Text: Distance restraints were derived from 15N- or 13C-resolved 3D NOESY. HN-N residual dipolar couplings were measured using a spin-state-selective 1H,15N correlation experiment in dilute liquid ...Text: Distance restraints were derived from 15N- or 13C-resolved 3D NOESY. HN-N residual dipolar couplings were measured using a spin-state-selective 1H,15N correlation experiment in dilute liquid crystalline medium. Restraints for the backbone angles phi and psi were derived from TALOS. Stereospecific assignments of Leu, Val methyl groups were obtained using a 10% fractionally 13C-labelled sample.
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試料調製
詳細
Solution-ID
内容
溶媒系
1
0.2 - 1 mM 15N, 13C/15N or 2H/13C/15N labelled B2 protein in 50 mM sodium phosphate pH 6.3, 50 mM sodium chloride, 1 mM DTT, 90% H2O / 10% D2O
90% H2O/10% D2O
2
0.2 - 1 mM 13C/15N labelled B2 protein in 50 mM sodium phosphate pH 6.3, 50 mM sodium chloride, 1 mM DTT, 100% D2O
100% D2O
試料状態
イオン強度: 50 mM NaPi, 50 mM NaCl / pH: 6.3 / 圧: 1 atm / 温度: 295 K
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NMR測定
放射
プロトコル: SINGLE WAVELENGTH / 単色(M)・ラウエ(L): M
放射波長
相対比: 1
NMRスペクトロメーター
タイプ
製造業者
モデル
磁場強度 (MHz)
Spectrometer-ID
Bruker DRX
Bruker
DRX
500
1
Bruker DRX
Bruker
DRX
600
2
Bruker DRX
Bruker
DRX
900
3
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解析
NMR software
名称
バージョン
開発者
分類
XwinNMR
3.5
collection
NMRPipe
Delaglioetal.
解析
NMRView
5
Johnsonetal.
データ解析
TALOS
Cornilescuetal.
データ解析
ARIA
1.2
Lingeetal.
構造決定
CNS
1.1
Brungeretal.
構造決定
CNS
1.1
Brungeretal.
精密化
精密化
手法: molecular dynamics, simulated annealing / ソフトェア番号: 1 詳細: The experimentally determined distance, dihedral and dipolar coupling restraints were applied in a simulated annealing protocol using ARIA and CNS. Non-crystallographic symmetry (NCS) ...詳細: The experimentally determined distance, dihedral and dipolar coupling restraints were applied in a simulated annealing protocol using ARIA and CNS. Non-crystallographic symmetry (NCS) restraints were used to enforce the dimer symmetry. The final ensemble of NMR structures was refined in a shell of water molecules.
代表構造
選択基準: lowest energy
NMRアンサンブル
コンフォーマー選択の基準: structures with the lowest energy 計算したコンフォーマーの数: 100 / 登録したコンフォーマーの数: 10