Complexes of rhodium(I) with 1,8-naphthyridine and related ligands. Crystal structure of [Rh2(µ-napy)2(nbd)2][ClO4]2·H2O

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Abstract
Reactions of stoicheiometric amounts of 1,8-naphthyridine (R-napy) type ligands with [{RhCl(diolefin)}2] or [Rh(diolefin)(OCMe2)x][ClO4] lead to formation of the complexes [RhCl(diolefin)(napy)], [Rh(diolefin)(2,7Me2-napy)][ClO4][diolefin = cyclo-octa-1,5-diene (cod), norborna-2,5-diene (nbd), tetrafluorobenzobarrelene (tfbb), trimethyltetrafluorobenzobarrelene (Me3tfbb)], [Rh2(µ-R-napy)2(diolefin)2][ClO4]2·H2O (R = H or 2-Me; diolefin = nbd or tfbb), or [Rh(cod)(2Me-napy)][ClO4]. Mononuclear complexes of the type [Rh(diolefin)(R-napy)2][ClO4] are obtained in the presence of an excess of the R-napy ligand. Several tetracarbonyl or dicarbonyl derivatives of formulae [Rh(napy)2(CO)2][ClO4], [Rh2(µ-R-napy)2(CO)4][ClO4]2, [Rh2(µ-R-napy)2(CO)2(PPh3)2][ClO4]2, and [(diolefin)Rh(µ-napy)2Rh(CO)(PPh3)][ClO4]2 have been prepared from [Rh(CO)(PPh3)(OCMe2)x][ClO4] or by carbonylation reactions. The structure of [Rh2(napy)2(nbd)2][ClO4]2·H2O has been determined by X-ray diffraction methods. Crystals are orthorhombic, space group Pccn with Z= 4 in a unit cell of dimensions a= 17.539(11), b= 10.252(7), and c= 17.211(12)Å. The structure was solved by Patterson and Fourier methods and refined by full-matrix least squares to R= 0.063 for 1 427 independent observed reflections. The cationic complex [Rh2(napy)2(nbd)2]2+, having an imposed symmetry C2, is binuclear with two napy ligands bridging the two metals. The co-ordination around each Rh atom is completed by a nbd molecule interacting through the two olefin bonds. The distance between the bridged Rh atoms is 2. 916(3)Å.

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