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首页> 外文期刊>Chemistry: A European journal >Potential Precursors for Terminal Methylidene Rare-Earth-Metal Complexes Supported by a Superbulky Tris(pyrazolyl)borato Ligand
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Potential Precursors for Terminal Methylidene Rare-Earth-Metal Complexes Supported by a Superbulky Tris(pyrazolyl)borato Ligand

机译：用于Superbulky Tris（吡唑基）硼酸盐配体的末端甲基稀土金属配合物的潜在前体

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摘要

A series of solvent-free heteroleptic terminal rareearth-metal alkyl complexes stabilized by a superbulky tris-(pyrazolyl)borato ligand with the general formula [TptBu,MeLnMeR] have been synthesized and fully characterized. Treatment of the heterobimetallic mixed methyl/tetramethylaluminate compounds [TptBu,MeLnMe(AlMe4)] (Ln=Y, Lu) with two equivalents of the mild halogenido transfer reagents SiMe3X (X=Cl, I) gave [TptBu,MeLnX2] in high yields. The addition of only one equivalent of SiMe3Cl to [TptBu,MeLuMe(AlMe4)] selectively afforded the desired mixed methyl/chloride complex [TptBu,MeLuMeCl]. Further reactivity studies of [TptBu,MeLuMeCl] with LiR or KR (R=CH_2Ph, CH_2SiMe_3) through salt metathesis led to the monomeric mixed-alkyl derivatives [TptBu,MeLuMe(CH_2SiMe_3)] and [TptBu,MeLuMe(CH_2Ph)], respectively, in good yields. The SiMe4 elimination protocols were also applicable when using SiMe3X featuring more weakly coordinating moieties (here X=OTf, NTf2). X-ray structure analyses of this diverse set of new [TptBu,MeLnMeR/X] compounds were performed to reveal any electronic and steric effects of the varying monoanionic ligands R and X, including exact cone-angle calculations of the tridentate tris(pyrazolyl)borato ligand. Deeper insights into the reactivity of these potential precursors for terminal alkylidene rare-earth-metal complexes were gained through NMR spectroscopic studies.
机译：通过Superbulky Tris-（Pyrazolyl）硼酸盐配体稳定的一系列无溶剂异素末端稀释 - 金属烷基复合物，其具有通式[TPTBU，Melnmer]已经合成并完全表征。用两当量的温和卤素转移试剂Sime3x（x = Cl，i）的偏异常混合甲基/四甲基/四甲基/四甲基/四甲基/四甲基铝酸盐化合物[TPTBU，MELNME（ALME4）]（LN = Y，Lu），得到高产率的[TPTBU，MELNX2] 。仅添加一种相当于SIME3Cl至[TPTBU，Melume4）]选择性地提供所需的混合甲基/氯化物复合物[TPTBU，Melumecl]。通过盐分离的Lir或Kr（R = CH_2ph，CH_2Sime_3）的[TPTBU，Melumecl]的进一步反应性研究通过盐复分解导致单体混合烷基衍生物[TPTBU，Melume（CH_2Sime_3）]和[TPTBU，Melume（CH_2PH）] ，良好的收益率。使用SIME3X具有更多弱协调部分时，SIME4消除协议也适用（这里X = OTF，NTF2）。进行这种多种新的新[TPTBU，Melnmer / X]化合物的X射线结构分析，揭示了不同单醌配体R和X的任何电子和空间效果，包括三叉子三（吡唑基）的精确锥角计算硼酸硼配体。通过NMR光谱研究获得了对末端亚烷基稀土金属配合物的这些潜在前体的反应性的更深层次的洞察力。

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