Synthesis and structural characterization of osmium cluster complexes containing 2-phenylazopyridine. Crystal structures of [Os3(CO)10(NC5H4-N=N-C6H5)] and [Os3(CO)10(μ-H)(NC5H3-N=N(O)-C6H5)]

Article abstract of DOI:10.1016/0020-1693(95)04705-E

The reaction of [Os3(CO)10(MeCN)2] with 2-phenyl azopyridine (2-PAP) affords [Os3(CO)10(NC5H4-N=N-C6H5)] (1), [OS3(CO)10(μ-H)(NC5H3-N=N(O)-C6H5)] (2) and a violet product 3, which is an isomer of I. In 1, the 2-PAP moiety acts as the rarely observed six-electron donor. Cluster 2 contains an 'oxidized' 2-PAP moiety bonding in the usual ortho-metallated mode of pyridine. Both clusters 1 and 2 have been fully characterized in solution by conventional spectroscopic methods and in the solid state by single crystal X-ray diffraction analysis. Crystals of 1 are orthorhombic, space group P2(1)2(1)2(1), Z = 4, with unit cell dimensions a = 9.123(1), b = 17.217(2), c = 16.168(2)? Crystals of 2 are triclinic, spacegroup P1-, Z = 2, with unit cell dimensions a = 9.308(2), b = 11.250(2) , c = 12.934(2)?, α = 77.23(1), β = 72.26(1), γ = 85.21(1)°.