稀土配合物La_2(m-MOBA)_6(Phen)_2的合成和晶体结构表征

Synthesis and Structural Characterization of Rare-earth Complex[La_2(m-MOBA)_6(Phen)_2]

本文介绍了标题化合物La2(m-MOBA)6(Phen)2(m-MOBA:间甲氧基苯甲酸;Phen:邻菲啉)(1)的合成和晶体结构.化合物1中两个La3+分别与来自配体m-MOBA羧基的7个0及1个邻菲啉的2个N配位构成9配位的畸变三帽三棱柱几何构型的LaO77N2中心.羧酸氧原子以螯合、桥联、螯合桥联三种形式与La3+配位,邻菲啉的氮原子与La3+螯合配位.配合物分子之间存在着π-π堆积、C—H…O氢键、C—H…π氢键和C—H…H—C二氢键分子间弱作用力。化合物晶体属于三斜晶系,空间群为P-1,晶胞参数:a=1.0549nm,b=1.1813nm,c=1.4518nm,a=108.9910(1)°,β=94.9630(1)°,γ=107.7130(1)°,V=1.5945nm3,Z=1,Dc=1.609g.cm-3,μ=1.400mm-1,F(000)=776,R=0.0208,Rw=0.0544,Mr=1545.04.

A new binuclear lanthanide complex, La2 （ m-MOBA）6 （Phen）2 （1, m-MOBA： m-methoxybenazoic acid; Phen： phenanthroline）, was synthesized and characetrized by X-ray diffraction. The complex crystallized in the triclinic space P-1 with a = 1.054 9 nm, b = 1.181 3 nm, c = 1.451 8 nm, α=108.991 0（10）°, β=94.963 0（10）°,γ = 107.713 0（10）°, V = 1.594 5 nm^3, Z = 1, Dc = 1.609 g/cm^-3 ,μ = 1.400 mm^-1 , F（000） = 776, R = 0.020 8, Rw = 0.054 4, Mr = 1 545.04. In the complex 1, two La^3＋ ions were coordinated by seven oxygen atoms from m-MOBA and two nitrogen atoms from Phen, respectively, and the nine coordinate LaO7N7 center exhibited a distorted tri-capped triangular prism geometry. The carboxylate group of m-MOBA linked to the center ion La^3＋ in three different modes： chelating mode, bridging model and bridging-chelating mode, and the Phen ligand adopted the chelating mode to coordinate the La^3＋ ion. Some kinds of weak intermolecular interaction existed in the crystal, such as π-π stacking forces, C-H…O hydrogen bonds, C-H…π hydrogen bonds and C-H…H-C dihydrogen bonds.