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Synthesis, Structure and Characterization of [Cu(2,2′-bpy)_2][{Cu(2,2′-bpy)_2}_2W_(12)O_(40)(H_2)]·4H_2O

Synthesis, Structure and Characterization of [Cu(2,2′-bpy)_2][{Cu(2,2′-bpy)_2}_2W_(12)O_(40)(H_2)]·4H_2O
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摘要 An organic-inorganic compound [Cu(2,2'-bpy)2][{Cu(2,2'-bpy)2}2W12O40(H2)]·4H2O (Mr = 4048.00) was prepared from the hydrothermal reaction of Na2WO4.2H2O, CuC12·2H20, 2,2'-bipyridine (2,2'-bpy) and H2O at 160 ℃ for 4 days. The compound crystallizes in the monoclinic system, space group P21/n with a = 18.9196(8), b = 20.4212(8), c = 21.8129(9)A, β = 96.992(3)^o, V= 8365.0(6)A3, Dc= 3.214 g/cm^3, Z = 4μ(MoKct) = 17.269mm^-1 and F(000) = 7324. Of the 119837 total reflections, 17315 were unique (Rint = 0.0489). The final R = 0.0385 and wR = 0.0770 for 11142 observed reflections with I 〉 2a(I). Single-crystal X-ray diffraction reveals that the structure is composed of [(Cu(2,2'-bpy)2}2W12040(H2)]^2- anions, discrete [Cu(2,2'-bpy)2]^2+ cations and lattice water molecules, and the anion is made up of a {W12O40(H2)}^6- α-Keggin core decorated with two [Cu(2,2'-bpy)2}^2+ groups through bridging oxygen atoms. An organic-inorganic compound [Cu(2,2'-bpy)2][{Cu(2,2'-bpy)2}2W12O40(H2)]·4H2O (Mr = 4048.00) was prepared from the hydrothermal reaction of Na2WO4.2H2O, CuC12·2H20, 2,2'-bipyridine (2,2'-bpy) and H2O at 160 ℃ for 4 days. The compound crystallizes in the monoclinic system, space group P21/n with a = 18.9196(8), b = 20.4212(8), c = 21.8129(9)A, β = 96.992(3)^o, V= 8365.0(6)A3, Dc= 3.214 g/cm^3, Z = 4μ(MoKct) = 17.269mm^-1 and F(000) = 7324. Of the 119837 total reflections, 17315 were unique (Rint = 0.0489). The final R = 0.0385 and wR = 0.0770 for 11142 observed reflections with I 〉 2a(I). Single-crystal X-ray diffraction reveals that the structure is composed of [(Cu(2,2'-bpy)2}2W12040(H2)]^2- anions, discrete [Cu(2,2'-bpy)2]^2+ cations and lattice water molecules, and the anion is made up of a {W12O40(H2)}^6- α-Keggin core decorated with two [Cu(2,2'-bpy)2}^2+ groups through bridging oxygen atoms.
出处 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 北大核心 2007年第12期1435-1440,共6页 结构化学(英文)
基金 This work was supported by the Natural Science Foundation of Fujian Province (No. E0420001) and NCETFJ.
关键词 POLYOXOTUNGSTATE copper compound hydrothermal synthesis crystal structure polyoxotungstate, copper compound, hydrothermal synthesis, crystal structure
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