一种抗肿瘤化合物(3aRS,4RS,7RS,7aSR)-2-(三环[3.3.1.1^(3,7)]癸烷)-4,5,6,7-四氢-4,7-异吲哚-1,3-二酮新晶型的制备及其X-射线衍射分析(英文)

Preparation and X-ray diffraction analysis of a new crystal form of(3aRS,4RS,7RS,7aSR)-2-(tricyclo[3.3.1.1^(3,7)]decan-1-yl)-4,5,6,7-tetrahydro-4,7-epoxyisoindoline-1,3-dione-a novel anticancer compound

目的确定标题化合物(C18H23NO3,Mr=301.37)的新晶型。方法制备化合物晶体,并用单晶X-射线对其晶型结构进行确定。结果新晶型属于单斜晶系,空间群为P21/n,晶胞参数为a=0.687 288(16)nm,b=1.026 47(2)nm,c=2.143 46(5)nm,β=94.579(2)°,V=1.507 34(6)nm3,Z=4,Dx=1.340mg/m3,λ(Cu Kα)=0.154 184 nm,F(000)=653.6,μ(Cu Kα)=0.74 mm-1,R=0.082,wR=0.219。测定中衍射仪共收集到2 707个独立反射,其中的2 396个符合条件I>2σ(I)。五元内酰胺环与C1～C4平面间的二面角为66.3°。晶体中的各分子通过C—H…O键相互连接,同时还存在分子内氢键C(10)—H(10A)…O(3)和C(13)—H(13A)…O(3)。分子内氢键和分子键范德华力的存在是该结构稳定的原因。结论标题化合物存在多晶型。

Objective To determine a new crystal form of the title compound（C18H23NO3,Mr=301.37）.Methods To prepare the crystals and determine the crystal structure by single-crystal X-ray diffraction.Results The crystal belonged to monoclinic,space group P21/n,with a=0.687 288（16） nm,b=1.026 47（2） nm,c=2.143 46（5） nm,β=94.579（2）°,V=1.507 34（6） nm3,Z=4,Dx=1.340 mg/m3,λ（Cu Kα）=0.154 184 nm,F（000）=653.6,μ（Cu Kα）=0.74 mm-1,R=0.082 and wR=0.219.A total of 2 707 independent reflections were collected,of which 2 396 with I2σ（I）were observed.The dihedral angle between five-membered lactam ring and the C1-C4 plane was 66.3°.The individual molecules in the crystal structure were linked via C—H…O interactions leading to the formation of a supra-molecule.To our interest,intramolecular C（10）—H（10A）…O（3） and C（13）—H（13A）…O（3） hydrogen bonds were found in each molecule.Intramolecular hydrogen bonds and intermolecular van der Waals force contributed to the stability of the structure.Conclusion The title compound had polymorphic crystal structure.