Structure of bhpBR3, the BAFF-binding loop of BR3 embedded in a beta-hairpin peptide
SOLUTION NMR
NMR Experiment | ||||||||
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Experiment | Type | Sample Contents | Solvent | Ionic Strength | pH | Pressure | Temperature (K) | Spectrometer |
1 | 2D NOESY | 2.9 mM bhpBR3 peptide | 92% H2O, 8% D2O, 0.1 mM DSS, pH 4.5 | no added salt | 4.5 | ambient | 293 | |
2 | 2D TOCSY | 2.9 mM bhpBR3 peptide | 92% H2O, 8% D2O, 0.1 mM DSS, pH 4.5 | no added salt | 4.5 | ambient | 293 | |
3 | DQF-COSY | 2.9 mM bhpBR3 peptide | 92% H2O, 8% D2O, 0.1 mM DSS, pH 4.5 | no added salt | 4.5 | ambient | 293 | |
4 | 2D NOESY | 2.9 mM bhpBR3 peptide | 100% D2O, 0.1 mM DSS, pH 4.5 | no added salt | 4.5 | ambient | 293 | |
5 | COSY-35 | 2.9 mM bhpBR3 peptide | 100% D2O, 0.1 mM DSS, pH 4.5 | no added salt | 4.5 | ambient | 293 |
NMR Spectrometer Information | |||
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Spectrometer | Manufacturer | Model | Field Strength |
1 | Bruker | DRX | 600 |
NMR Refinement | ||
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Method | Details | Software |
hybrid distance geometry/simulated annealing followed by restrained molecular dynamics. | Complete 1H resonance assignments were obtained using standard 2D homonuclear NMR methods. Distance restraints were derived from analysis of a 2D NOESY spectrum (250ms mixing time); HN-Ha coupling constants were obtained from analysis of a DQF-COSY spectrum acquired in water; and HaHb values were obtained from analysis of a COSY-35 spectrum acquired in D2O. Structures were calculated from a total of 119 NOE-derived (including 46 long-range) distance restraints and 16 dihedral angle restraints. Structures satisfy the experimental data very well with no distance or dihedral angle violations greater than 0.1 angstrom or 1 degree, respectively. | XwinNMR |
NMR Ensemble Information | |
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Conformer Selection Criteria | structures with the least restraint violations |
Conformers Calculated Total Number | 80 |
Conformers Submitted Total Number | 20 |
Representative Model | 1 (closest to the average) |
Computation: NMR Software | ||||
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# | Classification | Version | Software Name | Author |
1 | collection | XwinNMR | 1.37.4.2 | Bruker |
2 | data analysis | Felix | 98.0 | Accelrys |
3 | structure solution | DGII | 98.0 | Accelrys |
4 | refinement | Discover | 98.0 | Accelrys |