3,4-二氨基呋咱基氧化呋咱的制备及晶体结构研究  

Study on the Preparation and Crystal Structure of 3,4-Diaminofurazanofuroxan

作　　者：王军[1] 董海山[1] 黄奕刚[1] 李金山[1] 

机构地区：[1]中国工程物理研究院化工材料研究所,绵阳621900

出　　处：《化学学报》2006年第2期158-162,共5页Acta Chimica Sinica

基　　金：中国工程物理研究院重大基金(No.2002Z0501)资助项目.

摘　　要：首次通过3-氨基-4-氯肟基呋咱在热作用下脱HCl、[4+2]关环反应制备了新型呋咱(氧化呋咱)类含能化合物3,4-二氨基呋咱基氧化呋咱(DAFF),并培养出了DAFF单晶.用X射线单晶衍射、元素分析和红外光谱对其分子结构进行了表征.测试结果表明:DAFF晶体属三斜晶系,空间群P1,a=0.6400(4)nm,b=1.0609(8)nm,c=1.4634(7)nm,α=83.53(5)°,β=87.27(4)°,γ=77.74(5)°,V=0.9645(11)nm3,Z=4,Dc=1.737g?cm-3,F(000)=512,μ(MoKα)=0.149mm-1;R1=0.0568,wR2=0.1137.DAFF分子不共面,三环面扭曲,面间夹角为27.18(1.99)°和30.48(2.07)°,晶体中存在分子内和分子间氢键.A new furazano （furoxano） energetic compound 3,4-diaminofurazanofuroxan （DAFF） was first prepared under thermal conditions by losing HC1 followed by [4 ＋ 2] ring-closure reaction of 3-amino-4-chloroximinofurazan. Its single crystal was cultivated and the structure was characterized by X-ray single crystal diffraction, IR and elemental analysis. Its crystal is triclinic, space group P1 with crystal parameters a=0.6400（4） nm, b=1.0609（8） nm, c=1.4634（7） nm, α=83.53（5）°, β=87.27（4）°, γ= 77.74（5）°, V=0.9645（11） nm^3, Z=4, Dc=1.737 g·cm^-3, F（000）=512, μ（Mo Kα）=0.149 mm^-1; R1= 0.0568, wR2=0.1137. The obtained results indicate that DAFF is not a kind of planar molecule, the three ring-planes twist with the two clamp-angles between them are 27.18（1.99）° and 30.48（2.07）°, respectively. There are intramolecular and intermolecular hydrogen bonds in the crystal.

关 键 词：含能化合物 呋咱(氧化呋咱) 3 4-二氨基呋咱基氧化呋咱(DAFF) 制备 晶体结构 

分 类 号：O626.11[理学—有机化学]