4-(2′-羟基苯甲酰肼)苯亚甲基/亚乙基-5-甲基-2-苯基-2,4-二氢-吡唑啉酮-3超分子化合物的合成与晶体结构  

Synthesis and Crystal Structure of Supramolecular Compound of 4-(2′-Hydroxybenzoylhydrazinyl)benzal/ethylidene-5-methyl-2-phenyl-2,4-dihydropyrazol-3-one

作　　者：刘浪[1] 吉亚丽[1] 贾殿赠[1] 郁开北[2] 

机构地区：[1]新疆大学应用化学研究所,乌鲁木齐830046 [2]中国科学院成都分院分析测试中心,成都610041

出　　处：《化学学报》2003年第6期893-900,共8页Acta Chimica Sinica

基　　金：国家自然科学基金 (Nos.2 0 2 62 0 0 5 ;2 0 1 61 0 0 3)资助项目

摘　　要：报道了 4 (2′ 羟基苯甲酰肼 )苯亚甲基 5 甲基 2 苯基 2 ,4 二氢 -吡唑啉酮 3 (B1)和 4 (2′ 羟基苯甲酰肼 )亚乙基 5 甲基 2 苯基 2 ,4 二氢 -吡唑啉酮 3 (B2 )的合成、表征及晶体结构分析 ,B1晶体属单斜晶系 ,C2 /c空间群 ,所得晶胞参数为 :a =1.42 0 1(2 )nm ,b =1.65 5 42 (2 )nm ,c =1.845 5 (3 )nm ,β =10 1.3 2 (1)° ,V =4.2 5 41(10 )nm3 ,Z =8,Dc=1.3 44g/cm3 ,μ =0 .0 94mm-1,F(0 0 0 ) =180 8,R =0 .0 44 2 ,wR =0 .10 3 7.该化合物由水分子通过氢键连接成沿ac面无限延伸的二维网络结构的超分子 .B2 晶体属三斜晶系 ,P 1空间群 ,a =1.2 12 0 (2 )nm ,b =1.2 2 2 3 (2 )nm ,c =1.415 9(3 )nm ,α =70 .3 8(1)° ,β =74.91(1)° ,γ =63 .64 (1)° ,V =1.75 49(5 )nm3 ,Z =4,Dc=1.3 2 6g/cm3 ,μ =0 .0 92mm-1,F(0 0 0 ) =73 6,R =0 0 43 6,wR =0 .10 76.此化合物通过分子间氢键形成沿a轴无限延伸的一维链状结构的超分子 。The synthesis and crystal structure of 4-(2'-hydroxybenzoylhydrazinyl) benzal-5-methyl-2-phenyl-2, 4-dihydropyrazol-3-one (B-1) and 4-(2'-hydroxybenzoylhydrazinyl) ethylidene-5-methyl-2-phenyl-2,4-dihydropyrazol-3-one (B-2) are presented in this paper. The crystal structures were determined by X-ray single crystal diffraction study. Crystal structure of B-1 belongs to monoclinic system with space group C2/c. The unit cell parameters are a = 1.4201 (2) nm, b = 1.65542 (2) run, c = 1.8455(3) nm, beta = 10132(1)degrees, V = 4.2541(10) nm(3), Z = 8, D-c = 1.344 g/cm(3), mu = 0.094 mm(-1), F(000) = 1808, R = 0.0442, wR = 0.1037. The water molecules bridge the adjacent stacks by the hydrogen bonds leading to the formation of supramolecular compound with two-dimensional network structure along the ac side. The crystal structure of B-2 belongs to triclinic system with space group P (1) over bar. The unit cell parameters are a = 1.2120(2) nm, b = 1.2223 (2) mn, c = 1.4159(3) nm, alpha = 70.38 (1)degrees, beta = 74.91 (1)degrees, gamma = 63.64 (1)degrees, V = 1. 7549(5) nm(3), Z = 4, D-c = 1.326 g/cm(3), mu = 0.092 mm(-1), F (000) = 736, R = 0.0436, wR = 0.1076. The supramolecule with one dimensional chain structure was formed through hydrogen bonds along the a axis. The molecules piled the layered structure along the b axis due to intermolecular interactions.

关 键 词：4-(2′-羟基苯甲酰肼)苯亚甲基-5-甲基-2-苯基-2 4-二氢-吡唑啉酮-3 超分子化合物 合成 晶体结构 4-(2′-羟基苯甲酰肼)亚乙基-5-甲基-2-苯基-2 4-二氢-吡唑啉酮-3 氢键 

分 类 号：O72[理学—晶体学]