Laboratory X-ray powder diffraction was used to solve and refine the crystal structures of appended guest molecules within the pores of metal–organic frameworks (MOFs). Herein, we report the crystal structure of 1-propanethiol adsorbed in the pores of Co2(dobdc) (dobdc4– = 2,5-dioxido-1,4-benzenedicarboxylate, MOF-74). Soaking the activated MOF in neat 1-propanethiol resulted in the formation of 1-propanethiol–Co2(dobdc). The thiol appendant MOF maintained the crystal symmetry, with a rhombohedral space group R-3 and unit-cell parameters a = 25.9597(9) Å, c = 6.8623(5) Å, and V = 4005.0(4) Å3. As expected, the thiol sulfur formed a bond with the open cobalt metal site. The alkane chain was directed toward the center of the pore, participating in numerous van der Waals weak interactions with neighboring molecules. For the final Rietveld refinement, soft restrains were applied using bond distances obtained by periodic density functional theory (DFT) geometry optimization.

中文翻译：

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来自实验室 X 射线粉末衍射数据的 1-丙硫醇–Co2(dobdc) 的晶体结构

实验室 X 射线粉末衍射用于解决和细化金属有机框架 (MOF) 孔隙内附加客体分子的晶体结构。在此，我们报告了吸附在 Co 孔中的 1-丙硫醇的晶体结构。2(dobdc) (dobdc)4–= 2,5-二氧化-1,4-苯二甲酸酯，MOF-74)。将活化的 MOF 浸泡在纯 1-丙硫醇中导致 1-丙硫醇-Co 的形成2(dobdc)。硫醇附加物 MOF 保持晶体对称性，具有菱面体空间群R-3 和单胞参数一种= 25.9597(9) 埃，C= 6.8623(5) Å，和五= 4005.0(4) Å3. 正如预期的那样，硫醇硫与开放的钴金属位点形成了键。烷烃链指向孔的中心，参与了与相邻分子的大量范德华弱相互作用。对于最终的 Rietveld 细化，使用通过周期性密度泛函理论 (DFT) 几何优化获得的键距离应用软约束。