1QBO
BOVINE TRYPSIN 7-[[6-[[1-(1-IMINOETHYL)PIPERIDIN-4-YL]OXY]-2-METHYL-BENZIMIDAZOL-1-YL]METHYL]NAPHTHALENE-2-CARBOXIMIDAMID ZK-806711 INHIBITOR COMPLEX
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | ROTATING ANODE |
Source details | RIGAKU RU300 |
Temperature [K] | 297 |
Detector technology | IMAGE PLATE |
Collection date | 1994-12-20 |
Detector | RIGAKU RAXIS II |
Spacegroup name | P 31 2 1 |
Unit cell lengths | 55.020, 55.020, 109.140 |
Unit cell angles | 90.00, 90.00, 120.00 |
Refinement procedure
Resolution | 10.000 - 1.800 |
R-factor | 0.187 * |
Rwork | 0.187 |
R-free | 0.22400 |
Structure solution method | DIRECT REPLACEMENT |
RMSD bond length | 0.016 |
RMSD bond angle | 0.032 |
Data reduction software | DENZO |
Data scaling software | SCALEPACK |
Refinement software | PROFFT |
Data quality characteristics
Overall | Outer shell | |
Low resolution limit [Å] | 10.000 | 2.100 |
High resolution limit [Å] | 1.800 | 1.800 |
Rmerge | 0.098 * | 0.202 * |
Number of reflections | 15600 | |
<I/σ(I)> | 7.6 | |
Completeness [%] | 95.4 | 95 |
Redundancy | 2.7 | 2.0 * |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, HANGING DROP | 7.4 | 297 | MICROCRYSTALS WERE INITIALLY GROWN USING THE HANGING DROP METHOD IN LINBRO CULTURE PLATES. CRYSTALLIZATION RESERVOIRS CONTAIN 1.8 - 2.0 M AMMONIUM SULFATE, 50 MM TRIS HCL, 10 MM CACL2, PH 7.4. SIX UL OF 15 MG/ML BOVINE TRYPSIN IN 20 MM 2-AMINOBENZIMIDAZOLE WAS ADDED TO 6 UL OF RESERVOIR. MACROSEEDING WAS USED TO GROW LARGE CRYSTALS (REF 5). SINGLE CRYSTALS WERE WASHED IN 0.8 M AMMONIUM SULFATE, 50 MM TRIS HCL, 10 MM CACL2, PH 7.4. THE WASHED CRYSTALS WERE PLACED IN A 18 HOUR OLD HANGING, VAPOR DIFFUSION, HANGING DROP, temperature 297K |
Crystallization Reagents in Literatures
ID | crystal ID | solution | reagent name | concentration (unit) | details |
1 | 1 | reservoir | ammonium sulfate | 1.8-2.0 (M) | |
2 | 1 | reservoir | Tris-HCl | 50 (mM) | |
3 | 1 | reservoir | 10 (mM) | ||
4 | 1 | drop | trypsin | 15 (mg/ml) | |
5 | 1 | drop | 2-aminobenzimidazole | 20 (mM) |