CRYSTAL PACKING AND ANALYTICAL SIZE EXCLUSION CHROMATOGRAPHY ANALYSES SUPPORT THE ASSIGNMENT OF A DIMER AS THE SIGNIFICANT OLIGOMERIZATION STATE IN SOLUTION.
THIS CONSTRUCT (1-406) WAS EXPRESSED WITH THE PURIFICATION TAG MGSDKIHHHHHHENLYFQG. THE TAG WAS ...THIS CONSTRUCT (1-406) WAS EXPRESSED WITH THE PURIFICATION TAG MGSDKIHHHHHHENLYFQG. THE TAG WAS REMOVED WITH TEV PROTEASE LEAVING ONLY A GLYCINE (0) FOLLOWED BY THE TARGET SEQUENCE.
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
0.97947
1
反射
解像度: 2.15→29.775 Å / Num. obs: 47045 / % possible obs: 100 % / 冗長度: 4.1 % / Biso Wilson estimate: 20.962 Å2 / Rsym value: 0.16 / Net I/σ(I): 7.2
反射 シェル
Diffraction-ID: 1
解像度 (Å)
冗長度 (%)
Rmerge(I) all
Rmerge(I) obs
Mean I/σ(I) obs
Num. measured all
Num. unique all
Rpim(I) all
Rrim(I) all
Rsym value
Net I/σ(I) obs
% possible all
2.15-2.21
4.2
0.723
0.631
2.2
14304
3436
0.349
0.723
0.631
2.2
100
2.21-2.27
4.2
0.626
0.546
1.4
13830
3328
0.303
0.626
0.546
2.6
100
2.27-2.33
4.2
0.521
0.455
1.7
13720
3293
0.251
0.521
0.455
3.1
100
2.33-2.4
4.2
0.513
0.448
1.7
13141
3151
0.248
0.513
0.448
3.1
100
2.4-2.48
4.2
0.457
0.399
1.9
12804
3067
0.221
0.457
0.399
3.6
100
2.48-2.57
4.2
0.4
0.349
2.2
12353
2968
0.193
0.4
0.349
4
100
2.57-2.67
4.2
0.343
0.3
2.5
11908
2858
0.166
0.343
0.3
4.7
100
2.67-2.78
4.2
0.284
0.248
3
11616
2788
0.137
0.284
0.248
5.5
100
2.78-2.9
4.2
0.252
0.22
3.4
10983
2645
0.122
0.252
0.22
6
100
2.9-3.04
4.2
0.2
0.174
4.3
10622
2549
0.097
0.2
0.174
7.3
100
3.04-3.21
4.1
0.17
0.148
5.1
10085
2433
0.082
0.17
0.148
8.3
100
3.21-3.4
4.1
0.129
0.112
6.6
9556
2307
0.063
0.129
0.112
10.4
100
3.4-3.63
4.1
0.117
0.102
7
8915
2155
0.057
0.117
0.102
11.8
100
3.63-3.93
4.1
0.103
0.09
7.8
8409
2038
0.05
0.103
0.09
13.4
100
3.93-4.3
4.1
0.084
0.073
9.4
7616
1863
0.041
0.084
0.073
15.6
100
4.3-4.81
4.1
0.077
0.067
9.6
7023
1717
0.038
0.077
0.067
16
100
4.81-5.55
4
0.079
0.069
10.1
6147
1521
0.039
0.079
0.069
14.4
100
5.55-6.8
4
0.085
0.074
9.6
5156
1300
0.042
0.085
0.074
12.7
100
6.8-9.62
3.9
0.064
0.055
10.2
4004
1034
0.032
0.064
0.055
15.6
100
9.62-29.775
3.6
0.058
0.049
10.8
2110
594
0.031
0.058
0.049
15.5
96.8
-
位相決定
位相決定
手法: 多波長異常分散
-
解析
ソフトウェア
名称
バージョン
分類
NB
REFMAC
5.5.0110
精密化
PHENIX
精密化
SOLVE
位相決定
MolProbity
3beta29
モデル構築
SCALA
3.3.15
データスケーリング
PDB_EXTRACT
3.006
データ抽出
MOSFLM
データ削減
精密化
構造決定の手法: 多波長異常分散 / 解像度: 2.15→29.775 Å / Cor.coef. Fo:Fc: 0.959 / Cor.coef. Fo:Fc free: 0.937 / Occupancy max: 1 / Occupancy min: 0.15 / SU B: 8.014 / SU ML: 0.112 / 交差検証法: THROUGHOUT / σ(F): 0 / ESU R Free: 0.171 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 RECORDS CONTAIN SUM OF TLS AND RESIDUAL B FACTORS. ANISOU RECORDS CONTAIN SUM OF TLS AND RESIDUAL U FACTORS. 3. WATERS WERE ...詳細: 1. HYDROGENS HAVE BEEN ADDED IN THE RIDING POSITIONS. 2. ATOM RECORDS CONTAIN SUM OF TLS AND RESIDUAL B FACTORS. ANISOU RECORDS CONTAIN SUM OF TLS AND RESIDUAL U FACTORS. 3. WATERS WERE EXCLUDED FROM AUTOMATIC TLS ASSIGNMENT. 4. 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. 5. ELECTRON DENSITY REVEALS RESIDUE LYS-252 TO BE COVALENTLY ATTACHED TO PYRIDOXAL-5'-PHOSPHATE (PLP) VIA A SCHIFF-BASE LINKAGE. THIS COVALENTLY MODIFIED RESIDUE HAS BEEN MODELED AS 2-LYSINE(3-HYDROXY-2-METHYL-5-PHOSPHONOOXYMETHYL- PYRIDIN-4-YLMETHANE) (LLP). 6. BASED ON THE ADDITIONAL ELECTRON DENSITY SURROUNDING THE CYS-325 SIDE-CHAIN, THIS CYSTEINE HAS BEEN MODELED AS A CYSTEINE-S-DIOXIDE (CSD) IN BOTH CHAINS A AND B. 7. RESIDUES 12-26 OF CHAIN A AND RESIDUES 12-20 OF CHAIN B WERE UNMODELED DUE TO DISORDER AND LACK OF ELECTRON DENSITY IN THESE REGIONS. 8. CHLORIDE (CL) IONS, GLYCEROL (GOL), AND POLYETHYLENE GLYCOL (PEG) FROM THE PURIFICATION, CRYSTALLIZATION, AND CRYOPROTECTANT SOLUTIONS HAVE BEEN MODELED INTO THE SOLVENT STRUCTURE. 9. TLS GROUPS WERE ASSIGNED WITH THE AID OF THE TLSMD SERVER.
Rfactor
反射数
%反射
Selection details
Rfree
0.2
2382
5.1 %
RANDOM
Rwork
0.153
-
-
-
obs
0.156
46978
99.99 %
-
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