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Lutetium complexes with tetraphenylethylene dianion. Synthesis and structure

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Abstract

The reactions of dipotassium and disodium salts of the tetraphenylethylene dianion with LuCl3(THF)3 or CpLuCl2(THF)3 yielded the homoleptic ate-complexes [Na(THF)5][Lu(Ph2CCPh2)2] (1) and [K(THF)5][Lu(Ph2CCPh2)2] (2) or the heteroleptic complex CpLu(Ph2CCPh2)(THF)2 (4), respectively. Recrystallization of complex 1 from a diglyme—THF mixture afforded [Na(diglyme)2][Lu(Ph2CCPh2)2](THF)0,5 (3). Recrystallization of complex 4 from 1,2-dimethoxyethane gave [CpLu(Ph2CCPh2)(DME)](DME) (5). The structures of complexes 3 and 5 were established by X-ray diffraction analysis. In both complexes, the unusual η6-coordination of the (Ph2CCPh2)2− dianion to lutetium is observed. The Lu-C distances vary from 2.441(2) to 2.643(2) Å (3) and from 2.470(3) to 2.763(3) Å (5). In complexes 3 and 5, a redistribution of the C-C bond lengths was observed in the Ph groups coordinated to lutetium. Studies by 1H, 13C, and 2D NMR spectroscopy demonstrated that the η6-coordination of the tetraphenylethylene dianion in homoleptic ate-complexes 1 and 2 is retained in a THF solution, whereas the coordination of this dianion in heteroleptic complex 4 changes from η6 to η4.

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Authors and Affiliations

  1. L. Ya. Karpov Institute of Physical Chemistry, 10 ul. Vorontsovo Pole, 105064, Moscow, Russian Federation

    D. M. Roitershtein & M. E. Minyaev

  2. A. N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, 28 ul. Vavilova, 119991, Moscow, Russian Federation

    K. A. Lyssenko & M. Yu. Antipin

  3. N. D. Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences, 47 Leninsky prosp., 119991, Moscow, Russian Federation

    P. A. Belyakov

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  1. D. M. Roitershtein
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Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 2060–2068, October, 2004.

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Roitershtein, D.M., Minyaev, M.E., Lyssenko, K.A. et al. Lutetium complexes with tetraphenylethylene dianion. Synthesis and structure. Russ Chem Bull 53, 2152–2161 (2004). https://doi.org/10.1007/s11172-005-0089-7

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