Glinski J A, Asibal C F, Van Derveer D, Zalkow L H
School of Chemistry, Georgia Institute of Technology, Atlanta 30332.
Acta Crystallogr C. 1988 Sep 15;44 ( Pt 9):1593-8. doi: 10.1107/s0108270188004214.
lambda(Mo K alpha) = 0.71069 A, T = 298 K. Anonamine (I) (12,21-dihydroxy-4-methyl-4,8-secosenecionan-8,11,16-trione): C19H27NO7, Mr = 381.2, monoclinic, C2, a = 24.247 (7), b = 8.766 (2), c = 9.072 (1) A, beta = 99.21 (2) degrees, U = 1903.3 (8) A3, Z = 4, Dm = 1.32 (1), D chi = 1.330 g cm-3, mu(Mo K alpha) = 1.09 cm-1, F(000) = 816. Neosenkirkine (II) (12-hydroxy-4-methyl-4,8-secosenecionan-8,11,16-trione): C19H27NO6, Mr = 365.2, monoclinic, C2, a = 24.45 (1), b = 8.781 (2), c = 9.029 (2) A, beta = 98.99 (3) degrees, U = 1915 (1) A3, Z = 4, Dm = 1.27 (1), D chi = 1.267 g cm-3, mu(Mo K alpha) = 1.01 cm-1, F(000) = 784. Hydroxysenkirkine (III) [12,18-dihydroxy-4-methyl-4,8-secosenecionan-8, 11,16-trione-methanol (1/1)]: C19H27NO7.CH3OH, Mr = 413.2, orthorhombic, P2(1)2(1)2(1), a = 9.052 (3), b = 13.150 (4), c = 17.404 (8) A, U = 2071 (1) A3, Z = 4, Dm = 1.33 (1), D chi = 1.325 g cm-3, mu(Mo K alpha) = 1.10 cm-1, F(000) = 888. Full-matrix least squares refinement converged at R values of 0.042, 0.043 and 0.051 for 3163, 2894 and 2896 reflections for (I), (II), (III), respectively. All three crystals exhibit hydrogen bonds, including intramolecular O11...HO12 and intermolecular O8...HO12. In addition, intermolecular hydrogen bonds appear in (I) between O21...HO21' and in (III) between O8...HOCH3. The observed N...C8 distances across the eight-membered otonecine rings were 2.200, 2.245 and 1.712 A in (I), (II) and (III) respectively.
λ(钼Kα)= 0.71069埃,温度T = 298K。去甲千里光胺(I)(12,21 - 二羟基 - 4 - 甲基 - 4,8 - 断千里光烷 - 8,11,16 - 三酮):C₁₉H₂₇NO₇,Mr = 381.2,单斜晶系,C2,a = 24.247(7),b = 8.766(2),c = 9.072(1)埃,β = 99.21(2)°,晶胞体积U = 1903.3(8)埃³,Z = 4,Dm = 1.32(1),Dc = 1.330克/立方厘米,μ(钼Kα)= 1.09厘米⁻¹,F(000) = 816。新千里光碱(II)(12 - 羟基 - 4 - 甲基 - 4,8 - 断千里光烷 - 8,11,16 - 三酮):C₁₉H₂₇NO₆,Mr = 365.2,单斜晶系,C2,a = 24.45(1),b = 8.781(2),c = 9.029(2)埃,β = 98.99(3)°,U = 1915(1)埃³,Z = 4,Dm = 1.27(1),Dc = 1.267克/立方厘米,μ(钼Kα)= 1.01厘米⁻¹,F(000) = 784。羟基千里光碱(III)[12,18 - 二羟基 - 4 - 甲基 - 4,8 - 断千里光烷 - 8,11,16 - 三酮 - 甲醇(1/1)]:C₁₉H₂₇NO₇·CH₃OH,Mr = 413.2,正交晶系,P2(1)2(1)2(1),a = 9.052(3),b = 13.150(4),c = 17.404(8)埃,U = 2071(1)埃³,Z = 4,Dm = 1.33(1),Dc = 1.325克/立方厘米,μ(钼Kα)= 1.10厘米⁻¹,F(000) = 888。全矩阵最小二乘法精修分别对(I)、(II)、(III)的3163、2894和2896个反射收敛,R值分别为0.042、0.043和0.051。所有三种晶体都存在氢键,包括分子内的O11…HO12和分子间的O8…HO12。此外,(I)中在O21…HO21'之间以及(III)中在O8…HOCH₃之间出现分子间氢键。在(I)、(II)和(III)中,观察到跨越八元奥托千里光环的N…C8距离分别为2.200、2.245和1.712埃。