THE CONSTRUCT (20-294) WAS EXPRESSED WITH A PURIFICATION TAG MGSDKIHHHHHHENLYFQG. THE TAG WAS ...THE CONSTRUCT (20-294) WAS EXPRESSED WITH A PURIFICATION TAG MGSDKIHHHHHHENLYFQG. THE TAG WAS REMOVED WITH TEV PROTEASE LEAVING ONLY A GLYCINE (0) FOLLOWED BY THE TARGET SEQUENCE.
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実験情報
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実験
実験
手法: X線回折 / 使用した結晶の数: 1
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試料調製
結晶
マシュー密度: 2.54 Å3/Da / 溶媒含有率: 51.48 %
結晶化
温度: 277 K / 手法: 蒸気拡散法, シッティングドロップ法 / pH: 5.5 詳細: 40.000000000% PEG-600, 0.1M Citrate pH 5.5, VAPOR DIFFUSION,SITTING DROP,NANODROP, temperature 277K, VAPOR DIFFUSION, SITTING DROP
モノクロメーター: Single crystal Si(111) bent monochromator (horizontal focusing) プロトコル: MAD / 単色(M)・ラウエ(L): M / 散乱光タイプ: x-ray
放射波長
ID
波長 (Å)
相対比
1
0.91837
1
2
0.97941
1
3
0.97894
1
反射
解像度: 1.35→27.993 Å / Num. obs: 68533 / % possible obs: 97.7 % / Observed criterion σ(I): -3 / Biso Wilson estimate: 10.556 Å2 / Rmerge F obs: 0.164 / Rmerge(I) obs: 0.058 / Rrim(I) all: 0.075 / Net I/σ(I): 10.61 / Num. measured all: 297194
反射 シェル
解像度 (Å)
最高解像度 (Å)
Rmerge F obs
Rmerge(I) obs
Mean I/σ(I) obs
Num. measured obs
Num. possible
Num. unique obs
Rrim(I) all
% possible all
1.35-1.4
0.861
0.505
1.9
28471
13740
13087
0.657
95.2
1.4-1.45
0.684
0.396
2.4
25252
11841
11410
0.516
96.4
1.45-1.52
0.531
0.308
3.1
30507
14080
13642
0.401
96.9
1.52-1.6
0.373
0.222
4.2
29318
13271
12963
0.288
97.7
1.6-1.7
0.292
0.168
5.5
29515
13174
12921
0.219
98.1
1.7-1.83
0.197
0.118
7.6
30053
13197
12944
0.153
98.1
1.83-2.02
0.124
0.075
11.5
31493
13629
13432
0.098
98.6
2.02-2.31
0.075
0.05
16.5
30508
13094
12930
0.065
98.7
2.31-2.91
0.052
0.038
21
30934
13209
13082
0.049
99
2.91
0.027
0.025
31.6
31143
13253
13079
0.032
98.7
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位相決定
位相決定
手法: 多波長異常分散
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解析
ソフトウェア
名称
バージョン
分類
NB
SHELX
位相決定
REFMAC
5.5.0110
精密化
XSCALE
データスケーリング
PDB_EXTRACT
3.1
データ抽出
XDS
データ削減
SHELXD
位相決定
autoSHARP
位相決定
精密化
構造決定の手法: 多波長異常分散 / 解像度: 1.35→27.993 Å / Cor.coef. Fo:Fc: 0.972 / Cor.coef. Fo:Fc free: 0.967 / Occupancy max: 1 / Occupancy min: 0.11 / SU B: 1.292 / SU ML: 0.027 / 交差検証法: THROUGHOUT / σ(F): 0 / ESU R: 0.046 / ESU R Free: 0.045 立体化学のターゲット値: MAXIMUM LIKELIHOOD WITH PHASES 詳細: (1). HYDROGENS HAVE BEEN ADDED IN THE RIDING POSITIONS. (2). ATOM RECORD CONTAINS SUM OF TLS AND RESIDUAL B FACTORS. ANISOU RECORD CONTAINS SUM OF TLS AND RESIDUAL U FACTORS. (3). A MET- ...詳細: (1). HYDROGENS HAVE BEEN ADDED IN THE RIDING POSITIONS. (2). ATOM RECORD CONTAINS SUM OF TLS AND RESIDUAL B FACTORS. ANISOU RECORD CONTAINS SUM OF TLS AND RESIDUAL U FACTORS. (3). A MET-INHIBITION PROTOCOL WAS USED FOR SELENOMETHIONINE INCORPORATION DURING PROTEIN EXPRESSION. THE OCCUPANCY OF THE SE ATOMS IN THE MSE RESIDUES WAS REDUCED TO 0.75 TO ACCOUNT FOR THE REDUCED SCATTERING POWER DUE TO PARTIAL S-MET INCORPORATION. (4). CL AND CITRATE (CIT) IONS, AND PEG-600 FRAGMENTS (PEG) FROM CRYSTALLIZATION CONDITION WERE MODELED INTO THE STRUCTURE. (5). RAMACHANDRAN OUTLIER OF RESIDUE GLN144 IS SUPPORTED BY ELECTRON DENSITY.
Rfactor
反射数
%反射
Selection details
Rfree
0.1595
3466
5.1 %
RANDOM
Rwork
0.1468
65006
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obs
0.1475
68472
98.8 %
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溶媒の処理
イオンプローブ半径: 0.8 Å / 減衰半径: 0.8 Å / VDWプローブ半径: 1.4 Å / 溶媒モデル: MASK