Lynch V M, Lee W C, Martin S F, Davis B E
Department of Chemistry and Biochemistry, University of Texas, Austin 78712.
Acta Crystallogr C. 1991 May 15;47 ( Pt 5):1117-20. doi: 10.1107/s0108270190012008.
(3S,4R,5S,6R,7R,9R,10S,11S,12S,13S,- 14R)-14-Benzyloxymethoxy-10,12-O-carbonyl-4-N- imidazolylcarbonyl-6,7-O-isopropylidene-3,5,7,9,11,- 13-hexamethylhexadec-1-ene-4,6,7,10,12,14-hexol, C38H56N2O9, Mr = 684.87, monoclinic, P2(1), a = 8.7302 (12), b = 15.597 (2), c = 14.463 (2) A, beta = 104.797 (10) degrees, V = 1904.1 (4) A3, Z = 2, Dx (198 K) = 1.19 g cm-3, mu = 0.7893 cm-1, Mo K alpha radiation, lambda = 0.7107 A, F(000) = 740, T = 198 K, R = 0.0301 for 3141 reflections [Fo greater than or equal to 4 sigma (Fo)]. The crystal structure was undertaken to determine the stereochemistry of the title compound. The molecule is folded on itself in such a way that the portion of the molecule from the phenyl ring at C44 and extending to C28 forms nearly a single turn of a right-handed screw. Large deviations from ideality for several Csp3-Csp3 bond angles are observed that are presumably due to intramolecular steric effects. The largest deviations are: C3-C4-C5 117.8 (2), C5-C6-C7 121.2 (2), C7-C8-C9 115.3 (2), C9-C10-C11 116.2 (2), C11-C12-C13 117.2 (2), C14-C15-C16 115.5 (3) degrees.
(3S,4R,5S,6R,7R,9R,10S,11S,12S,13S,-14R)-14-苄氧基甲氧基-10,12-O-羰基-4-N-咪唑基羰基-6,7-O-异亚丙基-3,5,7,9,11,-13-六甲基十六碳-1-烯-4,6,7,10,12,14-己醇，C38H56N2O9，Mr = 684.87，单斜晶系，P2(1)，a = 8.7302 (12)，b = 15.597 (2)，c = 14.463 (2) Å，β = 104.797 (10)°，V = 1904.1 (4) Å3，Z = 2，Dx (198 K) = 1.19 g cm-3，μ = 0.7893 cm-1，钼Kα辐射，λ = 0.7107 Å，F(000) = 740，T = 198 K，对于3141个反射[Fo≥4σ(Fo)]，R = 0.0301。进行晶体结构分析以确定标题化合物的立体化学。分子自身折叠，使得从C44处的苯环延伸至C28的分子部分形成近乎一个右旋螺旋的单圈。观察到几个Csp3-Csp3键角与理想值有较大偏差，这可能是由于分子内的空间效应。最大偏差为：C3-C4-C5 117.8 (2)，C5-C6-C7 121.2 (2)，C7-C8-C9 115.3 (2)，C9-C10-C11 116.2 (2)，C11-C12-C13 117.2 (2)，C14-C15-C16 115.5 (3)°。
