Cationic bronsted acids for the preparation of Sn-IV salts: Synthesis and characterisation of [Ph3Sn(OEt2)][H2N{B(C6F5)(3)}(2)], [Sn(NMe2)(3)(HNMe2)(2)][B(C6F5)(4)] and [Me3Sn(HNMe2)(2)][B(C6F5)(4)]

Sarazin, Y., Coles, S.J., Hughes, D.L., Hursthouse, M.B. and Bochmann, M. (2006) Cationic bronsted acids for the preparation of Sn-IV salts: Synthesis and characterisation of [Ph3Sn(OEt2)][H2N{B(C6F5)(3)}(2)], [Sn(NMe2)(3)(HNMe2)(2)][B(C6F5)(4)] and [Me3Sn(HNMe2)(2)][B(C6F5)(4)]. European Journal of Inorganic Chemistry, (16), 3211-3220. (doi:10.1002/ejic.200600397).

Abstract

Ph3SnN(SiMe3)(2) (1) was prepared in good yields by reaction of [{NaN(SiMe3)(2)}(2)center dot THF] (2) with Ph3SnF. Treatment of 1 with [H(OEt2)(2)][H2N{B(C6F5)(3)}(2)] (4) in dichloromethane afforded the stannylium cation [Ph3Sn(OEt2)][H2N{B(C6F5)(3)}(2)] (5), which was characterised by H-1, C-13{H-1}, B-11, F-19 and Sn-119 NMR spectroscopy. The reaction of Sn(NMe2)(4) with [Ph2MeNH][B(C6F5)(4)] (3) gave the amidotin(IV) compound [Sn(NMe2)(3)(HNMe2)(2)][B(C6F5)4] (6) which proved very stable towards ligand substitution and resisted treatment with Et2O, THF, TMEDA and pyrazine. Two new Bronsted acid salts [H(NMe2H)(2)][B(C6F5)(4)] (7). and [(C4H4N2)H center dot OEt2]-[H2N{B(C6F5)(3)}(2)] (8) were synthesised. The reaction of 7 with Sn(NMe2)(4) in Et2O allowed the preparation of 6 in a much improved yield (83%). The treatment of 7 with Me-3-SnN(SiMe3)(2) in Et2O yielded [Me3Sn(HNMe2)(2)][B(C6F5)(4)] (9) nearly quantitatively. Compounds 1, 2, 6, 8 and 9 were characterised by single-crystal X-ray diffraction analyses; 6 is the first example of a structurally characterised amidotin(IV) cation.

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Contributors

Author: S.J. Coles

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