Solvothermal Synthesis and Structure Studies of a Mixed-valence Oxochloromolybdenum Complex

摘要

Emerald green crystals of a new mixed-valence oxochloromolybdenum complex, Mo(OH)2(2,2'-bipy)Cl2([MoO(2,2'-bipy)Cl3]2, were obtained in an attempt to synthesize the Mo-S cluster compounds under solvothermal conditions. The title compound was characterized by EPR and X-ray single-crystal diffraction techniques. Crystallographic data: orthorhombic, space group Fdd2, a = 12.684(1), b = 21.518(2), c = 29.096(3)(A。), Mr = 1103.97, V = 7941(1) (A。)3, Z = 8, Dc = 1.843 g/cm3, μ = 1.514 mm－1, F(000) = 4304, R = 0.0654 and wR = 0.1544 for 1944 observed reflections with I ≥ 2σ(I). The compound consists of two different neutral molecules, MoⅣ- (OH)2(2,2'-bipy)Cl2 and MoⅤO(2,2'-bipy)Cl3. Both MoⅣ and MoⅤ ions are in a distorted octahedral environment. The Mo(1)Ⅳ atom is surrounded by two Cl－ ions and two O atoms from OH－ and two N atoms from a 2,2'-bipy ligand. The Mo(2) atom is surrounded by three Cl－ ions, one O2－ anion and two N atoms from another 2,2'-bipy ligand. The bipyridine occupies two cis-equatorial sites, while the Cl－ ions are located at the axial and equatorial positions.