Crystal structure of tropone at –60 °C
Crystal structure of tropone at –60 °C
复制标题
–60 °C 时托品酮的晶体结构
DOI：
10.1039/c39730000066
复制
发表时间：
1973
期刊：
影响因子：
--
通讯作者：
G. Filippini
中科院分区：
文献类型：
--
作者：
M. Barrow;O. S. Mills;G. Filippini
尽管在过去的二十年中，已经有许多尝试将tropone的化学和物理性质与结构模型联系起来，并且已经报道了大量的理论计算，但令人惊讶的是，没有发表准确的三维x射线分析。在室温下，tropone是一种液体（mp-7”C），对光和空气不稳定。我们进行了60”C温度下的晶型分析，晶型数据：C， H， O， M= 106-1，单斜晶型，a= 6.1 (3), b= 7* 91 (3)， U= 572 A3, 2= 4, D = 1.23。空间群Pc （C:, No. 7）的系统缺失与分析。801个摄影强度，其中80个为“零”，通过视觉估计（Weissenberg技术）。所有反射的r5.4，仅观察到的反射为4.9。用直接方法进行的分析由于每个不对称单元出现两个分子而变得复杂。此外，这两个分子的环是通过双螺旋轴的伪对称操作联系起来的（见图）。
ALTHOUGH there has been a number of attempts to relate the chemical and physical properties of tropone to structural models, and extensive theoretical calculations have been reported over the past twenty years, it is surprising that no accurate three-dimensional X-ray analysis has been published. At room temperature, tropone is a liquid (mp-7" C), unstable to light and air. We have undertaken the analysis of crystalline tropone at-60" C. Crystal data: C, H, O, M= 106-1, monoclinic, a= 6.1 1 (3), b= 7* 91 (3), U= 572 A3, 2= 4, D,= 1.23. Space group Pc (C:, No. 7) by systematic absences and analysis. 801 photographic intensities, of which 80 were'zero', were estimated visually (Weissenberg technique). R 5.4 for all reflexions, 4.9 for observed reflexions only. The analysis, by direct methods, was complicated by the occurrence of two molecules per asymmetric unit. Moreover, the rings of these two molecules were related by the pseudo-symmetry operation of a twofold screw axis (see Figure).