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用X射线晶体结构分析法测定了氯代羟基六氢茚二酮(1)和环氧十氢萘二酮(2)的晶体结构和分子构型.化合物1属正交晶系,空间群为Pbca,晶胞参数α=10.439(1),b=19.950(2),c=9.455(1)A,Z=8;化合物2属单斜晶系,空间群为P2_1/c,晶胞参数α=8.355(2),b=9.221(2),c=25.801(4)A,β=294.19(1)°,Z=8.在RASA-IIS型四圆衍射仪上收集了这两个化合物的衍射数据,用直接法解晶体结构,经块对角矩阵最小二乘修正,对化合物1的1810个独立的可观察反射,R=0.043;对化合物2的1804个独立的可观察反射,R=0.064.化合物l带有α-Cl,β-CH_3和β-OH.由此推断环氧六氢茚二酮(3)的分子构型带有β-CH_3和β-环氧.化合物2中的甲基和环氧基均为β构型,与3相似.因此Danishefsky等由核磁共振所推断的关于2的分子构型中的α环氧应校正为β环氧.
The crystal structure and molecular configuration of chlorohexahydroindione (1) and epoxy decahydronaphthacene (2) were determined by X-ray crystal structure analysis. Compound 1 belongs to orthorhombic system with space group of Pbca. The unit cell parameters α = 10.439 (1), b = 19.950 (2), c = 9.455 (1) A and Z = 8. Compound 2 belongs to monoclinic system with space group P2_1 / = 8.355 (2), b = 9.221 (2), c = 25.801 (4) A, β = 294.19 (1) °, Z = 8. The two compounds were collected on a RASA-IIS four-circle diffractometer The diffraction data were solved using the direct method for crystal structure, corrected for block diagonal matrix least squares, for 1810 independent observable reflections of compound 1, R = 0.043; for 1804 independently observable reflections of compound 2, R = 0.064. Compound 1 carries α-Cl, β-CH_3 and β-OH, which suggests that the molecular configuration of hexanedione (3) carries β-CH_3 and β-epoxy. Both the methyl and epoxy groups are in the β configuration, similar to 3. Therefore, the α-epoxy in the molecular configuration of 2 deduced by NMR by Danishefsky et al. Should be corrected to β-epoxy.