吡咯并内酰胺生物碱:2-溴-6,7-二氢-1H,5H-吡咯并2,3-C氮杂-4,8-二酮的X-ray晶体结构研究

摘要

从中国南海海绵Phacellia fusca Schmidt的乙醇浸提物中,分离得到一吡咯并内酰胺:2-bro-moaldisin.通过X-射线单晶衍射法测定了该化合物的晶体结构.结果表明:晶体属正交晶系,Pbca空间群,a=12.984(7),b=7.429(4),c=18.580(10)A,V=179.2(16)A3,Z=8,Mr=243.07,Dx=1.802mg/cm3,F(000)=960,μ(Mo-Ka)=4.553 mm-1,λ=0.71073 A.在2.19＜θ＜27.27°范围内共收集了1978个独立衍射点,其中可观测衍射点1361个(|F| 2＞4σ|F|2).晶体结构用直接法解出,经全矩阵最小二乘法修正,最终偏离因子R=0.0535,Rw=0.0803.%The title compound(CsH7BrN2O2)has been isolated from the marinesponge Phakellia fusca Schimidt collected around the South China Sea, andformed colorless rhombus crystal by slow evaporation from methanol at roomtemperature. Its structure was established by single-crystal X-ray diffraction, andfurther characterized by NMR spectroscopy. The crystal belongs to orthorhom-bic system,space group Pbca with a = 12. 984(7), b = 7. 429(4), c = 18. 580(10) A, V = 1792.2( 16)A3, Z = 8, Mr = 243.07, Dx = 1. 802 mg/cm3, F (000)=960,μ (Mo-Ka) = 4. 553 mm-1, λ = 0. 71073 A. The structure was refinedto R = 0. 0535 and Rw = 0. 0803 for 1361 observed reflections(|F|2 ＞ 4σ|F|2).