[Nd(C_(10)H_9N_2O_4)(C_(10)H_8N_2O_4)(H_2O)_3]_2·phen·4H_2O超分子化合物的合成、晶体结构及热稳定性

Synthesis, Crystal Structure and Thermal Stability of Supra-molecule Complex of [Nd(C_(10)H_9N_2O_4)(C_(10)H_8N_2O_4)(H_2O)_3]_2·phen·4H_2O

在水-乙醇混合体系中,以2-羰基丙酸水杨酰腙(C10H10N2O4)、1,10-菲啉(C12H8N2,简称phen)与N d(NO3)3.4H2O反应,首次培养出黄色单晶[N d(C10H9N2O4)(C10H8N2O4)(H2O)3]2.phen.4H2O.该晶体属三斜晶系,空间群为P-1,晶胞参数a=1.390 1(2)nm,b=1.407 3(2)nm,c=1.764 5(3)nm,α=74.298(2),°β=68.911(2),°γ=71.703(2),°V=3.009 1(8)nm3,Z=2,μ=1.800 mm-1,Dc=1.690 g/cm3,F(100)=1 544,R=0.028 4,wR=0.063 0,GOF=1.010.所测单晶的每个配合物分子中含有两个N d(Ⅲ)的9配位结构单元,每个N d(Ⅲ)分别与两个2-羰基丙酸水杨酰腙和三个水分子配位;每个2-羰基丙酸水杨酰腙中的羧基氧、酰胺基中的羰基氧和C=N中的氮与N d3+配位,形成两个共边的稳定五元环,另三个配位原子则分别来自三个水分子中的氧原子,该结构单元呈扭曲的单帽四方反棱柱,而在每两个N d的九配位单元周围还有一个游离的1,10-菲啉分子和四个水分子.整个配合物通过氢键连结成一个三维网状超分子化合物.IR及热分析佐证了配合物的组成.

Neodymium （ Ⅲ） complex with 2-oxo-propionic acid salicyloyl hydrazone （C10H10N2O4） and 1, 10-phenanthrolines （C12H8N2, phen） have synthesized. A yellow prismatic crystal of the complex [Nd（C10H9N2O4）（H2O）3]2·phen·4H2O was obtained for the first time, the molecular structure crystallized in the triclinic space group P-1 with a=1. 390 1 （2） nm, b=1.407 3（2） nm, c=1. 764 5（3） nm, α=74. 298（2）°,β=68. 911（2）°,7=71. 703（2）°,V =3. 009 1（8）nma, Z=2, μ=1. 800 mm^-1, Dc=1. 690 g/cm^3, F（000） =1 544, R=0. 028 4, ωR= 0. 063 9, GOF=1. 010. There are two 9-coordinated units in every moleculer, every Nd （ Ⅲ ） is coordinated by carboxyl and carbonyl O atoms and N atom of two tridentate ligands, which forming two stable pentacyclic with a same border, the other coordinated atoms came from three water mlecules. The coordination polyhedron around Nda＋was described as a single cap square antiprism. In the crystal cell, there are one free 1, 10-phenanthrolines and four water molecules. The coordination polyhedron around Nd^3＋ was described as a single cap square antiprism. In the crystal cell, there are one free 1,10-phenanthrolines and four water molecules that are connected with 2-oxo-Propionic acid salicyloyl hydrazone and water mo lecule by hydrogen bonds. Because of the hydrogen bonds the complex formed a supera-molecule in space. The IR and thermal decomposition verified the composition of the complex.