High-Field and High-Speed CP-MAS13C NMR Heteronuclear Dipolar-Correlation Spectroscopy of Solids with Frequency-Switched Lee–Goldburg Homonuclear Decoupling

Rossum, Barth van; Förster, Hans; Groot, Huub J. M. de

doi:10.1006/jmre.1996.1089

Cited by 430 publications

(380 citation statements)

References 17 publications

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“…The lipid methylenic 13 C is clearly resolved at 28.7 ppm (7,12). The associated phospholipid methylenic proton response at 2.7 ppm was used to calculate a Lee Goldburg scaling factor of 0.610, which is in line with the theoretical value of 1͞√3 ϭ 0.577 (25).…”

Section: Methodssupporting

confidence: 60%

¹ H and ¹³ C MAS NMR evidence for pronounced ligand–protein interactions involving the ionone ring of the retinylidene chromophore in rhodopsin

Creemers

Kiihne

Bovée-Geurts

et al. 2002

Proc. Natl. Acad. Sci. U.S.A.

119

184

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Rhodopsin is a member of the superfamily of G-protein-coupled receptors. This seven ␣-helix transmembrane protein is the visual pigment of the vertebrate rod photoreceptor cells that mediate dim light vision. In the active binding site of this protein the ligand or chromophore, 11-cis-retinal, is covalently bound via a protonated Schiff base to lysine residue 296. Here we present the complete 1 H and 13 C assignments of the 11-cis-retinylidene chromophore in its ligand-binding site determined with ultra high field magic angle spinning NMR. Native bovine opsin was regenerated with 99% enriched uniformly 13 C-labeled 11-cis-retinal. From the labeled pigment, 13 C carbon chemical shifts could be obtained by using two-dimensional radio frequency-driven dipolar recoupling in a solid-state magic angle spinning homonuclear correlation experiment.

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Section: Methodssupporting

confidence: 60%

¹ H and ¹³ C MAS NMR evidence for pronounced ligand–protein interactions involving the ionone ring of the retinylidene chromophore in rhodopsin

Creemers

Kiihne

Bovée-Geurts

et al. 2002

Proc. Natl. Acad. Sci. U.S.A.

119

184

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“…For the assignment of the 1 H shifts, the FSLG technique was applied to solid samples of chlorins 1 and 2 (16). Fig.…”

Section: Resultsmentioning

confidence: 99%

“…Two-dimensional 1 H-13 C heteronuclear correlation datasets were obtained by using the frequency-switched Lee-Goldburg (FSLG) experiment, by using a short CP time of 256 s and a 1 H 90°pulse of 3.1 s (16). The 1 H chemical shift scale was calibrated from a FSLG spectrum of solid tyrosine⅐HCl salt (16). For each of 256 steps in the indirect 1 H dimension, 1536 13 C scans were accumulated.…”

Section: Methodsmentioning

confidence: 99%

Zinc chlorins for artificial light-harvesting self-assemble into antiparallel stacks forming a microcrystalline solid-state material

Ganapathy¹,

Sengupta²,

Wawrzyniak³

et al. 2009

Proc. Natl. Acad. Sci. U.S.A.

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We introduce a concept to solve the structure of a microcrystalline material in the solid-state at natural abundance without access to distance constraints, using magic angle spinning (MAS) NMR spectroscopy in conjunction with X-ray powder diffraction and DFT calculations. The method is applied to a novel class of materials that form (semi)conductive 1D wires for supramolecular electronics and artificial light-harvesting. The zinc chlorins 3-devinyl-3 1 -hydroxymethyl-13 2 -demethoxycarbonylpheophorbide a (3 ,5 -bisdodecyloxy)benzyl ester zinc complex 1 and 3-devinyl-3 1 -methoxymethyl-13 2 -demethoxycarbonylpheophorbide a (3 ,5 -bis-dodecyloxy)benzyl ester zinc complex 2, self-assemble into extended excitonically coupled chromophore stacks. 1 H-13 C heteronuclear dipolar correlation MAS NMR experiments provided the 1 H resonance assignment of the chlorin rings that allowed accurate probing of ring currents related to the stacking of macrocycles. DFT ring-current shift calculations revealed that both chlorins selfassemble in antiparallel -stacks in planar layers in the solid-state. Concomitantly, X-ray powder diffraction measurements for chlorin 2 at 80°C revealed a 3D lattice for the mesoscale packing that matches molecular mechanics optimized aggregate models. For chlorin 2 the stacks alternate with a periodicity of 0.68 nm and a 3D unit cell with an approximate volume of 6.28 nm 3 containing 4 molecules, which is consistent with space group P2 1221. artificial antenna ͉ density functional theory ͉ microcrystalline structure ͉ solid state NMR ͉ X-ray diffraction

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“…The 2D H} frequency-switched Lee-Goldburg heteronuclear correlation (FSLG-HETCOR) experiment [17] used a MAS frequency of 15.0 kHz, a recycle delay of 2 s, a cross polarization (CP) contact time of 3.0 ms and 1,152 scans for a total of 36 t 1 increments. Each t 1 increment had a span of five basic FSLG [18] blocks (81.6 μs).…”

Section: Methodsmentioning

confidence: 99%

Solid-State Organization and Ambipolar Field-Effect Transistors of Benzothiadiazole-Cyclopentadithiophene Copolymer with Long Branched Alkyl Side Chains

et al. 2013

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Abstract:The solid-state organization of a benzothiadiazole-cyclopentadithiophene copolymer with long, branched decyl-tetradecyl side chains (CDT-BTZ-C14,10) is investigated. The C14,10 substituents are sterically demanding and increase the π-stacking distance to 0.40 nm from 0.37 nm for the same polymer with linear hexadecyls (C16). Despite the bulkiness, the C14,10 side chains tend to crystallize, leading to a small chain-to-chain distance between lamellae stacks and to a crystal-like microstructure in the thin film. Interestingly, field-effect transistors based on solution processed layers of CDT-BTZ-C14,10 show ambipolar behavior in contrast to CDT-BTZ-C16 with linear side chains, for which hole transport was previously observed. Due to the increased π-stacking distance, the mobilities are only 6 × 10

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High-Field and High-Speed CP-MAS13C NMR Heteronuclear Dipolar-Correlation Spectroscopy of Solids with Frequency-Switched Lee–Goldburg Homonuclear Decoupling

Cited by 430 publications

References 17 publications

¹ H and ¹³ C MAS NMR evidence for pronounced ligand–protein interactions involving the ionone ring of the retinylidene chromophore in rhodopsin

¹ H and ¹³ C MAS NMR evidence for pronounced ligand–protein interactions involving the ionone ring of the retinylidene chromophore in rhodopsin

Zinc chlorins for artificial light-harvesting self-assemble into antiparallel stacks forming a microcrystalline solid-state material

Solid-State Organization and Ambipolar Field-Effect Transistors of Benzothiadiazole-Cyclopentadithiophene Copolymer with Long Branched Alkyl Side Chains

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High-Field and High-Speed CP-MAS13C NMR Heteronuclear Dipolar-Correlation Spectroscopy of Solids with Frequency-Switched Lee–Goldburg Homonuclear Decoupling

Cited by 430 publications

References 17 publications

1 H and 13 C MAS NMR evidence for pronounced ligand–protein interactions involving the ionone ring of the retinylidene chromophore in rhodopsin

1 H and 13 C MAS NMR evidence for pronounced ligand–protein interactions involving the ionone ring of the retinylidene chromophore in rhodopsin

Zinc chlorins for artificial light-harvesting self-assemble into antiparallel stacks forming a microcrystalline solid-state material

Solid-State Organization and Ambipolar Field-Effect Transistors of Benzothiadiazole-Cyclopentadithiophene Copolymer with Long Branched Alkyl Side Chains

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¹ H and ¹³ C MAS NMR evidence for pronounced ligand–protein interactions involving the ionone ring of the retinylidene chromophore in rhodopsin

¹ H and ¹³ C MAS NMR evidence for pronounced ligand–protein interactions involving the ionone ring of the retinylidene chromophore in rhodopsin