SOLUTION NMR
NMR Experiment | ||||||||
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Experiment | Type | Sample Contents | Solvent | Ionic Strength | pH | Pressure | Temperature (K) | Spectrometer |
1 | 2D_COSY | 2.5 mM calbindin; 95% H2O; 5% D2O | 95% H20; 5% D2O | no added salts | 6.0 | ambient | 300 | |
2 | 2D_NOESY | 2.5 mM calbindin; 95% H2O; 5% D2O | 95% H20; 5% D2O | no added salts | 6.0 | ambient | 300 | |
3 | 2D_TOCSY | 2.5 mM calbindin; 95% H2O; 5% D2O | 95% H20; 5% D2O | no added salts | 6.0 | ambient | 300 | |
4 | 2D_NOESY | 2.5 mM calbindin D9k; 100% D20 | 100% D2O | no added salts | 6.0 | ambient | 300 | |
5 | 2D_15N-1H_HSQC | 2.5 mM calbindin D9k U-15N; 95% H2O; 5% D2O | 95% H2O/5% D2O | no added salts | 6.0 | ambient | 300 | |
6 | 3D_15N-separated_TOCSY | 2.5 mM calbindin D9k U-15N; 95% H2O; 5% D2O | 95% H2O/5% D2O | no added salts | 6.0 | ambient | 300 | |
7 | 3D_15N-separated_NOESY | 2.5 mM calbindin D9k U-15N; 95% H2O; 5% D2O | 95% H2O/5% D2O | no added salts | 6.0 | ambient | 300 | |
8 | HNHA | 2.5 mM calbindin D9k U-15N; 95% H2O; 5% D2O | 95% H2O/5% D2O | no added salts | 6.0 | ambient | 300 | |
9 | HNHB | 2.5 mM calbindin D9k U-15N; 95% H2O; 5% D2O | 95% H2O/5% D2O | no added salts | 6.0 | ambient | 300 |
NMR Spectrometer Information | |||
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Spectrometer | Manufacturer | Model | Field Strength |
1 | Bruker | AMX | 500 |
2 | Bruker | DMX | 750 |
NMR Refinement | ||
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Method | Details | Software |
distance geometry, simulated annealing | The structures are based on 1042 NOE restraints (186 intraresidue, 269 sequential, 289 medium range (2-4 residues apart), 298 long range), 18 hydrogen bond restraints (assigned as described in Skelton et al., 1995), and 115 dihedral constraints (45 phi, 42 psi, and 28 chi1). | DIANA |
NMR Ensemble Information | |
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Conformer Selection Criteria | The full ensemble was ordered by lowest residual constraint violations, then the top 22 with favorable covalent geometries and AMBER energies were selected |
Conformers Calculated Total Number | 50 |
Conformers Submitted Total Number | 22 |
Representative Model | 1 (closest to the average) |
Additional NMR Experimental Information | |
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Details | This structure was determined using a combination of standard 2D homonuclear and 15N-based 3D methods. |
Computation: NMR Software | ||||
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# | Classification | Version | Software Name | Author |
1 | structure solution | DIANA | 2.8 | Guntert |
2 | structure solution | Amber | 4.1 | Pearlmann |
3 | data analysis | Felix | 97 | Molecular Simulations, Inc. |
4 | data analysis | GLOMSA | unknown | Guntert |
5 | data analysis | GENXPK | 1 | Gippert |
6 | refinement | Amber | 4.1 | Pearlmann |