温度: 293 K / 手法: 蒸気拡散法, ハンギングドロップ法 詳細: 0.275 M K2SO4, 19% (w/v) PEG 3350, and 0.1 M HEPES pH 6.9. Crystals were cryoprotected by soaking for 10 min with 2 mM mannuronate tetrasaccharide and 20% (v/v) PEG 4000.
-
データ収集
回折
平均測定温度: 100 K / Serial crystal experiment: N
放射光源
由来: SEALED TUBE / タイプ: BRUKER D8 QUEST / 波長: 1.5406 Å
検出器
タイプ: BRUKER PHOTON 100 / 検出器: CMOS / 日付: 2015年5月13日
放射
モノクロメーター: M / プロトコル: SINGLE WAVELENGTH / 単色(M)・ラウエ(L): M / 散乱光タイプ: x-ray
放射波長
波長: 1.5406 Å / 相対比: 1
反射
解像度: 2.5→20.305 Å / Num. obs: 10903 / % possible obs: 99.3 % / 冗長度: 10.3 % / Rmerge(I) obs: 0.098 / Net I/σ(I): 16
反射 シェル
解像度: 2.5→2.6 Å / Rmerge(I) obs: 0.435 / Num. unique obs: 1196 / % possible all: 100
解像度: 2.5→20.305 Å / Cor.coef. Fo:Fc: 0.912 / Cor.coef. Fo:Fc free: 0.878 / SU B: 29.256 / SU ML: 0.295 / 交差検証法: THROUGHOUT / ESU R: 1.643 / ESU R Free: 0.337 / 詳細: Hydrogens have been added in their riding positions
Rfactor
反射数
%反射
Rfree
0.2689
571
5.237 %
Rwork
0.2461
10332
-
all
0.247
-
-
obs
-
10332
99.299 %
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: 1.2 Å / 溶媒モデル: MASK BULK SOLVENT
原子変位パラメータ
Biso mean: 39.375 Å2
Baniso -1
Baniso -2
Baniso -3
1-
-0.699 Å2
0 Å2
-0 Å2
2-
-
1.296 Å2
-0 Å2
3-
-
-
-0.597 Å2
精密化ステップ
サイクル: LAST / 解像度: 2.5→20.305 Å
タンパク質
核酸
リガンド
溶媒
全体
原子数
2432
0
0
38
2470
拘束条件
Refine-ID
タイプ
Dev ideal
Dev ideal target
数
X-RAY DIFFRACTION
r_bond_refined_d
0.007
0.013
2518
X-RAY DIFFRACTION
r_bond_other_d
0.001
0.017
2289
X-RAY DIFFRACTION
r_angle_refined_deg
1.503
1.644
3424
X-RAY DIFFRACTION
r_angle_other_deg
1.273
1.58
5249
X-RAY DIFFRACTION
r_dihedral_angle_1_deg
6.151
5
316
X-RAY DIFFRACTION
r_dihedral_angle_2_deg
30.293
21.799
139
X-RAY DIFFRACTION
r_dihedral_angle_3_deg
15.638
15
385
X-RAY DIFFRACTION
r_dihedral_angle_4_deg
17.024
15
19
X-RAY DIFFRACTION
r_chiral_restr
0.066
0.2
316
X-RAY DIFFRACTION
r_gen_planes_refined
0.006
0.02
2917
X-RAY DIFFRACTION
r_gen_planes_other
0.001
0.02
617
X-RAY DIFFRACTION
r_nbd_refined
0.2
0.2
567
X-RAY DIFFRACTION
r_symmetry_nbd_other
0.188
0.2
2104
X-RAY DIFFRACTION
r_nbtor_refined
0.163
0.2
1243
X-RAY DIFFRACTION
r_symmetry_nbtor_other
0.081
0.2
1096
X-RAY DIFFRACTION
r_xyhbond_nbd_refined
0.16
0.2
73
X-RAY DIFFRACTION
r_symmetry_xyhbond_nbd_other
0.098
0.2
1
X-RAY DIFFRACTION
r_symmetry_nbd_refined
0.125
0.2
11
X-RAY DIFFRACTION
r_nbd_other
0.202
0.2
35
X-RAY DIFFRACTION
r_symmetry_xyhbond_nbd_refined
0.262
0.2
2
X-RAY DIFFRACTION
r_mcbond_it
1.46
3.18
1258
X-RAY DIFFRACTION
r_mcbond_other
1.451
3.177
1257
X-RAY DIFFRACTION
r_mcangle_it
2.494
4.753
1570
X-RAY DIFFRACTION
r_mcangle_other
2.495
4.756
1571
X-RAY DIFFRACTION
r_scbond_it
1.395
3.344
1259
X-RAY DIFFRACTION
r_scbond_other
1.393
3.341
1258
X-RAY DIFFRACTION
r_scangle_it
2.421
4.931
1851
X-RAY DIFFRACTION
r_scangle_other
2.413
4.93
1851
X-RAY DIFFRACTION
r_lrange_it
6.771
58.763
10818
X-RAY DIFFRACTION
r_lrange_other
6.771
58.736
10805
LS精密化 シェル
解像度 (Å)
Rfactor Rfree
Num. reflection Rfree
Rfactor Rwork
Num. reflection Rwork
Refine-ID
% reflection obs (%)
2.5-2.564
0.31
35
0.327
750
X-RAY DIFFRACTION
100
2.564-2.634
0.289
45
0.321
731
X-RAY DIFFRACTION
100
2.634-2.71
0.289
37
0.321
714
X-RAY DIFFRACTION
100
2.71-2.793
0.329
35
0.299
694
X-RAY DIFFRACTION
100
2.793-2.883
0.381
33
0.273
657
X-RAY DIFFRACTION
99.5671
2.883-2.984
0.224
34
0.265
661
X-RAY DIFFRACTION
99.8563
2.984-3.095
0.243
36
0.247
641
X-RAY DIFFRACTION
100
3.095-3.22
0.295
33
0.255
588
X-RAY DIFFRACTION
100
3.22-3.361
0.278
31
0.249
579
X-RAY DIFFRACTION
100
3.361-3.523
0.407
33
0.255
559
X-RAY DIFFRACTION
99.3289
3.523-3.711
0.332
35
0.264
522
X-RAY DIFFRACTION
98.4099
3.711-3.932
0.205
25
0.242
501
X-RAY DIFFRACTION
97.7695
3.932-4.199
0.193
28
0.203
484
X-RAY DIFFRACTION
99.2248
4.199-4.528
0.274
36
0.195
433
X-RAY DIFFRACTION
99.5754
4.528-4.949
0.252
26
0.182
403
X-RAY DIFFRACTION
99.7674
4.949-5.514
0.238
29
0.231
372
X-RAY DIFFRACTION
99.5037
5.514-6.332
0.299
12
0.242
357
X-RAY DIFFRACTION
100
6.332-7.67
0.118
14
0.236
294
X-RAY DIFFRACTION
100
7.67-10.509
0.179
10
0.186
247
X-RAY DIFFRACTION
100
10.509-20.305
0.302
4
0.304
143
X-RAY DIFFRACTION
83.5227
精密化 TLS
手法: refined / Origin x: 9.039 Å / Origin y: 82.556 Å / Origin z: 19.965 Å