论文部分内容阅读
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℃。
Anderson-B-type polyoxometallate [Co (2,2-bpypy3) 3] has been synthesized from AlCl3.6H2O, Na2MoO4.2H2O, CoCl2.6H2O and 2,2’-bipyridyl ] H [A l (OH) 6 (Mo6O18)] .5H2O. The infrared spectra, UV spectra, DTA and single crystal structures were determined. The crystallographic results show that the compounds belong to the triclinic system, Pī space group with unit cell parameters of a = 1.216 0 (2), b = 1.221 5 (2), c = 1.780 0 (4) nm and 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. Structural analysis of the compounds showed that the title compound crystallographically consisted of one [Co (2,2-bpypy) 3] 2+ cation, one H + ion, two ½ [A l (OH ) 6 (Mo6O18)] 3-polyanion and 5 crystal water molecules. The polyanion [Al (OH) 6 (Mo6-O18)] 3- forms a two-dimensional network structure by the action of supramolecules with water molecule and metal ion, and the three-dimensional infinite extension structure . Differential thermal analysis showed that the weight loss of the title compound was divided into two steps, and the destruction temperature of polyanion skeleton was 547.5 ℃.