Text: The structure was determined using triple-resonance 3D NMR spectroscopy for resonance assignments and double-resonance 3D NMR spectroscopy for obtaining NOESY data.
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試料調製
詳細
Solution-ID
内容
溶媒系
1
0.002 M gamma delta resolvase (1-105) U-15N; 0.020 M phosphate buffer, pH 6.5; 90% H2O, 10% D2O
90% H2O/10% D2O
2
0.002 M gamma delta resolvase (1-105) U-15N,13C; 0.020 M phosphate buffer, pH 6.5; 90% H2O, 10% D2O
90% H2O/10% D2O
3
0.002 M gamma delta resolvase (1-105) U-15N,13C; 0.020 M phosphate buffer, pH 6.5; 99% D2O
99% D2O
試料状態
イオン強度: 1M / pH: 6.5 / 圧: 1 atm / 温度: 298 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
Varian INOVA
Varian
INOVA
600
1
Varian INOVA
Varian
INOVA
500
2
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解析
NMR software
名称
バージョン
開発者
分類
VNMR
6.1
Varian
collection
NMRPipe
1.7
Delaglio
解析
XEASY
1.3.13
XiaandBartels
データ解析
DYANA
1.5
Guentert
構造決定
XPLOR
4
Brunger
精密化
精密化
手法: torsion angle dynamics, simulated annealing / ソフトェア番号: 1 詳細: The NMR restraints included 2109 useful NOE determined upper distance restraints, 35 hydrogen bonds, and 297 torsion angle restraints. Structures were calculated in the DYANA using torsion ...詳細: The NMR restraints included 2109 useful NOE determined upper distance restraints, 35 hydrogen bonds, and 297 torsion angle restraints. Structures were calculated in the DYANA using torsion angle dynamics. The calculation started with 200 randomized structures. The 19 structures with the lowest target function were refined within XPLOR using simulated annealing. The 19 refined structural conformers displayed no NOE violations >0.3 angstroms and no dihedral angle violations >3 degrees.
NMRアンサンブル
コンフォーマー選択の基準: lowest energy and agreement with experimental NOESY 計算したコンフォーマーの数: 200 / 登録したコンフォーマーの数: 19