三维孔道结构钒磷酸盐[H_3N(CH_2)_3NH_3]_2[H_3N(CH_2)_3NH_2][H_2N(CH_2)_3NH_2]-[V(H_2O)_2(VO)_8(OH)_4(PO_4)_4(HPO_4)_4]·4H_2O的水热合成和结构表征(英文)

Hydrothermal Synthesis and Structural Characterization of a Three-dimensional Open-framework Vanadium Phosphate DAP-V_9P_8

以1,3-丙二胺为模板,水热合成了三维孔道结构钒磷酸盐[H3N (CH2)3NH3]2[H3N(CH2)3NH2〗[H2N(CH2)3NH2V(H2O)2(VO)8(OH)4(PO4)4(HPO4)4].4H2O (DAP-V9P8)。用单晶X射线衍射、红外光谱和热重法对该化合物的晶体结构进行了表征。DAP-V9P8的无机骨架由[VO5]、[VO6]、[PO4]和[HPO4]通过共顶点连接而成。孔道中充填的丙二胺分子随所处结晶学位置不同,有三种完全不同的分子构象。其中,位于∥b轴直径达1.82nm椭圆形孔道中心的丙二胺分子碳链呈独特的直线状分布。晶体学参数:a=1.4820(9)nm,b=1.0255(4)nm,c=1.8181(9)nm ,β=90.391(8)°;P21/n(No.14);R1 =0.0772,wR2 =0.2004(I>(2σI))。与等结构的其它化合物进行了系统的结构比较。

A new three dimensional open-framework vanadium phosphate, [H3N （CH2）3NH3]2[H3N（CH2）3NH2][H2N（CH2）3NH2][V（H2O）2（VO）8（OH）4（PO4）4（HPO4）4]·4H2O （DAP-V9P8）, has been hydrothermaly synthesized using 1,3-diaminopropane （1,3-DAP） as structure-directing molecule and characterized by single crystal X-ray diffraction, infrared spectrum and thermogravimetric analysis. The compound exhibits a complicated framework structure consisted of corner-linked [VO5], [VO6], [PO4] and [HPO4] polyhedrons. There are interconnected channel system including a very large channel of 1.82nm of diameter in the structure. The 1,3-DAP molecules located inside the channels have three different conformations based on their crystallographic positions. It is noteworthy that the carbon chain of 1,3-DAP molecules in the center of the elliptical cavity is a linear type. Crystal data：a=1.4820（9）nm,b=1.0255 （4）nm,c=1.8181（9）nm,β=90.391（8）°,P21/n （No.14）,R1=0.0772,wR2=0.2004 （I〉（2σI））. Systematic structural comparison of DAP-V9P8 with isoframework compounds also been made.