The synthesis and characterisation of complexes of tin and antimony

Abstract

The complexes of 80X4 (X = CI, Br) with macrocyclic thio- and selenoether ligands ([12]aneS4, [14]aneS4, [16]aneS6, [SjaneSez and [16]aneSe4) have been synthesised and characterised by multinuclear ''^Sn and ^^Se) spectroscopy, IR spectroscopy and elemental analysis. Snl4 adducts were also studied. Single crystal X-ray diffraction has been employed to structurally characterise [SnBr4([12]aneS4)], [SnBr4([14]aneS4)] and [SnBr4([16]aneS4)], and each reveals a polymeric chain structure. There is a considerable structural dependence on the macrocyclic ring size, as the ring size of the macrocycle is increased the coordination environment at tin(IV) changes, [SnBr4([12]aneS4)] adopts a cz^-octahedral geometry at Sn(IV), octahedral geometry at Sn(IV). [SnBr4([14aneS4)].2/3CH2Cl2 and [SnBr4([16]aneS4)] show a trans- NMR ('H, The complex [SbCl3([8]aneSe2)] has been synthesised and structurally characterised using single crystal X-ray diffraction, the structure reveals [SbiC^q'- [8]aneSe2)2] dimers, the dimers are linked together to form an infinite ladder structure. This is the first example involving a trans deposition of the Se atom on the Sb(III) acceptor. A range of complexes of the form [SbClsCL)] where L = OPMe;, OPPhs, OPMePhz, OAsPh], Ph2P(0)CH2P(0)Ph2 and Ph2As(0)CH2As(0)Ph2 have characterised by multinuclear NMR (^H, ^'P and ^^Se) spectroscopy, IR spectroscopy and elemental analysis. L - been prepared and and [(SbCls);^ where and SePPh] SPPh] A study on the promotion of oxidation of a variety of arylphosphines including PhsP, o-C6H4(PPh2)2 and Ph2P(CH2)2PPh2 to the corresponding phosphine oxides on reaction with dry air or dioxygen in the presence of catalytic amounts of Snl4 has been undertaken. The phosphine oxides have been characterised by ^^P{^H} NMR spectroscopy and IR spectroscopy. The reaction with PhsP was conducted using ^^0% and the product was shown to be exclusively PhsP^^O by both IR spectroscopy and EI mass spectrometry, establishing air/dioxygen as the source of the oxygen in the phosphine oxides.

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