Gallucci J C, Taylor R T, Kobayashi T, Weber J C, Krause J, Paquette L A
Evans Chemical Laboratories, Ohio State University, Columbus 43210.
Acta Crystallogr C. 1989 Jun 15;45 ( Pt 6):893-8. doi: 10.1107/s0108270188013721.
Methyl dodecahedranecarboxylate, C22H22-O2, (4), Mr = 318.42, monoclinic, C2/c, a = 12.600 (2), b = 7.992 (4), c = 28.975 (7) A, beta = 101.79 (2) degrees, V = 2856 A3, Z = 8, Dx = 1.48 g cm-3, lambda(Mo K-alpha) = 0.71073 A, mu = 0.84 cm-1, F(000) = 1360, T = 294 K, R = 0.044 for 2109 unique reflections with Fo2 greater than 3 sigma(Fo2). 21-Phenylcyclopropadodecahedrane, C27H24, (5), Mr = 348.49, tetragonal, P4(2)/n, a = 17.528 (3), c = 10.752 (2) A, V = 3303 A3, Z = 8, Dx = 1.40 g cm-3, lambda(Mo K-alpha) = 0.71069 A, mu = 0.85 cm-1, F(000) = 1488, T = 295 K, R = 0.053 for the 1773 unique reflections with Fo2 greater than 1 sigma(Fo2). The molecular geometries of methoxycarbonyldodecahedrane (4) and 21-phenylcyclopropadodecahedrane (5) are compared to those of the parent C20H20 hydrocarbon (1) and its 1,16-dimethyl derivative (2). For both (2) and (4), the framework is modestly distorted by the substituents, the intracavity distance being more extended along the axis that contains the pendant group(s). Remarkably for (5), its cyclopropane ring has all C-C bonds and internal angles essentially equal, and those dodecahedrane bonds in the immediate vicinity of the ring fusion are extensively perturbed.
十二面体羧酸甲酯，C₂₂H₂₂ - O₂，（4），Mr = 318.42，单斜晶系，C2/c，a = 12.600（2），b = 7.992（4），c = 28.975（7）Å，β = 101.79（2）°，V = 2856 ų，Z = 8，Dx = 1.48 g cm⁻³，λ（Mo K - α） = 0.71073 Å，μ = 0.84 cm⁻¹，F(000) = 1360，T = 294 K，对于2109个Fo²大于3σ(Fo²)的独立反射，R = 0.044。21 - 苯基环丙基十二面体烷，C₂₇H₂₄，（5），Mr = 348.49，四方晶系，P4(2)/n，a = 17.528（3），c = 10.752（2）Å，V = 3303 ų，Z = 8，Dx = 1.40 g cm⁻³，λ（Mo K - α） = 0.71069 Å，μ = 0.85 cm⁻¹，F(000) = 1488，T = 295 K，对于1773个Fo²大于1σ(Fo²)的独立反射，R = 0.053。将甲氧基羰基十二面体烷（4）和21 - 苯基环丙基十二面体烷（5）的分子几何结构与母体C₂₀H₂₀烃（1）及其1,16 - 二甲基衍生物（2）的分子几何结构进行了比较。对于（2）和（4），骨架因取代基而有适度扭曲，腔内距离沿包含侧基的轴方向延伸得更多。对于（5）而言，其显著之处在于其环丙烷环的所有C - C键和内角基本相等，并且在环融合紧邻处的那些十二面体烷键受到了广泛扰动。
