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Synthesis and properties of pentamethylmetallocene derivatives Cp*MCp (M = Ru, Fe). Crystal structure of the salt [CpRuC5Me4CH2 +OC6H2(NO2)3 -]

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Abstract

Photolysis of a solution of Cp*RuCp (1) in CF3CO2H generates salt [CpRu(C5Me4CH2)]-(O2CCF3)(2 • O2CCF3). The reaction of compound 1 with oleum at 20 °C through the intermediate dication [η5-(CH2C5Me4)Ru(μ:η55-C5H4C5H5)Ru(C5Me4CH2)-η6]2+ leads to the triply charged cation η7CH2)2C5Me3Ru(μη55-C5H4C5H4)Ru(C5Me4CH2)-η6]3+. Synthesis of pentamethylmetallocene derivatives CpMC5Me4X (M = Ru, Fe; X = CHO, CH2OH, CH2An) has been accomplished. The reactions of 1-hydroxymethyl-2,3,4,5-tetramethylruthenocene with acids CF3CO2H, HBF4, CF3CO2H/NaB[C6H3(CF3)2]4, and picric acid C6H2(NO2)3OH afforded salts 2•X (X = CF3CO2, BF4, B[C6H3(CF3)2]4), and (2,3,4,5-tetram ethylruthenocenyl)methyl picrate [CpRu(C5Me4CH2)-η6][(C6H2(NO2)3O] (2•C6H2(NO2)3O). Structure of the latter was characterized by single crystal X-ray diffraction.

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Correspondence to A. Z. Kreindlin.

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Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 4, pp. 794-799, April, 2009.

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Kreindlin, A.Z., Petrovskii, P.V., Suponitsky, K.Y. et al. Synthesis and properties of pentamethylmetallocene derivatives Cp*MCp (M = Ru, Fe). Crystal structure of the salt [CpRuC5Me4CH2 +OC6H2(NO2)3 -]. Russ Chem Bull 58, 810–816 (2009). https://doi.org/10.1007/s11172-009-0099-y

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  • DOI: https://doi.org/10.1007/s11172-009-0099-y

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