温度: 277 K / 手法: 蒸気拡散法, ハンギングドロップ法 / pH: 8 詳細: 3 uL protein solution (20 mg/mL lyophilized hCAII in 50 mM Tris-sulfate, 1 mM methyl mercuric acetate) and 5 uL precipitating buffer (2.6 M ammonium sulfate, 50 mM Tris-sulfate were mixed and ...詳細: 3 uL protein solution (20 mg/mL lyophilized hCAII in 50 mM Tris-sulfate, 1 mM methyl mercuric acetate) and 5 uL precipitating buffer (2.6 M ammonium sulfate, 50 mM Tris-sulfate were mixed and equilibrated against 500 uL precipitating buffer. Single crystals were transferred into a cross-linking buffer, which was prepared from 10 uL precipitating buffer and 5 uL glutaraldehyde solution (0.8 % glutaraldehyde, 4 M ammonium sulfate, 50 mM Tris-sulfate) and equilibrated for 18 h. Cross-linked crystals were transferred into soaking buffer (9 uL precipitating buffer, 0.5 uL 60 mM {(6-benzene)Ru(bispy 3)Cl}+ in DMSO) and equilibrated for 54 h, pH 8.0, VAPOR DIFFUSION, HANGING DROP, temperature 277K
解像度: 1.3→30.6 Å / Cor.coef. Fo:Fc: 0.978 / Cor.coef. Fo:Fc free: 0.964 / SU B: 1.461 / SU ML: 0.028 / 交差検証法: THROUGHOUT / ESU R: 0.048 / ESU R Free: 0.047 / 立体化学のターゲット値: MAXIMUM LIKELIHOOD / 詳細: HYDROGENS HAVE BEEN ADDED IN THE RIDING POSITIONS
Rfactor
反射数
%反射
Selection details
Rfree
0.16471
2984
5.1 %
RANDOM
Rwork
0.12756
-
-
-
obs
0.12947
59007
98.74 %
-
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
原子変位パラメータ
Biso mean: 12.373 Å2
Baniso -1
Baniso -2
Baniso -3
1-
-0.04 Å2
-0 Å2
-0.28 Å2
2-
-
0.15 Å2
0 Å2
3-
-
-
-0.26 Å2
精密化ステップ
サイクル: LAST / 解像度: 1.3→30.6 Å
タンパク質
核酸
リガンド
溶媒
全体
原子数
2058
0
48
420
2526
拘束条件
Refine-ID
タイプ
Dev ideal
Dev ideal target
数
X-RAY DIFFRACTION
r_bond_refined_d
0.01
0.022
2238
X-RAY DIFFRACTION
r_bond_other_d
0.001
0.02
1513
X-RAY DIFFRACTION
r_angle_refined_deg
1.454
1.987
3084
X-RAY DIFFRACTION
r_angle_other_deg
0.87
3
3701
X-RAY DIFFRACTION
r_dihedral_angle_1_deg
6.622
5
270
X-RAY DIFFRACTION
r_dihedral_angle_2_deg
32.962
24.804
102
X-RAY DIFFRACTION
r_dihedral_angle_3_deg
12.195
15
368
X-RAY DIFFRACTION
r_dihedral_angle_4_deg
17.319
15
7
X-RAY DIFFRACTION
r_chiral_restr
0.088
0.2
309
X-RAY DIFFRACTION
r_gen_planes_refined
0.007
0.021
2496
X-RAY DIFFRACTION
r_gen_planes_other
0.001
0.02
443
X-RAY DIFFRACTION
r_nbd_refined
X-RAY DIFFRACTION
r_nbd_other
X-RAY DIFFRACTION
r_nbtor_refined
X-RAY DIFFRACTION
r_nbtor_other
X-RAY DIFFRACTION
r_xyhbond_nbd_refined
X-RAY DIFFRACTION
r_xyhbond_nbd_other
X-RAY DIFFRACTION
r_metal_ion_refined
X-RAY DIFFRACTION
r_metal_ion_other
X-RAY DIFFRACTION
r_symmetry_vdw_refined
X-RAY DIFFRACTION
r_symmetry_vdw_other
X-RAY DIFFRACTION
r_symmetry_hbond_refined
X-RAY DIFFRACTION
r_symmetry_hbond_other
X-RAY DIFFRACTION
r_symmetry_metal_ion_refined
X-RAY DIFFRACTION
r_symmetry_metal_ion_other
X-RAY DIFFRACTION
r_mcbond_it
3.195
1.5
1326
X-RAY DIFFRACTION
r_mcbond_other
1.233
1.5
534
X-RAY DIFFRACTION
r_mcangle_it
4.386
2
2146
X-RAY DIFFRACTION
r_scbond_it
6.395
3
912
X-RAY DIFFRACTION
r_scangle_it
8.349
4.5
914
X-RAY DIFFRACTION
r_rigid_bond_restr
2.895
3
3751
X-RAY DIFFRACTION
r_sphericity_free
X-RAY DIFFRACTION
r_sphericity_bonded
LS精密化 シェル
解像度: 1.3→1.334 Å / Total num. of bins used: 20
Rfactor
反射数
%反射
Rfree
0.285
181
-
Rwork
0.241
3837
-
obs
-
-
92.2 %
精密化 TLS
手法: refined / Origin x: 11.76 Å / Origin y: -1.003 Å / Origin z: 16.314 Å