论文部分内容阅读
在乙腈和水的混合溶剂中制得四水·四 (N 甲基吡咯烷酮 )合钐 (Ⅲ )配离子与硅钼酸阴离子形成的复合物[Sm(NMP) 4(H2 O) 4][HSiMo1 2 O4 0 ]·2NMP·H2 O (NMP =N 甲基吡咯烷酮 ) ,并对其进行了晶体结构测定 .结构分析结果表明该晶体属单斜晶系 ,P2 1 c空间群 .晶胞参数a =1 75 0 1(4)nm ,b=1 82 6 9(4)nm ,c=2 32 6 4 (5 )nm ,β =10 6 6 7(3)°,Z =4 ,V =7 12 6 (2 )nm3,Dc=2 4 5 7g cm3,R =0 0 6 71,wR =0 16 35 .结构测定结果表明 ,复合物中Sm3+ 与 4个N 甲基吡咯烷酮和 4个H2 O分子配位 ,以八配位的三角十二面体结构阳离子通过静电作用与SiMo1 2 O4 04 - 阴离子相结合 ,分子中的质子氢存在于两个游离的N 甲基吡咯烷酮的羰基氧之间 .光照后复合物的低温ESR谱出现了Mo5+ 的顺磁信号 ,求得Mo5+ 的g值为 1 94 4 7.热性质的研究表明 ,形成标题化合物后 ,阴离子热稳定性增强
(Sm (NMP) 4 (H 2 O) 4] [HSiMo 1 (II)) was prepared by the complexation of samarium (III) methyltetrakis (N-methylpyrrolidone) complex ion with silicomolybdic acid anion in a mixed solvent of acetonitrile and water 2 O 4 0] · 2NMP · H 2 O (NMP = N-methylpyrrolidone) was synthesized and its crystal structure was determined.The structural analysis showed that the crystal belongs to the monoclinic space group P2 1 c with a = 1 75 0 1 (4) nm, b = 1 82 6 9 (4) nm, c = 2 32 6 4 (5) nm, β = 10 6 6 7 (3) °, Z = 4, V = 7 12 6 (2) nm3, Dc = 2 4 5 7g cm3, R = 0 0 6 71, wR = 0 16 35. The results of the structure determination show that Sm3 + complex with 4 N-methylpyrrolidone and 4 H2 O molecules , The octahedron dodecahedron cation is combined with SiMo1 2 O4 04 - anion through electrostatic interaction, and the proton hydrogen in the molecule exists between the two free N-methyl pyrrolidone carbonyloxy groups The low temperature ESR spectrum of the material shows the paramagnetic signal of Mo5 +, and the value of g of Mo5 + is found to be 1 94 4 7. Studies on the thermal properties show that the thermal stability of the anion is enhanced after the formation of the title compound