| Solvothermal Synthesis and Structure Studies of a Mixed-valence Oxochloromolybdenum Complex |
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| 作者姓名： | 宋立军 曾卉一 蔡丽珍 董振超 郭国聪 黄锦顺 |
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| 作者单位： | State Key Laboratory of Structural Chemistry，Fujian Institute of Research on the Structure of Matter，The Chinese Academy of Sciences，Fuzhou，Fujian 350002，China |
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| 基金项目： | the Innovative Project (No. IP01007)，the Introduction of Overseas Elitists Program (No. IB990168)，the Chinese Academy of Sciences |
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| 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/cm^3,μ= 1.514 mm^-1, F(000) = 4304, R = 0.0654 and wR = 0.1544 for 1944 observed reflections with 1 ≥/ 2σ(I). The compound consists of two different neutral molecules, Mo^IV-(OH)2(2,2′-bipy)Cl2 and MoVO(2,2′-bipy)Cl3. Both Mo^IV and Mo^V 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 O^2- 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.
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| 关 键 词： | 固态反应 溶剂热合成 单晶结构 氧代氯化钼 配合物 X射线分析 |
Solvothermal Synthesis and Structure Studies of a Mixed-valence Oxochloromolybdenum Complex |
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| SONGLi-Jun ZENGHui-Yi CAILi-Zhen DONGZhen-Chao GUOGuo-Cong HUANGJin-Shun.Solvothermal Synthesis and Structure Studies of a Mixed-valence Oxochloromolybdenum Complex[J].Chinese Journal of Structural Chemistry,2003,22(4):395-398. |
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| Authors: | SONGLi-Jun ZENGHui-Yi CAILi-Zhen DONGZhen-Chao GUOGuo-Cong HUANGJin-Shun |
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| Institution: | State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences, Fuzhou, Fujian 350002, China |
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| Abstract: | 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. |
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| Keywords: | oxochloromolybdenum solvothermal synthesis structure |
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