3D 15N-NOESY, 3D 13C-NOESY (aliphatic and aromatic)
1
2
2
4D 13C-separated NOESY
1
3
1
HNHA
1
4
3
high resolution 13C,1H-HSQC
1
5
1
H/Dexchange
1
6
1
backboneTRexperiments, and3DTOCSYs
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 CONFORMATIONS FOR RESIDUES 1-3, 5-6, 18-20, 22-23, 34-35, 48-49, 57-71, ARE NOT WELL-DEFINED [S(PHI) + S(PSI) < 1.8] IN THIS SOLUTION NMR STRUCTURE.
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試料調製
詳細
Solution-ID
内容
溶媒系
1
1.0 MM JR19 U-15N,13C 20 mM MES, 100 mM NaCl, 5 mM CaCl2, 10 mM DTT, 0.02% NaN3, pH 6.5
5% D2O/95% H2O
2
1.0 MM JR19 U-15N,13C 20 mM MES, 100 mM NaCl, 5 mM CaCl2, 10 mM DTT, 0.02% NaN3, pH 6.5
D2O
3
1.0 MM JR19 U-15N, 5%-13C 20 mM MES, 100 mM NaCl, 5 mM CaCl2, 10 mM DTT, 0.02% NaN3, pH 6.5
5% D2O/95% H2O
試料状態
イオン強度: 100 mM NaCl / pH: 6.5 / 圧: ambient / 温度: 293 K
結晶化
*PLUS
手法: other / 詳細: NMR
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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
800
1
Varian INOVA
Varian
INOVA
750
2
Varian INOVA
Varian
INOVA
750
3
Varian INOVA
Varian
INOVA
600
4
Varian INOVA
Varian
INOVA
500
5
Varian UNITY
Varian
UNITY
600
6
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解析
NMR software
名称
バージョン
開発者
分類
VNMR
6.1B
Varian
collection
NMRPipe
2.1
Delaglio
解析
Sparky
3.106
Goddard
データ解析
AutoAssign
1.9
Zimmerman, Moseley, Montelione
データ解析
AutoStructure
1.1.2
Huang, Montelione
精密化
HYPER
3.2
Tejero, Montelione
構造決定
DYANA
1.5
Guntert
精密化
PdbStat
3.27
Tejero, Montelione
構造決定
精密化
手法: torsion angle dynamics / ソフトェア番号: 1 詳細: THE STRUCTURES ARE BASED ON A TOTAL OF 828 CONFORMATIONALLY-RESTRICTING NOE-DERIVED DISTANCE RESTRAINTS, 99 DIHEDRAL ANGLE RESTRAINTS, AND 28 HYDROGEN BOND RESTRAINTS. (13.5 CONSTRAINTS PER ...詳細: THE STRUCTURES ARE BASED ON A TOTAL OF 828 CONFORMATIONALLY-RESTRICTING NOE-DERIVED DISTANCE RESTRAINTS, 99 DIHEDRAL ANGLE RESTRAINTS, AND 28 HYDROGEN BOND RESTRAINTS. (13.5 CONSTRAINTS PER RESIDUE; 5.2 LONG-RANGE RESTRAINTS PER RESIDUE). STRUCTURE DETERMINATION WAS PERFORMED ITERATIVELY USING AUTOSTRUCTURE (DYANA). THE UNSTRUCTURED 11 RESIDUE C-TERMINAL TAG (AAALEHHHHHH) WAS INCLUDED IN THE STRUCTURE CALCULATIONS BUT IS OMITTED FROM THIS DEPOSITION.
代表構造
選択基準: lowest target function
NMRアンサンブル
コンフォーマー選択の基準: target function / 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