CRYSTAL PACKING ANALYSIS AND ANALYTICAL SIZE-EXCLUSION CHROMATOGRAPHY SUPPORT THE ASSIGNMENT OF A DIMER AS THE SIGNIFICANT OLIGOMERIC FORM IN SOLUTION.
THIS CONSTRUCT (RESIDUES 1-224) WAS EXPRESSED WITH A PURIFICATION TAG MGSDKIHHHHHHENLYFQG. THE TAG ...THIS CONSTRUCT (RESIDUES 1-224) WAS EXPRESSED WITH A 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
0.97944
1
3
0.97894
1
反射
解像度: 2.2→29.127 Å / Num. obs: 24823 / % possible obs: 97.6 % / Observed criterion σ(I): -3 / Biso Wilson estimate: 30.791 Å2 / Rmerge(I) obs: 0.095 / Net I/σ(I): 8.35
反射 シェル
Diffraction-ID: 1
解像度 (Å)
最高解像度 (Å)
Rmerge(I) obs
Mean I/σ(I) obs
Num. measured obs
Num. unique obs
% possible all
2.2-2.28
0.651
1.6
9434
4849
96.4
2.28-2.37
0.473
2.2
9359
4799
97.7
2.37-2.48
0.425
2.4
9667
4942
97.6
2.48-2.61
0.325
3.1
9287
4750
98.1
2.61-2.77
0.235
4.1
9202
4708
97.7
2.77-2.98
0.17
5.4
9495
4842
98.2
2.98-3.28
0.109
7.9
9426
4826
98.2
3.28-3.76
0.058
13.6
9694
4948
98.1
3.76-4.72
0.035
19.8
9350
4780
97.6
4.72
0.03
23
9572
4903
96.9
-
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
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: 2.2→29.127 Å / Cor.coef. Fo:Fc: 0.962 / Cor.coef. Fo:Fc free: 0.935 / Occupancy max: 1 / Occupancy min: 0.25 / SU B: 10.753 / SU ML: 0.136 / 交差検証法: THROUGHOUT / σ(F): 0 / ESU R Free: 0.188 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.A MET-INHIBITION PROTOCOL WAS USED FOR SELENOMETHIONINE INCORPORATION DURING PROTEIN EXPRESSION. THE OCCUPANCY OF THE SE ATOMS IN THE ...詳細: 1.HYDROGENS HAVE BEEN ADDED IN THE RIDING POSITIONS. 2.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 FOR THE REDUCED SCATTERING POWER DUE TO PARTIAL S-MET INCORPORATION. 3.ATOM RECORDS CONTAIN SUM OF TLS AND RESIDUAL B FACTORS. ANISOU RECORD CONTAINS SUM OF TLS AND RESIDUAL U FACTORS. 4.SOLVENTS WERE EXCLUDED FROM AUTOMATIC TLS ASSIGNMENT. 5.ZINC (ZN), NICKEL (NI) AND IRON (FE) HAVE BEEN MODELED IN THE PUTATIVE ACTIVE SITE AT PARTIAL OCCUPANCIES BASED ON PEAKS IN AN X-RAY FLUORESCENCE EMISSION SPECTRA AND ANOMALOUS DIFFERENCE FOURIER MAPS CALCULATED FROM DIFFRACTION DATA COLLECTED BELOW AND ABOVE THE K-ABSORPTION EDGES FOR THESE METALS. 6.GLYCEROL (GOL) FROM THE CRYSTALLIZATION SOLUTION HAS BEEN MODELED INTO ELECTRON DENSITY AT THE PUTATIVE ACTIVE AND IT MAY BE A SUBSTRATE MIMIC.
Rfactor
反射数
%反射
Selection details
Rfree
0.2112
1263
5.1 %
RANDOM
Rwork
0.1644
-
-
-
obs
0.1667
24753
99.57 %
-
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: BABINET MODEL WITH MASK