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

作　　者：宋立军 曾卉一 蔡丽珍 董振超 郭国聪 黄锦顺 

机构地区：[1]State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences, Fuzhou, Fujian 350002, China

出　　处：《Chinese Journal of Structural Chemistry》2003年第4期395-398,共4页结构化学（英文）

基　　金：the Innovative Project (No. IP01007);the Introduction of Overseas Elitists Program (No. IB990168);the Chinese Academy of Sciences

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 MoS 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) , Mr = 1103.97, V = 7941(1) 3, Z = 8, Dc = 1.843 g/cm3, = 1.514 mm-1, F(000) = 4304, R = 0.0654 and wR = 0.1544 for 1944 observed reflections with I ≥ 2(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.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 MoS 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) , Mr = 1103.97, V = 7941(1) 3, Z = 8, Dc = 1.843 g/cm3, = 1.514 mm-1, F(000) = 4304, R = 0.0654 and wR = 0.1544 for 1944 observed reflections with I ≥ 2(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.

关 键 词：oxochloromolybdenum solvothermal synthesis STRUCTURE 

分 类 号：O614.612[理学—无机化学] O641.4[理学—化学]