三维孔道结构钒磷酸盐[H3N(CH2)3NH3]2[H3N(CH2)3NH2][H2N(CH2)3NH2]-[V(H2O)2(VO)8(OH)4(PO4)4(HPO4)4]·4H2O的水热合成和结构表征

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)3NH2][V(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.

Hydrothermal Synthesis and Structural Characterization of a Three-dimensional Open-framework Vanadium Phosphate DAP-V9P8

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.