A Series of Cyclopentadienyl Lanthanum Complexes with Metalloid Germanium Clusters.

IF 4.3 2区化学 Q1 CHEMISTRY, INORGANIC & NUCLEAR Inorganic Chemistry Pub Date : 2024-07-10 DOI:10.1021/acs.inorgchem.4c01082

Kevin Woern, Andrey I Poddel'sky, Alex Mayer, Claudio Schrenk, Andreas Schnepf, Svetlana V Klementyeva

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Abstract

A series of cyclopentadienyllanthanum complexes with the disilylated metalloid germanium cluster [Ge₉(Hyp)₂]^2- [Hyp = Si(SiMe₃)₃] has been prepared and fully characterized. The synthetic procedure is based on the salt metathesis reaction of two different cyclopentadienyllanthanum diiodides CpLaI₂ (Cp: Cp*, pentamethylcyclopentadienyl; Cp^ttt, 1,2,4-tri-tert-butylcyclopentadienyl) with K₂[Ge₉(Hyp)₂] in tetrahydrofuran (THF) with a subsequent extraction with n-hexane. The composition of the obtained compounds and the mode of coordination of the germanium cluster to the rare-earth metal are strongly influenced by the steric demand of the cyclopentadienyl ligands and the crystallization conditions. The centrosymmetric dimeric compounds with the common formula [CpLa(solv)(η^2,3-Ge₉(Hyp)₂)]₂ [1, Cp = Cp*, solv-THF; 2, Cp = Cp^ttt, solv-NCCH₂C(Me)NSiMe₃] have been isolated by the slow evaporation of a n-hexane solution, while a mononuclear complex [Cp^tttLa(THF)₂(η³-Ge₉(Hyp)₂)] (4) was found by crystallization from THF. The repeated recrystallization of 1 from n-hexane afforded the asymmetric dimer [Cp*La(THF)(η^2,3-Ge₉(Hyp)₂)][Cp*La(η^2,3-Ge₉(Hyp)₂)] (3) with only one coordinated THF molecule.

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具有类金属锗簇的环戊二烯镧配合物系列。

我们制备了一系列具有二硅烷化金属锗簇[Ge9(Hyp)2]2- [Hyp = Si(SiMe3)3]的环戊二烯镧配合物，并对其进行了全面表征。合成过程基于两种不同的环戊二烯镧二碘化物 CpLaI2（Cp：Cp*，五甲基环戊二烯；Cpttt，1,2,4-三叔丁基环戊二烯）与 K2[Ge9(Hyp)2] 在四氢呋喃（THF）中的盐元合成反应，随后用正己烷萃取。环戊二烯配体的立体需求和结晶条件对所获化合物的组成以及锗团簇与稀土金属的配位方式有很大影响。中心对称二聚化合物的共同式为 [CpLa(solv)(η2,3-Ge9(Hyp)2)]2 [1, Cp = Cp*, solv-THF；2, Cp = Cpttt, solv-NCCH2C(Me)NSiMe3] 是通过正己烷溶液的缓慢蒸发分离出来的，而单核复合物 [CptttLa(THF)2(η3-Ge9(Hyp)2)] (4) 则是从 THF 中结晶出来的。从正己烷中反复重结晶 1 得到了不对称二聚体[Cp*La(THF)(η2,3-Ge9(Hyp)2)][Cp*La(η2,3-Ge9(Hyp)2)](3)，其中只有一个配位的 THF 分子。

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来源期刊

Inorganic Chemistry 化学-无机化学与核化学

CiteScore

7.60

自引率

13.00%

发文量

1960

审稿时长

1.9 months

期刊介绍： Inorganic Chemistry publishes fundamental studies in all phases of inorganic chemistry. Coverage includes experimental and theoretical reports on quantitative studies of structure and thermodynamics, kinetics, mechanisms of inorganic reactions, bioinorganic chemistry, and relevant aspects of organometallic chemistry, solid-state phenomena, and chemical bonding theory. Emphasis is placed on the synthesis, structure, thermodynamics, reactivity, spectroscopy, and bonding properties of significant new and known compounds.