摘要
以A lC l3.6H2O、Na2MoO4.2H2O、CoC l2.6H2O和2,2′-联吡啶为主要原料合成了Anderson-B-型多金属氧酸盐[Co(2,2-′b ipy)3]H[A l(OH)6(Mo6O18)].5H2O,进行了红外光谱、紫外光谱、差热分析和单晶结构测定。晶体学测定结果表明,化合物属于三斜晶系,Pī空间群,晶胞参数:a=1.216 0(2),b=1.221 5(2),c=1.780 0(4)nm,α=86.83(3)°,β=88.76(3)°,γ=89.82(3)°,V=2.639 4(9)nm3,Z=2,R1=0.079 4,wR2=0.176 6。化合物结构分析表明,在晶体学上,标题化合物分子是由1个[Co(2,2-′b ipy)3]2+配阳离子,1个H+离子,2个1/2[A l(OH)6(Mo6O18)]3-多阴离子和5个结晶水分子组成。多阴离子[A l(OH)6(Mo6-O18)]3-借助水分子和金属配离子通过超分子作用形成二维网状结构,网状结构之间又借助超分子作用形成三维无限伸展结构。差热分析表明,标题化合物的失重过程分为2步,多阴离子骨架破坏温度为547.5℃。
A B-Anderson-type polyoxometalate [ Co （ 2,2＇-bipy）3 ] H [ Al （OH） 6 （ Mo6O8 ） ] · 5H2O has been synthesized from AlCl3 · H2O, Na2MoO4 · 2H2O, CoCl2 · 6H2O and 2,2＇-bipydine and characterized by means of IR, UV spectra, thermogravimetric analysis and X-ray diffraction. The X-ray crystallography indicates that the title compound crystallizes in a triclinic lattice, P1^- space group, with a = 1. 216 0 （2）, b = 1. 221 5（2）, c = 1. 780 0（4） nm, α =86. 83（3）°, β =88.76（3）°, γ =89. 82（3）°, V=2. 639 4（9） nm^3, Z=2, R1 =0. 079 4, wR2 =0. 176 6. Structural analysis reveals that the molecule of the title compound is composed of one [ Co（2,2＇-bipy） 3 ] 2. coordination cation, one H^＋ ion, two crystallographically independent ＂one-half＂ polyoxoanions [ Al （OH） 6 （ Mo6O18 ） ]^3 - and five hydration water molecules. Under the participation of water and coordinated metal ions, the [ Al（OH） 6 （ Mo6O18 ） ]^3- polyoxoanions form a two-dimensional network structure by means of supramolecular interaction. The adjacent network structures interact with each other, generating a three-dimensional structure infinitely extended via supramolecular interaction. Thermogravimetric analysis elucidates that the process of weight loss of the title compound is divided into two stages and also reveals that the backbone of heteropolyoxoanion decomposes at 547.5 ℃.
出处
《应用化学》
CAS
CSCD
北大核心
2006年第3期289-293,共5页
Chinese Journal of Applied Chemistry
基金
河南省高校杰出科研人才创新工程项目
河南省自然科学基金
河南省教育厅基金资助项目
