New Nickel Pincer Complexes Based on Pentamethylruthenocene

IF 1.1 3区化学 Q4 CHEMISTRY, INORGANIC & NUCLEAR

Russian Journal of Coordination Chemistry Pub Date : 2025-05-26 DOI:10.1134/S1070328424601559

S. V. Safronov, Yu. V. Nelyubina

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Abstract

New nickel(II) pincer complexes based on the pentamethylruthenocene, NiCl[{2,5-(R₂PCH₂)₂C₅H₂}Ru(Cp*)] (Cp* = C₅Me₅, Ia: R = ^tBu; Ib: R = ⁱPr), were synthesized via a two-step route starting from the 1,3-functionally substituted diol {1,3-(HOCH₂)C₅H₃}Ru(Cp*). In the first step, diol was reacted with dialkylphosphines (^tBu₂PH, ⁱPr₂PH) in acetic acid to give diphosphines{1,3-(R₂PCH₂)₂C₅H₃}Ru(Cp*) (R = ^tBu; ⁱPr), which were not isolated in a pure state, but after the removal AcOH, was immediately subjected to cyclometallation with nickel(II) chloride hexahydrate in the presence of pyridine. After all purification procedures, the yields of products Ia and Ib were 31 and 16%, respectively. The complexes were fully characterized by ¹H, ³¹P{¹H}, and ¹³C{¹H} NMR spectroscopy data. The purity of the products was confirmed by elemental analysis. The structure of complex Ia was established by single crystal X-ray diffraction (CCDC no. 2408463).

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新型五甲基鲁二茂镍螯合物

新型五甲基钌烯二世镍螯合物NiCl[{2,5-(R2PCH2)2C5H2}Ru(Cp*)] (Cp* = C5Me5, Ia: R = tBu；Ib: R = iPr)，以1,3-功能取代二醇{1,3-(HOCH2)C5H3}Ru（Cp*）为起始，采用两步法合成。第一步，二醇与二烷基膦（tBu2PH, iPr2PH）在乙酸中反应得到二膦{1,3-(R2PCH2)2C5H3}Ru(Cp*) (R = tBu；在去除AcOH后，在吡啶存在下，立即与六水氯化镍（II）进行环金属化反应。经过所有纯化程序，产物Ia和Ib的收率分别为31%和16%。通过1H、31P{1H}和13C{1H} NMR数据对配合物进行了全面表征。通过元素分析证实了产品的纯度。通过单晶x射线衍射（CCDC no. 1）确定了配合物Ia的结构。2408463)。

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来源期刊

Russian Journal of Coordination Chemistry 化学-无机化学与核化学

CiteScore

2.40

自引率

15.80%

发文量

审稿时长

7.2 months

期刊介绍： Russian Journal of Coordination Chemistry is a journal that publishes reviews, original papers, and short communications on all aspects of theoretical and experimental coordination chemistry. Modern coordination chemistry is an interdisciplinary science that makes a bridge between inorganic, organic, physical, analytical, and biological chemistry.