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Asymmetric simultaneous phase-inversion cross-polarization in solid-state MAS NMR: Relaxing selective polarization transfer condition between two dilute spins

机译:固态MAS NMR中的不对称同时相反转交叉极化:两个稀疏自旋之间松弛的选择性极化转移条件

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摘要

Double cross polarization (DCP) has been widely used for heteronuclear polarization transfer between ~(13)C and ~(15)N in solid-state magic-angle spinning (MAS) NMR. However, DCP is such sensitive to experimental settings that small variations or deviations in RF fields would deteriorate its efficiency. Here, we report on asymmetric simultaneous phase-inversion cross polarization (referred as aSPICP) for selective polarization transfer between low-γ ~(13)C and ~(15)N spins. We have demonstrated through simulations and experiments using biological solids that the asymmetric duration in the simultaneous phase-inversion cross polarization scheme leads to efficient polarization transfer between ~(13)C and ~(15)N even with large chemical shift anisotropies in the presence of B_1 field variations or mismatch of the Hartmann-Hahn conditions. This could be very useful in the aspect of long-duration experiments for membrane protein studies at high fields.
机译:在固态魔术角旋转(MAS)NMR中,双交叉极化(DCP)已广泛用于〜(13)C和〜(15)N之间的异核极化转移。但是,DCP对实验设置非常敏感,以至于RF场中的微小变化或偏差都会降低其效率。在这里,我们报道了在低γ〜(13)C和〜(15)N自旋之间进行选择性极化转移的非对称同时反相反转极化(称为aSPICP)。通过使用生物固体的仿真和实验,我们证明了同时相反转交叉极化方案中的不对称持续时间会导致〜(13)C和〜(15)N之间的有效极化转移,即使存在较大的化学位移各向异性B_1场变化或Hartmann-Hahn条件不匹配。这对于在高场进行膜蛋白研究的长期实验而言可能非常有用。

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