β Scribed by Lingling Chen; J. Michael Kaiser; Jinfeng Lai; Tatyana Polenova; Jun Yang; Chad M. Rienstra; Leonard J. Mueller
No coin nor oath required. For personal study only.
Scalar-based two-dimensional heteronuclear experiments are reported for NCO and NCA chemical shift correlation in the solid state. In conjunction with homonuclear CACO correlation, these experiments form a useful set for tracing connectivities and assigning backbone resonances in solid-state proteins. The applicability of this approach is demonstrated on two proteins, the b 1 immunoglobulin binding domain of protein G at 9.4 T and reassembled thioredoxin at 14.1 T, using different decoupling conditions and MAS frequencies. These constant-time J-based correlation experiments exhibit increased resolution in the indirect dimension owing to homonuclear and heteronuclear decoupling, and because the indirect evolution and transfer periods are combined into a single constant time interval, this increased resolution is not obtained at the cost of sensitivity. These experiments are also shown to be compatible with in-phase anti-phase (IPAP) selection, giving increased resolution in the directly detected dimension.
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A variant of the solid-state wideline heteronuclear NMR correlation experiment is described which overcomes some of the drawbacks associated with the routine experiment. The modified experiment results in spectra which are sign-discriminated in the 1 dimension, but without the loss in sensitivity ex
A solid-state analogue of the double echo sequence and gated decoupling used previously for the determination of carbon multiplicities in liquids is described; it was applied to the simplification and assignment of "C CP-MAS spectra in solids. This procedure permits partially edited "C CP-MAS subspe
## Abstract We show that weak ^2^__J__(^71^Gaο£ΏOο£Ώ^31^P), typically βΌ12 Hz in GaPO~4~, can be used to efficiently establish heteronuclear ^31^Pο£Ώ^71^Ga correlation using a MAS HMQC experiment in galloβphosphate materials. The experiment demonstrated for cristobalite GaPO~4~ is then applied to Ga(PO~3~