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  

作　　者：王子梁 魏林恒 李明雪 

机构地区：[1]College of Chemistry and Chemical Engineering, Henan University [2]College of Environment and Planning, Henan University

出　　处：《Chinese Journal of Structural Chemistry》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)

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.

关 键 词：POLYOXOMETALATE SANDWICH TUNGSTOPHOSPHATE cobalt KEGGIN 

分 类 号：O621.3[理学—有机化学]