New nickel pincer complexes based on pentamethylruthenocene

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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. The purity of the products was confirmed by elemental analysis. The structure of complex Ia was established by single-crystal X-ray diffraction (CCDC № 2408463).

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S. Safronov

Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences

编辑信件的主要联系方式.
Email: sergiosfr.svs@gmail.com
俄罗斯联邦, Moscow

Yu. Nelyubina

Federal Research Center of Problems of Chemical Physics and Medicinal Chemistry, Russian Academy of Sciences

Email: sergiosfr.svs@gmail.com
俄罗斯联邦, Chernogolovka

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2. Fig. 1. General view of complex Ia with atoms represented by thermal vibration ellipsoids (p = 50%). The molecular structure of one of the two crystallographically independent molecules of Ia is shown. Hydrogen atoms are not shown, and numbering is given only for metal ions, heteroatoms, and selected carbon atoms.

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3. Scheme 1. Preparation of diphosphines {1,3-(R2PCH2)2C5H3}Ru(Cp*) (R = tBu, iPr) and pincer nickel complexes Ia, Ib.

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