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首页> 外文期刊>Chemistry: A European journal >Rare-Earth-Metal Methyl, Amide, and Imide Complexes Supported by a Superbulky Scorpionate Ligand
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Rare-Earth-Metal Methyl, Amide, and Imide Complexes Supported by a Superbulky Scorpionate Ligand

机译：超级大块蝎形配体支持的稀土金属甲基，酰胺和酰亚胺配合物

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The reaction of monomeric [(Tp(tBu,Me)) LuMe2] (Tp(tBu,Me) = tris(3-Me-5-tBu-pyrazolyl) borate) with primary aliphatic amines H2NR (R= tBu, Ad= adamantyl) led to lutetium methyl primary amide complexes [(Tp(tBu,Me)) LuMe(NHR)], the solid-state structures of which were determined by XRD analyses. The mixed methyl/tetramethylaluminate compounds [(Tpt(tBu,Me))LnMe({mu(2)-Me}AlMe3)] (Ln= Y, Ho) reacted selectively and in high yield with H2NR, according to methane elimination, to afford heterobimetallic complexes: [(Tp(tBu,Me)) Ln({mu(2)-Me}AlMe2)(mu(2)-NR)] (Ln= Y, Ho). X-ray structure analyses revealed that the monomeric alkylaluminum-supported imide complexes were isostructural, featuring bridging methyl and imido ligands. Deeper insight into the fluxio-nal behavior in solution was gained by H-1 and C-13 NMR spectroscopic studies at variable temperatures and H-1-Y-89 HSQC NMR spectroscopy. Treatment of [(Tp(tBu,Me))LnMe(AlMe4)] with H2NtBu gave dimethyl compounds [(Tp(tBu,Me)) LnMe(2)] as minor side products for the mid-sized metals yttrium and holmium and in high yield for the smaller lutetium. Preparative- scale amounts of complexes [(Tp(tBu,Me)) LnMe(2)] (Ln= Y, Ho, Lu) were made accessible through aluminate cleavage of [(Tp(tBu,Me)) LnMe(AlMe4)] with N, N, N', N'-tetramethylethylenediamine (tmeda). The solid-state structures of [(Tp(tBu,Me))HoMe(AlMe4)] and [(Tp(tBu,Me))HoMe2] were analyzed by XRD.
机译：单体[（Tp（tBu，Me））LuMe2]（Tp（tBu，Me）=三（3-Me-5-tBu-吡唑基）硼酸酯）与伯脂肪胺H2NR（R = tBu，Ad =金刚烷基）的反应）生成methyl甲基伯酰胺配合物[（Tp（tBu，Me））LuMe（NHR）]，其固态结构由XRD分析确定。根据甲烷消除，混合的甲基/四甲基铝酸盐化合物[（Tpt（tBu，Me））LnMe（{mu（2）-Me} AlMe3）]（Ln = Y，Ho）与H2NR选择性地高产率反应，生成甲烷提供杂双金属配合物：[（Tp（tBu，Me））Ln（{mu（2）-Me} AlMe2）（mu（2）-NR）]（Ln = Y，Ho）。 X射线结构分析表明，单体烷基铝负载的酰亚胺配合物是同构的，具有桥连的甲基和酰亚胺配体。通过在可变温度下进行H-1和C-13 NMR光谱研究以及H-1-Y-89 HSQC NMR光谱，可以更深入地了解溶液中的通量行为。用H2NtBu处理[（Tp（tBu，Me））LnMe（AlMe4）]得到二甲基化合物[（Tp（tBu，Me））LnMe（2）]，作为中等尺寸金属钇和的次要副产物。较小的yield产量高。通过[[Tp（tBu，Me））LnMe（AlMe4）的铝酸盐裂解可得到制备规模的复合物[（Tp（tBu，Me））LnMe（2）]（Ln = Y，Ho，Lu）。与N，N，N'，N'-四甲基乙二胺（tmeda）。用XRD分析了[（Tp（tBu，Me））HoMe（AlMe4）]和[（Tp（tBu，Me））HoMe2]的固态结构。

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