Constant-time 2D and 3D through-bond correlation NMR spectroscopy of solids under 60 kHz MAS
作者： Rongchun Zhang , Ayyalusamy Ramamoorthy
DOI: 10.1063/1.4940029
关键词:
摘要: Establishing connectivity and proximity of nuclei is an important step in elucidating the structure dynamics molecules solids using magic angle spinning (MAS) NMR spectroscopy. Although recent studies have successfully demonstrated feasibility proton-detected multidimensional solid-state experiments under ultrafast-MAS frequencies obtaining high-resolution spectral lines protons, assignment proton resonances a major challenge. In this study, we first re-visit demonstrate 2D constant-time uniform-sign cross-peak correlation (CTUC-COSY) experiment on rigid conditions, where sensitivity enhanced by reduced spin-spin relaxation rate use low radio-frequency power for heteronuclear decoupling during evolution intervals pulse sequence. addition, experimentally performance sequence to obtain 3D (1)H/(13)C/(1)H chemical shift spectrum incorporating additional cross-polarization period CTUC-COSY enable detection incrementable t1 t3 periods, respectively. addition through-space through-bond (13)C/(1)H (13)C/(13)C correlations, also provides COSY-type (1)H/(1)H spectrum, only shifts those which are bonded two neighboring carbons, correlated. By extracting F1/F3 slices ((1)H/(1)H spectrum) at different (13)C from atoms located close specific carbon atom can be identified. Overall, homonuclear/heteronuclear proximities determined would useful study variety biological solids.
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