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Unexpected results of the reactions of manganese and vanadium β-diketiminate halide complexes with Na[HBEt3]

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Abstract

The reaction of [(MenacnacDipp)Mn(μ-Cl)]2(2) (MenacnacDipp = HC(C(Me)NDipp)2; Dipp = 2,6-Pri2C6H3) with sodium triethylborohydride in a toluene—THF mixture afforded the complex [(MenacnacDipp)Mn(μ-H)2BEt2(THF)] (3). The reaction of 2 with Na[HBEt3] in toluene under THF-free conditions gave a mixture of products. The set and the ratio of these products in the resulting crystalline mixture were established by quantitative powder X-ray diffraction analysis: [(MenacnacDipp)Mn(μ-H)]2(1), [(MenacnacDipp)−Mn(μ-H)2BEt2] (4), and unreacted compound 2 in the ratio of 15:4:1 and traces of an unknown crystalline phase. The reaction of [(MenacnacDipp)VCl2] (5) with Na[HBEt3] yielded the compound [(MenacnacDipp)V(μ-H)(μ,κ1:1−C:C′−C2H4)BEt2] (6) containing the unusual ligand [HBEt2(CH2CH2)]2−. The vanadium analog of compound 3, [(MenacnacDipp)V(μ-H)2BEt2(THF)] (7), was isolated in one experiment. Besides. a small amount of the complex [(MenacnacDipp)V(μ-H)BEt3(THF)] (8) was detected in the mixture of crystalline products. The structures of compounds 3, 4, 6, 7, and 8 were determined by single-crystal X-ray diffraction.

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Funding

This study was financially supported by the Russian Science Foundation (Project No. 19-73-00183) and the Ministry of Science and Higher Education of the Russian Federation (Project Nos 121031700321-3 and 121031700313-8).

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Authors and Affiliations

  1. Nikolaev Institute of Inorganic Chemistry, Siberian Branch of the Russian Academy of Sciences, 3 prosp. Akad. Lavrentieva, 630090, Novosibirsk, Russia

    M. Yu. Afonin, N. V. Stypnik, A. Yu. Konokhova, T. S. Sukhikh & S. N. Konchenko

  2. Novosibirsk State University, 2 ul. Pirogova, 630090, Novosibirsk, Russia

    N. V. Stypnik

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  1. M. Yu. Afonin
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Correspondence to S. N. Konchenko.

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Dedicated to Academician of the Russian Academy of Sciences V. I. Ovcharenko on the occasion of his 70th birthday.

Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 7, pp. 1429–1440, July, 2022.

No human or animal subjects were used in this research.

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Afonin, M.Y., Stypnik, N.V., Konokhova, A.Y. et al. Unexpected results of the reactions of manganese and vanadium β-diketiminate halide complexes with Na[HBEt3]. Russ Chem Bull 71, 1429–1440 (2022). https://doi.org/10.1007/s11172-022-3549-4

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