The synthesis and structural characterisation of Ru-Sn based derivatives bearing asymmetric X2ClSn- (X = Br and F) anions

摘要

Four remarkable ruthenium-tin based derivatives [Ru(eta(5)-Cp)(PPh3)(2)SnF2Cl] (1), [Ru(eta(5)-Cp)(PPh3)(2)SnBr2Cl] (2), [Ru(eta(5)- Cp)(dppe)SnF2Cl] (3) and [Ru(eta5-Cp)(dppe)SnBr2Cl] (4), CP = C5H5, were obtained by reacting [Ru(eta(5)-Cp)(PPh3)(2)Cl] or [Ru(eta5-Cp)(dppe)Cl] with SnX2 {X = F or Br}, respectively. They were studied by i.r. NMR (H-1, C-13, P-31 and Sn-119) and Sn-119-Mossbauer spectroscopies. Additionally, (1) and (4) were structurally authenticated by X-ray crystallography and the results were as follows: (1) orthorhombic, Pbca, V = 15181.7(12) Angstrom(3) and Z = 8; (4) monoclinic, P2(1)ln, V = 3503.74(8) Angstrom(3) and Z = 4. All compounds exist as formulated only in the solid sate, in solution they re-distribute in a mixture of species such as [Ru(eta(5)-Cp)(PPh3)(2)SnFnCl3-n] and [Ru(eta(5)-Cp)(dppe)SnBrnCl3-n] {n= 0, 1, 2, and 3 1, as revealed by variable temperature 119Sn NMR experiments. (C) 2003 Elsevier B.V. All rights reserved. [References: 15]