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Hydrothermal Synthesis and Characterization of a Sandwich-type Tungstophosphate, (1,3-H_2dap)_8H_4[Co_4(H_2O)_2(α-B-PW_9O_(34))_2]_2·5H_2O

Hydrothermal Synthesis and Characterization of a Sandwich-type Tungstophosphate, (1,3-H_2dap)_8H_4[Co_4(H_2O)_2(α-B-PW_9O_(34))_2]_2·5H_2O
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摘要 A sandwich-type tungstophosphate, (1,3-H2dap)8-14[Co4(H2O)2(α-B-PWgO34)2]2·5H20 (1,3-dap = 1,3-diaminopropane), was hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, IR and UV spectroscopy. The title compound crystallizes in triclinic, space group P1 with a = 13.691(3), b = 17.744(4), c = 20.620(5) A, a =113.466(5), β = 91.184(5), Y = 104.223(5)°, V = 4414.3(17)A^3, C24H96Co8N16O145P4W36, Mr = 10143.09, Dc = 3.816 g/cm^3,μ(MoKa) = 24.210 mm^-1, F(000) = 4452, Z = 1, the final R = 0.0694 and wR = 0.1519 for 9910 observed reflections (I 〉 2σ(I)). The compound consists of two sets of tetra-transition metal-substituted sandwich frameworks, [Co4(H2O)2(α-B-PW9O34)2]^10- having an inversion centre. Two lacunary α-B-[PW9O34]^9- Keggin units are linked by a rhomb-like Co4O14(H2O)2 cluster, in which the Co^2+ ions are coordinated by one water molecule. Isolatedly protonated 1,3-H2dap^2+ units act as counter-ions to interact with the [Co4(H2O)2(α-B-PWgO34)2]^10- heteropolyanions via hydrogen bonds, resulting in a three-dimensional framework. A sandwich-type tungstophosphate, (1,3-H2dap)8-14[Co4(H2O)2(α-B-PWgO34)2]2·5H20 (1,3-dap = 1,3-diaminopropane), was hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, IR and UV spectroscopy. The title compound crystallizes in triclinic, space group P1 with a = 13.691(3), b = 17.744(4), c = 20.620(5) A, a =113.466(5), β = 91.184(5), Y = 104.223(5)°, V = 4414.3(17)A^3, C24H96Co8N16O145P4W36, Mr = 10143.09, Dc = 3.816 g/cm^3,μ(MoKa) = 24.210 mm^-1, F(000) = 4452, Z = 1, the final R = 0.0694 and wR = 0.1519 for 9910 observed reflections (I 〉 2σ(I)). The compound consists of two sets of tetra-transition metal-substituted sandwich frameworks, [Co4(H2O)2(α-B-PW9O34)2]^10- having an inversion centre. Two lacunary α-B-[PW9O34]^9- Keggin units are linked by a rhomb-like Co4O14(H2O)2 cluster, in which the Co^2+ ions are coordinated by one water molecule. Isolatedly protonated 1,3-H2dap^2+ units act as counter-ions to interact with the [Co4(H2O)2(α-B-PWgO34)2]^10- heteropolyanions via hydrogen bonds, resulting in a three-dimensional framework.
出处 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 2013年第2期311-315,共5页 结构化学(英文)
基金 Supported by the Natural Science Foundation of Henan Province (No. 102300410021)
关键词 POLYOXOMETALATE SANDWICH TUNGSTOPHOSPHATE cobalt KEGGIN polyoxometalate, sandwich, tungstophosphate, cobalt, keggin
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