Department of Chemistry, University of Oslo, PO Box 1033, 0315 Oslo, Norway.
Chem Soc Rev. 2017 Aug 14;46(16):4867-4876. doi: 10.1039/c6cs00533k.
Single crystal X-ray diffraction (SC-XRD) is the principal method for determining the crystal structures of metal-organic frameworks (MOFs). This tutorial deals with the handling of MOF crystals and analysis of crystallographic data obtained from single-crystal X-ray diffraction, focusing on two features that are particularly important in MOF crystallography and have a large impact on the quality and reliability of the final crystal structures: (1) the treatment of pore-occupying entities (both in the physical crystals and in the crystallographic model) and (2) crystallographic twinning. Proper handling of samples and data will reduce the need for using solvent masking software (e.g. SQUEEZE) to obtain acceptable crystal structures. If SC-XRD is to retain its position as the definitive method of MOF structure determination, these issues must be addressed when a new MOF structure is determined and reported. The issues addressed in this review is also valid for other porous, crystalline solids such as porous organic cages, metal-organic polyhedra, covalent organic frameworks and zeotype materials.
单晶 X 射线衍射（SC-XRD）是确定金属有机骨架（MOF）晶体结构的主要方法。本教程介绍了 MOF 晶体的处理以及从单晶 X 射线衍射获得的晶体学数据的分析，重点介绍了在 MOF 晶体学中特别重要且对最终晶体结构的质量和可靠性有重大影响的两个特征：（1）孔占据实体（无论是在物理晶体还是晶体学模型中）的处理，以及（2）晶体学孪晶。正确处理样品和数据将减少使用溶剂掩蔽软件（例如 SQUEEZE）来获得可接受的晶体结构的必要性。如果 SC-XRD 要保持其作为 MOF 结构确定的权威方法的地位，那么在确定和报告新的 MOF 结构时，就必须解决这些问题。本文综述中讨论的问题也适用于其他多孔晶体固体，如多孔有机笼、金属有机多面体、共价有机骨架和沸石型材料。
