Solid-state NMR spectroscopy at ultrahigh resolution for structural and dynamical studies of MOFs

作     者：Qing Wang Min Peng Cong-Cong Liang Jing Tan Sophia Zhang Yue-Biao Zhang Haiming Liu Qing Wang;Min Peng;Cong-Cong Liang;Jing Tan;Sophia Zhang;Yue-Biao Zhang;Haiming Liu

作者机构：School of Physical Science and TechnologyShanghaiTech UniversityShanghai201210China Maling Middle SchoolSuqianJiangsu223800China Washington University in St.LouisSt.LouisMO63130USA 

出 版 物：《Magnetic Resonance Letters》 (磁共振快报（英文）)

年 卷 期：2023年第3卷第2期

页      面：175-186,I0005页

核心收录：

学科分类：081704[工学-应用化学] 07[理学] 070304[理学-物理化学(含∶化学物理)] 08[工学] 0817[工学-化学工程与技术] 0703[理学-化学] 

基　　金：supported by the start-up fund(2017F0201-000-10)from ShanghaiTech University the sponsorship by Double First-Class Initiative Fund of ShanghaiTech University(SYLDX0052022) the support from the Analytical Instrumentation Center(SPSTAIC10112914)at ShanghaiTech University 

主　　题：Solid-state NMR Ultrahigh resolution MOFs Structure and dynamics Magic angle calibration 

摘      要：To characterize the structure and dynamics of metal--organic frameworks(MOFs)indepth at the molecular level,it is necessary to pursue high-resolution solid-state magic angle spinning(MAS)nuclear magnetic resonance(NMR)*** resolution is usually affected by the quality of materials and various experimental conditions,of which magic angle(MA)accuracy is a crucial *** current industrial criteria for MA calibration based on the common standard of KBr were found insufficient in guaranteeing optimal resolution MAS NMR for highly ordered *** drive towards higher-resolution MAS NMR spectroscopy,we propose_a calibration protocol for more accurate MA with a higher-precision criterion based on 79Br MAS NMR of KBr,where the linewidth ratio of the fifth-order spinning sideband to the central band of KBr should be less than *** a result,ultrahigh-resolution 13C cross-polarization(CP)MAS NMR of MOF-5 is achieved with minimal linewidths as low as 4 Hz,and therefore MOF-5 can be used as a new standard convenient for verifying MA accuracy and also optimizing 13c CP *** high-precision MA under variable temperature(VT)was found challenging on certain commercial MAS NMR probes,as was systematically investigated by VT NMR using KBr and ***,ultrahigh-resolution MAS NMR spectroscopy with stable MA under VT is employed to reveal fine structures and linker dynamics of a series of Zn-based MOFs with highly regulated *** ultrahigh-resolution NMR methodcan be generally applied to study a broad range of MOFs and other materials.