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作 者:LIU Hong-Sheng CHEN Yan-Hui PENG Jun SHI Zhen-Yu DONG Bao-Xia KONG Yu-Mei
机构地区:[1]Institute of Polyoxometalate Chemistry, Department of Chemistry, Northeast Normal University, Changchun, Jilin 130024, China [2]Department of Chemzstry, Suihua University, Suihua, Heilongjiang 152061, China
出 处:《Chinese Journal of Structural Chemistry》2006年第7期830-836,共7页结构化学(英文)
基 金:This work was supported by the National Natural Science Foundation of China (No. 20271011)
摘 要:A new compound [Cu(I)(phen)2]5[HV15O36(Cl)]0.65[H3V16O38(Cl)]0.35·2H2O 1 (phen = 1,10′-phenanthroline) has been prepared from the hydrothermal reaction of V2O5, CuCl, phen, H2C2O4·2H2O, THMAM (tris(hydroxymethyl)aminomethane) and H2O in the molar ratio of 3:1:1:0.5:2.5:1400. Compound 1 crystallizes in the space group P42212 of the tetragonal system with a = b = 21.5009(8), c = 28.401(2) A, V= 13129.5(12) A^3 Z = 4, Dc = 1.800 g/cm^3, μ(MoKa) = 1.932 mm^-1, λ(MoKa) = 0.71073 A, F(000) = 7063.4, C120H81.20ClCu5N20O38.7V15.35, Mr = 3557.58, the final R = 0.0594 and wR= 0.1320 for 7761 observed reflections (I 〉 2σ(I)). Structure analysis shows that 1 exhibits a 3D channel framework formed by the supramolecular assembly of Cu complexes and polyoxovanadate clusters via intermolecular hydrogen bonding, and the channels contain Cu complexes. Other characterizations by elemental analysis, XPS, IR, XRD and thermal analysis are also described.A new compound [Cu(I)(phen)2]5[HV15O36(Cl)]0.65[H3V16O38(Cl)]0.35·2H2O 1 (phen = 1,10′-phenanthroline) has been prepared from the hydrothermal reaction of V2O5, CuCl, phen, H2C2O4·2H2O, THMAM (tris(hydroxymethyl)aminomethane) and H2O in the molar ratio of 3:1:1:0.5:2.5:1400. Compound 1 crystallizes in the space group P42212 of the tetragonal system with a = b = 21.5009(8), c = 28.401(2) A, V= 13129.5(12) A^3 Z = 4, Dc = 1.800 g/cm^3, μ(MoKa) = 1.932 mm^-1, λ(MoKa) = 0.71073 A, F(000) = 7063.4, C120H81.20ClCu5N20O38.7V15.35, Mr = 3557.58, the final R = 0.0594 and wR= 0.1320 for 7761 observed reflections (I 〉 2σ(I)). Structure analysis shows that 1 exhibits a 3D channel framework formed by the supramolecular assembly of Cu complexes and polyoxovanadate clusters via intermolecular hydrogen bonding, and the channels contain Cu complexes. Other characterizations by elemental analysis, XPS, IR, XRD and thermal analysis are also described.
关 键 词:hydrothermal synthesis crystal structure POLYOXOVANADATE supramolecular assembly
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