具有十二元环开放结构磷酸锌的非水合成与表征

Nonaqueous Synthesis and Characterization of a Zincophosphate with 12-Membered Ring Channel Open Framework

从非水体系中制备了 Zn2 ( HPO4) 3· H3NCH2 CH2 NH3单晶 ,用 X射线测定了晶体结构 ,用红外光谱 ,DTA-TG等方法对化合物进行了表征 .晶体属三斜晶系 ,P1空间群 .晶胞参数 a=0 .82 1 5( 3 ) nm,b=0 .8557( 3 ) nm,c=0 .9760 ( 3 ) nm,α=93 .8( 3 )°,β=95.3 8( 3 )°,γ=1 0 9.75( 3 )°,V=0 .63 94 nm3,Z=2 ,Dc=2 .50 g·cm- 3.结构中的锌和磷均与氧形成四面体配位 ,Zn O4和 HPO4四面体严格交替排列 ,骨架中的氧分为二桥氧和端氧 ,端氧只向 P原子配位 .三维开放式骨架结构中沿 a轴和 b轴方向有十二元环直孔道 ,质子化的有机胺在

Single crystal of Zn 2(HPO 4) 3·H 3NCH 2CH 2NH 3 was synthesized from nonaqueous system and its crystal structure was determined using single crystal X ray diffraction. The crystal structure was solved by direct method and refined by full matrix least square method and the crystal is triclinic, space group P 1 with a =0.821 5(3) nm, b =0.855 7(3) nm, c =0.976 0(3) nm, α =93.8(3)°, β =95.38(3)°, γ =109.75(3)°, V =0.639 4 nm 3, Z =2, D c=2.50 g·cm -3 , μ =43.0 cm -1 , R =0.031, R w=0.040. The framework is built up from ZnO 4 and HPO 4 tetrahedra, forming a three dimensional network, and the linkage of Zn and P tetrahedra displays a strict alternation of zinc and phosphorus. The open framework contains 8 membered ring channels and 12 membered ring channels. The results of XRD, IR and DTA TG for the compound are given.