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

By Bochmann M.

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These observations imply that there may be a continuous process leading from organosamarium hydroxo to oxo compounds. The solid-state IR spectrum of (Cp02Sm)2(-O)(-OH2) displays a broad band at 3300 cmÀ1 attributable to the O–H stretching frequency of the coordinated H2O molecule, while the spectra of the two forms of [Cp02Sm(-OH)]2 exhibit one sharp band at 3668 cmÀ1 that is assigned to the O–H stretching mode of the Ln(OH)Ln unit. Single crystal X-ray determinations on (Cp02Sm)2(-O)(-OH2) and [Cp02Sm(-OH)]2 confirmed their dimeric structures.

346 The bis(substituted cyclopentadienyl)lanthanide(III) halides [LnCpR2(-Cl)]2 (Ln ¼ Pr, Nd, Sm, Dy, Tb, Y), [LnCptt2(-X)]2 (X ¼ Cl, Ln ¼ La, Nd; X ¼ I, Ln ¼ Tm), 1 and [Nd(CpR 2SiMe2)(-Cl)]2, and bis(substituted cyclopentadienyl)lanthanide(II) complexes LnCpR2(THF)2 (Ln ¼ Sm, Eu, Yb), YbCpt2(THF)2, LnCptt2(THF)2 (Ln ¼ Sm, Yb), LnCpR2(Ln ¼ Sm, Eu, Yb), YbCpt2, LnCptt2 1 (Ln ¼ Sm, Yb), and Yb(CpR 2SiMe2)(THF)2 [CpR ¼ C5H4CH(SiMe3)2, Cpt ¼ C5H4SiMe2But, Cptt ¼ C5H3(SiMe2But)2-1,3, CpR1 ¼ C5H3CH(SiMe3)2-3] have been synthesized from the appropriate LnCl3, TmI3, or LnI2 with the selected sodium or potassium cyclopentadienide.

316 Sodium was shown to reduce [Cp02Sm(-F)]2 to Cp02Sm(THF). Upon treatment of [Cp02Sm(-F)]2 with an excess amount of NaCp0 in THF no Cp03Sm was isolated. Reaction of this complex with 1 equiv. of anhydrous AlCl3 gave [Cp02Sm(-Cl)]2. The bimetallic compound Cp02Sm(-F)(-Cl)AlCl2 was not isolated. [Cp02Sm(-F)]2 reacted with 1 equiv. 316 A facile new synthetic route to obtain [Cp2Yb(-F)(THF)]2, which involves the reaction of Cp2Yb(DME) with perfluorodecalin or perfluoro(methylcyclohexane) in THF, has been discovered.

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