Abstract
The silver( I) homoleptic complexes [Ag 2(dppy) n ](ClO 4) 2 n = 2 for 1 or 3 for 2) and [Ag(dppy) n ]ClO ( n = 3 for 3 or 4 for 4) [dppy = 2-(diphenylphosphino) pyridine] have been isolated in the solid state and characterised in solution by means of variable-temperature 31P NMR spectroscopy. Both dinuclear species 1 and 2 possess an 8-membered annular core structure with two ligands bridging head-to-tail the metal ions, while in the mononuclear derivatives all dppy ligands act as P-bound monodentate. Treatment of 1 with increasing amounts of dppy revealed (by 31P NMR spectroscopy) that complexes 2, 3 and 4 are formed in a stepwise manner. Surprisingly, no stable single complex is formed when the dppy/Ag(I) ratio is 2. A mixture of complexes 2, 3 and 4, along with unidentified products, is conversely present in solution. The solid state structures of complexes 2 and 4 have been determined by single-crystal X-ray diffraction. In 2 the Ag(I) centres posses different environments, one metal ion being two-coordinated (NP donor set) and the other being three-coordinated (NP 2 donor set). The cations of 4 present the metal bound to four dppy ligands in a slightly distorted tetrahedral environment. Of the two crystallographically independent cations, one showsthe axial Ag-P bond lenght shorter (2.566(8) Å) than the value for the off-axis Ag bonds (2.624(5) Å).
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