o,o-二(β-叠氮乙基)-α-对甲苯磺酰胺基对硝基苄基磷酸酯的合成与晶体结构  

SYNTHESIS AND CRYSTAL STRUCTURE OF o,o-BIS(β-AZIDOETHYL)-α-p-TOLUENESULFONAMIDO-α -p-NITROBENZALPHOSPHONATE

作　　者：李奇[1] 叶玲[2] 张锦楠[2] 石梅[1] 

机构地区：[1]北京师范大学化学系,北京100875 [2]首都医科大学基础医学院,北京100054

出　　处：《北京师范大学学报（自然科学版）》2002年第3期381-385,共5页Journal of Beijing Normal University(Natural Science)

基　　金：国家自然科学基金资助项目 (2 99730 0 5 )

摘　　要：合成了o ,o 二 (β 叠氮乙基 ) α 对甲苯磺酰胺基 对硝基苄基磷酸酯 (C18H2 1N8O7PS) ,通过元素分析、IR和1HNMR对化合物进行了表征 ,用X射线单晶衍射法测定了该化合物的晶体结构 .结果表明晶体属三斜晶系 ,P1空间群 ,a =0 .8136 (1)nm ,b =1.1872 (1)nm ,c=1.3412 (1)nm ,α =10 9.4 5 5 (7)°,β =90 .880 (8)° ,γ =96 .86 3(9)° ,V =1.2 10 6 (3)nm3,Mr=5 2 4 .4 6 ,ρc=1.4 39g·cm- 3,Z =2 ,μ(MoKα) =0 .2 6 0 mm- 1,F(0 0 0 ) =5 44,在 0° <2θ <5 0°范围内收集 35 6 0个独立衍射点 ,其中可观测衍射点 2 70 0个 (|F| 2 ≥ 6 .0σ|F| 2 ) .晶体结构用直接法解出 ,经全矩阵最小二乘法修正 ,最后的偏离因子为R =0 .10 6 ,RW=0 .0 95 .化合物的分子中 ,2个取代苯环位于分子主链的同一侧 ,2个苯环平面近于平行 .2个取代的叠氮乙基的取向近于平行地指向同一方向 ,向着几乎垂直于苯平面的方向伸展 .2个独立的分子之间以 1对N—H…O氢键连接形成中心对称的二聚体 ,成为晶体结构的基本重复单元 .The title compound ( C 18 H 21 N 8O 7PS ) are synthesized and characterized by elemental analysis, IR, 1HNMR and X ray single crystal diffraction. The crystal belongs to triclinic system, P1 space group with a =0.813 6(1) nm, b = 1.187 2(1) nm, c =1.341 2(2) nm, α =109.455(7)°, β =90.880(8)°, γ =96.863(9)°, V =1.210 6(3) nm 3 , M r=524.46, Z = 2, ρ c=1.439 g·cm -3 , F (000)=544, μ (MoKα)=0.260 mm -1 , R =0.106, R W =0.095 for 2 700 observed reflections (| F| 2≥6.0σ|F| 2). In the molecule of the title compound, the azidoethyl groups placed at the same side of the shielding area of α benzene ring are far from this area and almost vertical to it. These two groups are almost parallel to each other and point to the same direction. Two molecules in the unit cell are linked by a pair of N-H...O hydrogen bonds between the amino H atom and the phosphonic oxygen atom to form a centrosymmetric dimer. The crystal structure is built up from a stacking of these dimers such that the inter dimer interactions are mainly of van der Waals type.

关 键 词：合成 叠氮化合物 晶体结构 X射线单晶衍射法 o o-二(β-叠氮乙基)-α-对甲苯磺酰胺基-对硝基苄基磷酸酯 

分 类 号：O625.6[理学—有机化学] O627.51[理学—化学]