Metallorganische verbindungen der lanthanoide: LXXXV. Synthese und strukturaufklärung neuer cyclooctatetraenyl-cyclopentadienyl-sandwich-komplexe der seltenen erden
1994
Abstract The mixed sandwich complexes [(C 8 H 8 )Ln(C 5 Me 4 Et)(THF) x ] (Ln = Y 1 , La 2 , Nd 3 , Sm 4 , Gd 5 , Tm 6 , Lu 7 ), [(C 8 H 8 )Ln{C 5 H 2 (SiMe 3 ) 3 }(THF) x (Ln = Pr 8 , Dy 9 ) and [(C 8 H 8 )Pr(C 5 Ph 5 )] ( 10 ), have been prepared by the metathetic reaction of [(C 8 H 8 )Ln(μ-Cl)-(THF) n ] 2 with NaC 5 Me 4 Et, LiC 5 H 2 (SiMe 3 ) 3 and NaC 5 Ph 5 in THF. The 1:2 reaction of 7 with acetylacetone results in displacement of the (C 8 H 8 )-ligand to generate the new complex [(C 5 Me 4 Et)Ln(acac) 2 ] (acac = [CH 3 C(O)CHC(O)CH 3 ] − ) ( 11 ). The molecular structures of 7 (monoclinic space group P 2 1 / c with a = 990.4(5) pm, b = 1228.2(5) pm, c = 2757.5(16) pm, β = 93.92(4)°, V = 3346(3)·10 −30 m 3 and Z = 8) and 11 (triclinic space group P 1 with a = 957.3(3) pm, b = 1064.5(2) pm, c = 1068.3(2) pm, α = 94.19(12)°, β = 96.37(17)°, γ = 96.71(16)°, V = 1070.3(4)·10 −30 m 3 and Z = 2) have been determined by X-ray diffraction.
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