3D 13C-NOESY (aliphatic and aromatic), 13C,1H-HSQC
1
3
2
4D 13C-separated NOESY
1
4
1
3D-TOCSYs
1
5
4
H/DEXCHANGE
1
6
3
3D 15N-NOESY, backbone TR experiments
1
7
1
high-resolution/non-constant-time 13C,1H-HSQC
NMR実験の詳細
Text: THE STRUCTURE WAS DETERMINED USING TRIPLE-RESONANCE NMR SPECTROSCOPY. AUTOMATIC BACKBONE RESONANCE ASSIGNMENTS WERE MADE USING AUTOASSIGN. MANUAL SIDE CHAIN ASSIGNMENTS. AUTOMATIC NOESY ...Text: THE STRUCTURE WAS DETERMINED USING TRIPLE-RESONANCE NMR SPECTROSCOPY. AUTOMATIC BACKBONE RESONANCE ASSIGNMENTS WERE MADE USING AUTOASSIGN. MANUAL SIDE CHAIN ASSIGNMENTS. AUTOMATIC NOESY ASSIGNMENTS AS WELL AS DISTANCE AND HYDROGEN BOND RESTRAINTS WERE DETERMINED USING AUTOSTRUCTURE. DIHEDRAL ANGLE RESTRAINTS WERE DETERMINED USING HYPER AND TALOS. BACKBONE DIHEDRAL ANGLES FOR RESIDUES 1, 13-20, 26-27, 39-40, 47-51, 54, 63-66 AND 73-79 ARE NOT WELL-DEFINED [S(PHI) + S(PSI) < 1.8] IN THIS SOLUTION NMR STRUCTURE.
-
試料調製
詳細
Solution-ID
内容
溶媒系
1
1.07 MM PfR48 U-15N,13C 20 MM MES, 100 MM NACL, 5 MM CACL2, 10 MM DTT, 0.02% NAN3, PH 6.5
95% H2O/5% D2O
2
1.07 MM PfR48 U-15N,13C 20 MM MES, 100 MM NACL, 5 MM CACL2, 10 MM DTT, 0.02% NAN3, PH 6.5
100% D2O
3
0.1 MM PfR48 U-15N,5%-13C 20 MM MES, 100 MM NACL, 5 MM CACL2, 10 MM DTT, 0.02% NAN3, PH 6.5
95% H2O/5% D2O
4
0.5 MM PfR48 U-15N 20 MM MES, 100 MM NACL, 5 MM CACL2, 10 MM DTT, 0.02% NAN3, PH 6.5
95% H2O/5% D2O
試料状態
イオン強度: 100 mM / pH: 6.5 / 圧: ambient / 温度: 293 K
-
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
800
1
Varian INOVA
Varian
INOVA
750
2
Varian INOVA
Varian
INOVA
600
3
Varian UNITY
Varian
UNITY
600
4
-
解析
NMR software
名称
バージョン
開発者
分類
X-PLOR
NIH2.0.6
Schwieters, etal.
精密化
VNMR
6.1B
Varian
collection
NMRPipe
2.1
Delaglio, etal.
解析
Sparky
3.106
Goddard
データ解析
PdbStat
3.32
TejeroandMontelione
構造決定
AutoStructure
2.0.0
HuangandMontelione
精密化
HYPER
3.2
TejeroandMontelione
構造決定
AutoAssign
1.9
Zimmerman, MoseleyandMontelione
データ解析
TALOS
2.1
Cornilescu, DelaglioandBax
構造決定
精密化
手法: simulated annealing / ソフトェア番号: 1 詳細: THE STRUCTURES ARE BASED ON A TOTAL OF 1157 CONFORMATIONALLY-RESTRICTING NOE-DERIVED DISTANCE RESTRAINTS, 177 DIHEDRAL ANGLE RESTRAINTS, AND 32 HYDROGEN BOND RESTRAINTS. (14.4 CONSTRAINTS PER ...詳細: THE STRUCTURES ARE BASED ON A TOTAL OF 1157 CONFORMATIONALLY-RESTRICTING NOE-DERIVED DISTANCE RESTRAINTS, 177 DIHEDRAL ANGLE RESTRAINTS, AND 32 HYDROGEN BOND RESTRAINTS. (14.4 CONSTRAINTS PER RESIDUE; 6.1 LONG-RANGE RESTRAINTS PER RESIDUE). STRUCTURE DETERMINATION WAS PERFORMED ITERATIVELY USING AUTOSTRUCTURE (XPLOR). THE UNSTRUCTURED 8 RESIDUE C-TERMINAL TAG (LEHHHHHH) WAS INCLUDED IN THE STRUCTURE CALCULATIONS BUT IS OMITTED FROM THIS DEPOSITION.
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: 56 / 登録したコンフォーマーの数: 10