We demonstrate that high-resolution multidimensional solid state NMR methods can be used to correlate many backbone and side chain chemical shifts for hydrated micro-crystalline U-13C,15N Basic Pancreatic Trypsin Inhibitor (BPTI), using a field strength of 800 MHz for protons, magic angle sample spinning rates of 20 kHz and proton decoupling field strengths of 140 kHz. Results from two homonucl...

A suite of novel (5,3)D G2FT triple resonance NMR experiments encoding highly resolved 5D spectral information is presented for sequential resonance assignment of proteins exhibiting high chemical shift degeneracy. Efficient resonance assignment is achieved by separate joint sampling of (i) chemical shifts which solely serve to provide increased resolution and (ii) shifts which also provide seq...

Reagents were obtained from commercial suppliers and used as received. Lipase preparation PSIm was purchased from Amano Enzyme Inc. The other lipases were purchased from Sigma-Aldrich. 1H-NMR and 13C-NMR data were recorded on a Bruker Avance 400 (100) MHz and/or a Bruker Avance 500 (125) MHz, respectively. Chemical shifts are reported as δ values (ppm) with CDCl3 (1H-NMR δ 7.26, 13C-NMR δ 77.16...

Information about chemical shift anisotropy is usually difficult to extract from the spectrum of a nonspinning powdered sample because of the usually extensive overlap of the powder patterns from the chemically different sites in the molecule. Several types of experiments have been proposed to facilitate the measurement of chemical shift anisotropy (1-9). All have the common feature that the sa...

In this work we present a systematic, theoretical investigation of the 13C NMR chemical shifts for several mono-, di- and trisaccharides in solid state. The have been calculated using density functional theory (DFT) together with gauge including projector augmented wave (GIPAW) method as implemented CASTEP program. We studied changes particular due to formation one or two glycosidic linkages cr...

The C-8-(S) isomer of deoxyloganic acid (7-deoxyloganic acid), together with beta-sitosteryl glucoside, five known stereoisomeric pentacyclic oxindole alkaloids and the tetracyclic oxindole isorhyncophylline, were isolated from the inner bark of Uncaria tomentosa. Structures of the isolated compounds were based on 1H and 13C NMR data, mainly 2D NMR experiments, including 1H-13C HMBC and 1H-1H N...

We describe a new experiment for measuring homonuclear-decoupled anisotropic chemical shift patterns in doubly 13C-labeled compounds under magic-angle spinning. The experiment combines a pair of selective and non-selective 180 degrees pulses to suppress the 13C-13C scalar and dipolar interactions. This is combined with the recently developed SUPER technique to recouple the chemical shift anisot...