镧-酒石酸配合物的银辅助水热合成及晶体结构(英文)

Hydrothermal Synthesis and Crystal Structures of Two Lanthanum-Tartrate Complexes Cooperated with Ag(Ⅰ) Complexes

在反应体系中引入不同的银化合物,利用水热合成方法制备了2个镧-酒石酸配合物[La(TTA)(OA)0.5(H2O)]·2H2O(1)和[La2(TTA)3(H2O)4]·H2O(2)。利用元素分析及X-射线单晶结构测定对其进行了表征。结果表明配合物1的晶体属于单斜晶系,P21/c空间群;配合物2的晶体属于三斜晶系,P1空间群。在配合物1中,部分酒石酸被氧化分解成为草酸并作为桥联配体将配合物的层状双(6,3)拓扑结构连接形成三维多孔结构;化合物2和1具有相似的二维结构,其层状结构单元被不同配位模式的酒石酸配体连接成一个具有三维结构的超分子化合物。

By using hydrothermal method, two lanthanum-tartrate complexes, [La（TFA）（OA）0.5（H2O）]·2H2O （1） and [La2（TTA）3（H2O）4]·H2O （2）, were obtained with cooperation of different Ag（I） complexes. The complexes were characterized by elemental analysis and X-ray crystal structure determination. The crystal structures show that the complex 1 crystallizes in monoelinic, space group P21/c with a=0.61071（10） nm, b=0.769 62（12） nm, c=2.2702（3） nrn, β=91.645（2）°, V=1.066 6（3） nm^3, Z=4, Dc=2.385 g·cm^-3, F（000）=732,μ=4.058 cm^-1, the final R=0.048 5, wR =0.103 5. While the complex 2 crystallizes in triclinic, space group P1 with a=0.613 08（11） nm, b=0.745 8（1） nm, c=1.245 7（2） nm, α=74.662（1）°, β=88.835（3）°, 7=89.304（2）°, V=0.549 16（16） nm^3, g=l, Dc=2.456 g·cm^-3, F（000）= 392,μ=3.951 cm^-1, the final R=0.052 0, wR=0.088 7. In complex 1, oxidative cleavage was found and the resulted oxalic acid served as bridging-ligand to link the 2D layers of doubled-（6,3） topology to give a porous 3D framework. The complex 2 has similar 2D network with that in 1, but no cleavage is found. The 2D networks in 2 are further linked into 3D framework by other tartrate ligands with different coordination mode. CCDC： 705232, 1; 705233, 2.