TY - JOUR
T1 - Cationic Brønsted acids for the preparation of SnIV 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]
AU - Sarazin, Yann
AU - Coles, Simon J.
AU - Hughes, David L.
AU - Hursthouse, Michael B.
AU - Bochmann, Manfred
PY - 2006/6/28
Y1 - 2006/6/28
N2 - Ph3SnN(SiMe3)2 (1) was prepared in good yields by reaction of [{NaN(SiMe3)2}2·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 1H, 13C{1H}, 11B, 19F and 119Sn 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 Brønsted acid salts [H(NMe2H)2][B(C6F5)4] (7) and [(C4H4N2)H·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 Me3SnN(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.(© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2006)
AB - Ph3SnN(SiMe3)2 (1) was prepared in good yields by reaction of [{NaN(SiMe3)2}2·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 1H, 13C{1H}, 11B, 19F and 119Sn 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 Brønsted acid salts [H(NMe2H)2][B(C6F5)4] (7) and [(C4H4N2)H·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 Me3SnN(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.(© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2006)
U2 - 10.1002/ejic.200600397
DO - 10.1002/ejic.200600397
M3 - Article
VL - 2006
SP - 3211
EP - 3220
JO - European Journal of Inorganic Chemistry
JF - European Journal of Inorganic Chemistry
SN - 1434-1948
IS - 16
ER -