Single-crystal x-ray diffraction structures of covalent organic frameworks

Tianqiong Ma; Eugene A Kapustin; Shawn X Yin; Lin Liang; Zhengyang Zhou; Jing Niu; Li-Hua Li; Yingying Wang; Jie Su; Jian Li; Xiaoge Wang; Wei David Wang; Wei Wang; Junliang Sun; Omar M Yaghi

doi:10.1126/science.aat7679

Single-crystal x-ray diffraction structures of covalent organic frameworks

Science. 2018 Jul 6;361(6397):48-52. doi: 10.1126/science.aat7679.

Authors

Tianqiong Ma^{1

2}, Eugene A Kapustin³, Shawn X Yin⁴, Lin Liang¹, Zhengyang Zhou², Jing Niu¹, Li-Hua Li¹, Yingying Wang¹, Jie Su², Jian Li², Xiaoge Wang², Wei David Wang¹, Wei Wang^{5

6}, Junliang Sun⁷, Omar M Yaghi^{8

9}

Affiliations

¹ State Key Laboratory of Applied Organic Chemistry, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou, Gansu 730000, China.
² College of Chemistry and Molecular Engineering, Beijing National Laboratory for Molecular Sciences, Peking University, Beijing 100871, China.
³ Department of Chemistry, University of California-Berkeley; Materials Sciences Division, Lawrence Berkeley National Laboratory; Kavli Energy NanoSciences Institute at Berkeley; Berkeley Global Science Institute, Berkeley, CA 94720, USA.
⁴ Drug Product Science & Technology, Bristol-Myers Squibb Co., One Squibb Drive, New Brunswick, NJ 08903, USA.
⁵ State Key Laboratory of Applied Organic Chemistry, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou, Gansu 730000, China. wang_wei@lzu.edu.cn junliang.sun@pku.edu.cn yaghi@berkeley.edu.
⁶ Collaborative Innovation Center of Chemical Science and Engineering, Tianjin 300071, China.
⁷ College of Chemistry and Molecular Engineering, Beijing National Laboratory for Molecular Sciences, Peking University, Beijing 100871, China. wang_wei@lzu.edu.cn junliang.sun@pku.edu.cn yaghi@berkeley.edu.
⁸ Department of Chemistry, University of California-Berkeley; Materials Sciences Division, Lawrence Berkeley National Laboratory; Kavli Energy NanoSciences Institute at Berkeley; Berkeley Global Science Institute, Berkeley, CA 94720, USA. wang_wei@lzu.edu.cn junliang.sun@pku.edu.cn yaghi@berkeley.edu.
⁹ King Abdulaziz City for Science and Technology, Riyadh 11442, Saudi Arabia.

PMID: 29976818
DOI: 10.1126/science.aat7679

Abstract

The crystallization problem is an outstanding challenge in the chemistry of porous covalent organic frameworks (COFs). Their structural characterization has been limited to modeling and solutions based on powder x-ray or electron diffraction data. Single crystals of COFs amenable to x-ray diffraction characterization have not been reported. Here, we developed a general procedure to grow large single crystals of three-dimensional imine-based COFs (COF-300, hydrated form of COF-300, COF-303, LZU-79, and LZU-111). The high quality of the crystals allowed collection of single-crystal x-ray diffraction data of up to 0.83-angstrom resolution, leading to unambiguous solution and precise anisotropic refinement. Characteristics such as degree of interpenetration, arrangement of water guests, the reversed imine connectivity, linker disorder, and uncommon topology were deciphered with atomic precision-aspects impossible to determine without single crystals.

Publication types

Research Support, Non-U.S. Gov't
Research Support, U.S. Gov't, Non-P.H.S.