SOLUTION NMR
NMR Experiment | ||||||||
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Experiment | Type | Sample Contents | Solvent | Ionic Strength | pH | Pressure | Temperature (K) | Spectrometer |
1 | 3D_15N-separated_NOESY | 1.1 mM ThKaiA180C U-15N, 1.1 mM CIIABD, 20 mM NaCl, 20 mM Na2HPO4 pH 7.07 at 296K | 95% H2O/5% D2O | 20 mM NaCl, 20 mM NaPi | 7.0 | ambient | 323 | |
2 | 4D_13C-separated_NOESY | 1.1 mM ThKaiA180C U-15N,13C, 1.1 mM CIIABD, 20 mM NaCl, 20 mM Na2HPO4 pH 7.07 at 296K | 100% D2O | 20 mM NaCl, 20 mM NaPi | 7.0 | ambient | 323 | |
3 | 13C-edited/12C-filtered 3D NOESY | 1.1 mM ThKaiA180C U-15N,13C, 1.1 mM CIIABD, 20 mM NaCl, 20 mM Na2HPO4 pH 7.07 at 296K | 100% D2O | 20 mM NaCl, 20 mM NaPi | 7.0 | ambient | 323 | |
4 | 3D_13C-separated_NOESY | 1.2 mM ThKaiA180C, 1.2 mM CIIABD U-15N,13C, 20 mM NaCl, 20 mM Na2HPO4 pH 7.07 at 296K | 100% D2O | 20 mM NaCl, 20 mM NaPi | 7.0 | ambient | 323 | |
5 | 13C-edited/12C-filtered 3D NOESY | 0.8 mM ThKaiA180C U-15N,13C, 0.8 mM ThKaiA180C, 1.6 mM CIIABD U-15N,13C, 20 mM NaCl, 20 mM Na2HPO4 pH 7.07 at 296K | 100% D2O | 20 mM NaCl, 20 mM NaPi | 7.0 | ambient | 323 |
NMR Spectrometer Information | |||
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Spectrometer | Manufacturer | Model | Field Strength |
1 | Varian | INOVA | 600 |
2 | Varian | INOVA | 500 |
NMR Refinement | ||
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Method | Details | Software |
Distance geometry, Simulated annealing | The structure is based on 2420 total restraints: 1858 are NOE derived, 58 are from hydrogen bonds, 244 are dihedral angles and 260 are 13C chemical shifts. | VNMR |
NMR Ensemble Information | |
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Conformer Selection Criteria | lowest energy structures that satisfy all experimental restraints |
Conformers Calculated Total Number | 50 |
Conformers Submitted Total Number | 25 |
Representative Model | 11 (lowest energy) |
Additional NMR Experimental Information | |
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Details | Assignments of ThKaiA180C and CIIABD were performed through CBCA(CO)NH, CBCANH, HBHA(CO)NH and HC(C)H-COSY experiments. |
Computation: NMR Software | ||||
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# | Classification | Version | Software Name | Author |
1 | collection | VNMR | 6.1 Rev. C | |
2 | processing | NMRPipe | 2.1 Rev. 2002.044.17.08 | |
3 | data analysis | PIPP | 4.2.6 | |
4 | structure solution | XPLOR-NIH | 2.9.1 | |
5 | refinement | XPLOR-NIH | 2.9.1 |