)-allyl)(2)]. Similar reactions with [Pb(SeCH2CH2NMe2)(2)](n) resulted in the formation of a trinuclear complex [Pd3Cl2(kappa(2) -Se,N-SeCH2CH2NMe2)(eta(3)-allyl)(3)]. Treatment of [Pd(mu-SR)(eta(3)-C4H7)](2) with [Pd(SMes)(2)](n) in 1:1 ratio yielded [Pd-3(mu-SMes)(4)(eta(3)-C4H7)(2)]. These complexes were characterized by elemental analyses and mass, UV-vis, and NMR spectroscopy. The structures of [Pd-2(mu-EMes)(2)(eta(3)-C4H7)(2)] (E = S, Se) were established by single-crystal X-ray diffraction analysis, which revealed a syn configuration. Two new structural motifs for [Pd3Cl2(kappa(2)-Se,N-SeCH2CH2NMe2)(eta(3)-C3H5)(3)] and [Pd-3(mu-SMes)(4)(eta(3)-C4H7)(2)] have also been identified. Pyrolysis of [Pd(mu-ER)(eta(3)-C4H7)](2) yielded palladium chalcogenides, which were characterized by powder XRD and EDAX.
Synthesis and Characterization of Chalcogenolato-Bridged Allyl Palladium Complexes: Versatile Precursors for Palladium Chalcogenides
摘要:
The complexes [Pd(mu-ER)(eta(3)-allyl)](2) (ER = EMes; E = S, Se, allyl = C3H5, C4H7) have been isolated by the reaction of [Pb(ER)(2)](n) with [Pd-2(mu-Cl)(2)(eta(3)-allyl)(2)]. Similar reactions with [Pb(SeCH2CH2NMe2)(2)](n) resulted in the formation of a trinuclear complex [Pd3Cl2(kappa(2) -Se,N-SeCH2CH2NMe2)(eta(3)-allyl)(3)]. Treatment of [Pd(mu-SR)(eta(3)-C4H7)](2) with [Pd(SMes)(2)](n) in 1:1 ratio yielded [Pd-3(mu-SMes)(4)(eta(3)-C4H7)(2)]. These complexes were characterized by elemental analyses and mass, UV-vis, and NMR spectroscopy. The structures of [Pd-2(mu-EMes)(2)(eta(3)-C4H7)(2)] (E = S, Se) were established by single-crystal X-ray diffraction analysis, which revealed a syn configuration. Two new structural motifs for [Pd3Cl2(kappa(2)-Se,N-SeCH2CH2NMe2)(eta(3)-C3H5)(3)] and [Pd-3(mu-SMes)(4)(eta(3)-C4H7)(2)] have also been identified. Pyrolysis of [Pd(mu-ER)(eta(3)-C4H7)](2) yielded palladium chalcogenides, which were characterized by powder XRD and EDAX.