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Metallorganische Verbindungen der Lanthanoide. 111. Synthese und Charakterisierung kationischer Metallocen-Komplexe der Lanthanoide. Röntgenstrukturanalyse von [CpYb(THF)2][BPh4]
Authors:Herbert Schumann  Jrn Winterfeld  Markus R Keitsch  Katja Herrmann  Jrg Demtschuk
Institution:Herbert Schumann,Jörn Winterfeld,Markus R. Keitsch,Katja Herrmann,Jörg Demtschuk
Abstract:Organometallic Compounds of the Lanthanoids. 111. Synthesis and Characterization of Cationic Metallocene Complexes of the Lanthanoides. X-Ray Crystal Structure of Cp urn:x-wiley:00442313:media:ZAAC19966220905:tex2gif-stack-8 Yb(THF)2]BPh4] Cationic organolanthanoide compounds (C5H4R)2Sm(THF)2]BPh4] (R = tBu ( 1 ), SiMe3 ( 2 )), Pyrurn:x-wiley:00442313:media:ZAAC19966220905:tex2gif-stack-9Sm(THF)]BPh4] ( 3 ) (Pyr* = NC4H2tBu2-2,5), Cpurn:x-wiley:00442313:media:ZAAC19966220905:tex2gif-stack-10Ln(THF)2]BPh4] (Cp* = C5Me5; Ln = Y ( 4 ), Yb ( 5 )), and (C5Me4Et)2 Ln(THF)2]BPh4] (Ln = Y ( 6 ), Sm ( 7 )) have been synthesized by oxidation of the divalent metallocenes (C5H4R)2Sm(THF)2] (R = tBu, SiMe3), Pyrurn:x-wiley:00442313:media:ZAAC19966220905:tex2gif-stack-11Sm(THF)], Cpurn:x-wiley:00442313:media:ZAAC19966220905:tex2gif-stack-12Yb(THF), and (C5Me4Et)2Sm(THF)] with AgBPh4] and by protolysis of the lanthanoide alkyls Cpurn:x-wiley:00442313:media:ZAAC19966220905:tex2gif-stack-13YMe(THF)], Cpurn:x-wiley:00442313:media:ZAAC19966220905:tex2gif-stack-14YbCH(SiMe3)2], and (C5Me4Et)2LnCH(SiMe3)2] (Ln = Y, Sm) by NEt3H]BPh4]. The 1H- and 13C-NMR spectra of the new compounds are discussed. 5 crystallizes in the space group P21/c with a = 10.604(7), b = 21.749(3), c = 19.124(4) Å, β = 96.47(4)°, Z = 4 and V = 4383(3) Å3 (R = 0.0291 for 8517 observed reflections with Fo ≥ 4σ (Fo).
Keywords:Cationic Organolanthanoides  Lanthanoide(III) Tetraphenylborates  Yttrium  Samarium  Ytterbium
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