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Crystal Structure Solution of Radiation-Sensitive Porous Framework CL30 by Low-Dose Cryo 3D Electron Diffraction 认领 引用
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作者 Ke Wang Dapeng Sun +5 位作者 Penghe Li Zhiyuan Mao Yi Luo Hongxia Wang Hongyi Xu Yumei Wang 《Chinese Physics Letters》 SCIE EI CAS CSCD 2026年第3期294-299,共6页
To overcome the limitations of traditional single-crystal X-ray diffraction(SCXRD)for microcrystalline materials and the peak-overlapping issue of powder X-ray diffraction(PXRD),this study employed cryogenic continuou... To overcome the limitations of traditional single-crystal X-ray diffraction(SCXRD)for microcrystalline materials and the peak-overlapping issue of powder X-ray diffraction(PXRD),this study employed cryogenic continuous rotation electron diffraction(cryo-cRED)with a low-dose strategy to determine the crystal structure of CL30,a novel silicogermanate framework.It is confirmed that CL30 crystallizes in the C2/m space group and has layered topology composed of discontinuous zigzag chains connected by double four-membered ring(d4r)units,with fluoride anions(F-)occluded in the d4r units.In CL30,charge balance involves organic structure-directing agent(OSDA)cations,occluded F-,and terminal oxygen sites whose protonation state cannot be established from the present three dimensional(3D)ED data.F-encapsulated in the d4r units contributes to charge compensation as the counter-anion to OSDA cations,rather than only balancing the framework charge.Although the refinement indices(R1=0.29,wR2=0.71)exceeded typical small-molecule crystallography standards,the structural model remained highly reliable,as supported by geometric restraints and validation.In electron diffraction,elevated R1 values are commonly attributed to the intrinsic factors of the technique,such as dynamic scattering,detector noise from scintillator-based detectors,and TEM stage instability(large spheres of confusion).This study introduces a new structural prototype to the silicogermanate family and establishes a feasible workflow for determining the structures of radiation-sensitive microcrystalline porous materials. 展开更多
关键词 discontinuous zigzag chains low dose cryo d electron diffraction c m space group crystal structure radiation sensitive porous framework silicogermanate layered topology silicogermanate frameworkit
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