Yue-Biao Zhang,# Jie Su,# Hiroyasu Furukawa, Yifeng Yun, Felipe Gándara, Adam Doung, Xiaodong Zou,* Omar M. Yaghi,*
J. Am. Chem. Soc. 2013, 135, 16336‒16339.
The crystal structure of a new covalent organic framework, termed COF-320, is determined by single-crystal 3D electron diffraction using the rotation electron diffraction (RED) method for data collection. The COF crystals are prepared by an imine condensation of tetra-(4-anilyl)methane and 4,4′-biphenyldialdehyde in 1,4-dioxane at 120 °C to produce a highly porous 9-fold interwoven diamond net. COF-320 exhibits permanent porosity with a Langmuir surface area of 2400 m2/g and a methane total uptake of 15.0 wt % (176 cm3/cm3) at 25 °C and 80 bar. The successful determination of the structure of COF-320 directly from single-crystal samples is an important advance in the development of COF chemistry.