Compounds of Groups 3 to 4 and the f elements by Bochmann M.

By Bochmann M.

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279 The reaction of TlCp with a slurry of Sm(TpMe2)2 in THF [TpMe2 ¼ tris(3,5-dimethylpyrazolyl)hydroborate] resulted in the formation of thallium metal and CpSm(TpMe2)2. 281 Heating of CpSm(TpMe2)2 overnight in a sealed tube at 165  C gave two products: one is the result of an unprecedented transformation of the Tp ligand to the mixed pyrazolylborate [HB(3,5-Me2pz)2(C5H4)], the second product is 2n NaCpt + 2n LnCl3 THF 60 °C {[CptLn(THF)]2(μ 2-Cl)2(μ 3-Cl)3Na(THF)}n Ln = Nd, Sm, Gd, Yb Cpt = ButC5H4 {[CptSm(THF)]2(μ 2-Cl)2(μ 3-Cl)3Na(THF)}n Scheme 59 + Na2Se5 [Na(THF)6]2[Cpt6Sm6(μ 6-Se)(μ-Se2)6] 35 36 Complexes of Group 3 and Lanthanide Elements Si Ln[N(SiMe3)2]3 + Me2Si(C5Me4H)(ButNH) Ln toluene/reflux N SiMe3 SiMe3 N –2NH(SiMe3)2 Ln = Nd, Lu Si Sm[N(SiMe3)2]3 + Me2Si(C5Me4H)(ButNH) toluene/reflux Sm N SiMe3 SiMe3 N + major Ln[CH(SiMe3)2]3 + Me2Si(C5Me4H)(ButNH) toluene/reflux –2CH2(SiMe3)2 Si Sm N NH Si minor SiMe3 Si Ln N CH SiMe3 Ln = Yb, Lu Scheme 60 Sm(TpMe2)2(3,5-Me2pz), which was also generated from the reaction of CpSm(TpMe2)2 with 3,5-dimethylpyrazole.

280 The synthesis of cyclopentadienyl lanthanide pyrazolate complexes and their reactivity towards dimethylsilicone has been reported. Reactions of Cp3Ln (Ln ¼ Ho, Dy, Yb, Sm) with 2 equiv. of HPzMe2 (HPzMe2 ¼ 3,5-dimethylpyrazole) in THF at room temperature yield complexes of the type CpLn(PzMe2)2 (Ln ¼ Ho, Dy), and Cp2Yb(PzMe2)(HpzMe2), and Sm(PzMe2)3, respectively. 282–284 The different products indicate that the number of cyclopentadienyl groups liberated from a Cp3Ln moiety is influenced by the size of the lanthanide ion.

322 The deuterated complex [(C5D5)2Dy(-Br)]2 has been prepared and structurally characterized. The synthesis involved the reaction of anhydrous DyBr3 with 2 equiv. 323 The crystal structure of [Cp2Sc(-Cl)]2 has been found to be isomorphous with that of [Cp2Dy(-Br)]2. 325 The bis(butenylcyclopentadienyl)lanthanide chlorides (C5H4CH2CH2CHTCH2)2LnCl(THF)2 (Ln ¼ Sm, Y, Dy, Er) have been synthesized as air- and moisture-sensitive, free-flowing oils. 333 The trichlorides of yttrium, samarium, and lutetium reacted with 2 equiv.

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