Synthesis and Structural Characterization of a Lithium Alkynyl(hydrazinediido)zirconate and its Protonolysis to an Alkynylhydrazido(1-)zirconium Complex

Gehrmann Thorsten; Wadepohl Hubert; Gade Lutz H.

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Synthesis and Structural Characterization of a Lithium Alkynyl(hydrazinediido)zirconate and its Protonolysis to an Alkynylhydrazido(1-)zirconium Complex

机译：炔基（肼二基）锆酸锂的合成，结构表征及其质子水解成炔基（1-）锆配合物的质子分解

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Reaction of the hydrazinediido complex 1 with lithiated phenylacetylene selectively gave the lithium alkynyl(hydrazinediido)zirconate [((N2Npy)-N-TBS)Zr{mu-NNPh2-1 kappa N:2 kappa N}{mu-PhCC-1 kappa C:2 kappa C}Li(py)] (2), which reacted with one molar equivalent of TMEDA to give the corresponding Li-TMEDA derivative [((N2Npy)-N-TBS)Zr{mu-NNPh2-1.N:2 kappa N}{mu-PhCC-1.C:2 kappa C}-Li(TMEDA)] (3). The details of the molecular structure of complex 3 were established by single-crystal X-ray structure analysis. The lithium hydrazinediidozirconate 2 was treated with triethylammonium hydrochloride yielding the corresponding alkinylzirconium hydrazido(1-) complex 4 as a mixture of two diastereomers.

机译：肼二基配合物1与锂化的苯乙炔的反应选择性地得到炔基（肼二基）锆酸锂[[（（N2Npy）-N-TBS）Zr {mu-NNPh2-1 kappa N：2 kappa N} {mu-PhCC-1 kappa C ：2 kappa C} Li（py）]（2），与一摩尔当量的TMEDA反应，得到相应的Li-TMEDA衍生物[（（N2Npy）-N-TBS）Zr {mu-NNPh2-1.N： 2 k N} {mu-PhCC-1.C：2 k C} -Li（TMEDA）]（3）。通过单晶X射线结构分析来确定配合物3的分子结构的细节。用盐酸三乙铵处理肼二咪唑酸锂2，得到相应的炔基锆肼基（1-）配合物4，为两种非对映异构体的混合物。

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《Zeitschrift fur Anorganische und Allgemeine Chemie》 |2015年第1期|共5页
作者
Gehrmann Thorsten; Wadepohl Hubert; Gade Lutz H.;
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正文语种 eng
中图分类化学;
关键词
Hydrazides; Zirconium; Lithium; Crystal structure;

机译：酰肼;锆;锂;晶体结构;

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1. Synthesis and Structural Characterization of a Lithium Alkynyl(hydrazinediido)zirconate and its Protonolysis to an Alkynylhydrazido(1-)zirconium Complex [J] . Gehrmann Thorsten, Wadepohl Hubert, Gade Lutz H. Zeitschrift fur Anorganische und Allgemeine Chemie . 2015,第1期

机译：炔基（肼二基）锆酸锂的合成，结构表征及其质子水解成炔基（1-）锆配合物的质子分解
2. Zirconium hydrazinediido complexes derived from cyclic hydrazines and their role in the catalytic synthesis of 1,7-annulated indoles [J] . Scholl S.A., Wadepohl H., Gade L.H. Organometallics . 2013,第3期

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7. Fulvalene titanium and zirconium complexes: synthesis and NMR study of phosphanido-, alkyl-, and alkynyl-derivatives. X-ray crystal structures of { Ti(η5-C5 H 5)(μ-PPh2)}2{μ-(η5-C5H4-η5-C5H4)} and {Zr(η5-C5H5)(μ-C=CSiMe3)}2{μ-( η5-C5H4-η5-C5H4)} [O] . Cano Sierra Ana María, Cuenca Agreda Tomás, Galakhov Mikhail V., 1995

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Synthesis and Structural Characterization of a Lithium Alkynyl(hydrazinediido)zirconate and its Protonolysis to an Alkynylhydrazido(1-)zirconium Complex

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