1M8M
SOLID-STATE MAS NMR STRUCTURE OF THE A-SPECTRIN SH3 DOMAIN
SOLID-STATE NMR
| NMR Experiment | ||||||||
|---|---|---|---|---|---|---|---|---|
| Experiment | Type | Sample Contents | Solvent | Ionic Strength | pH | Pressure | Temperature (K) | Spectrometer |
| 1 | 13C-13C PROTON-DRIVEN SPIN- DIFFUSION (PDSD) | A 200 MM (NH4)2SO4 SOLUTION WAS ADDED TO A 1.15 MM SH3 SOLUTION (PH=3.5) AT A VOLUME RATIO 1:1. THE SOLID SAMPLE WAS OBTAINED BY PRECIPITATION, CHANGING THE PH TO 7.5 IN NH3 ATMOSPHERE. | SOLID SAMPLE | 7.5 | AMBIENT | 280 | ||
| 2 | 15N-15N PROTON-DRIVEN SPIN-DIFFUSION (PDSD) | A 200 MM (NH4)2SO4 SOLUTION WAS ADDED TO A 1.15 MM SH3 SOLUTION (PH=3.5) AT A VOLUME RATIO 1:1. THE SOLID SAMPLE WAS OBTAINED BY PRECIPITATION, CHANGING THE PH TO 7.5 IN NH3 ATMOSPHERE. | SOLID SAMPLE | 7.5 | AMBIENT | 280 | ||
| NMR Spectrometer Information | |||
|---|---|---|---|
| Spectrometer | Manufacturer | Model | Field Strength |
| 1 | Bruker | DMX | 750 |
| NMR Refinement | ||
|---|---|---|
| Method | Details | Software |
| SIMULATED ANNEALING, TORSION ANGLE DYNAMICS | THE STRUCTURES ARE BASED ON A TOTAL OF 286 13C-13C RESTRAINTS AND 6 15N-15N RESTRAINTS. ALL RESTRAINTS ARE EXTRACTED FROM PDSD SPECTRA. | CNS |
| NMR Ensemble Information | |
|---|---|
| Conformer Selection Criteria | structures with the lowest energy |
| Conformers Calculated Total Number | 200 |
| Conformers Submitted Total Number | 12 |
| Representative Model | 1 (lowest energy) |
| Additional NMR Experimental Information | |
|---|---|
| Details | THIS SOLID-STATE NMR STRUCTURE WAS DETERMINED BY COMBINING BROAD-BAND RECOUPLING METHODS WITH DILUTION OF THE 13C SPINS |
| Computation: NMR Software | ||||
|---|---|---|---|---|
| # | Classification | Version | Software Name | Author |
| 1 | refinement | CNS | 1.0 | BRUENGER ET AL. |
| 2 | structure solution | XwinNMR | 2.6 | |
| 3 | structure solution | Sparky | 3.1 | |
| 4 | structure solution | CNS | 1.0 | |
