1SIH
AGAO in covalent complex with the inhibitor MOBA ("4-(4-methylphenoxy)-2-butyn-1-amine")
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | ROTATING ANODE |
Source details | RIGAKU RU200 |
Temperature [K] | 100 |
Detector technology | IMAGE PLATE |
Collection date | 2003-08-01 |
Detector | MAR scanner 345 mm plate |
Spacegroup name | C 1 2 1 |
Unit cell lengths | 157.645, 62.787, 91.657 |
Unit cell angles | 90.00, 112.18, 90.00 |
Refinement procedure
Resolution | 22.810 - 1.730 |
R-factor | 0.14963 |
Rwork | 0.149 |
R-free | 0.16837 |
Structure solution method | MOLECULAR REPLACEMENT |
RMSD bond length | 0.010 |
RMSD bond angle | 1.367 |
Data reduction software | MOSFLM |
Data scaling software | CCP4 ((SCALA) |
Refinement software | REFMAC (5.1.24) |
Data quality characteristics
Overall | Outer shell | |
Low resolution limit [Å] | 22.810 | 1.770 |
High resolution limit [Å] | 1.730 | 1.730 |
Rmerge | 0.031 | 0.200 |
Number of reflections | 80205 | |
<I/σ(I)> | 29 | 7.4 |
Completeness [%] | 92.3 | 71.2 |
Redundancy | 5.5 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, HANGING DROP | 6.5 | 293 | 2 microlitres of (AGAO 10 mg/ml, 50mM HEPES pH 7.0) plus 2 microlitres of the reservoir solution (1.1M (NH4)2SO4, 150mM Na-citrate pH 6.5) Crystals were cryoprotected and soaked with MOBA. Crystals were soaked in well solution plus 20% glycerol plus 10-fold excess of MOBA., for 48 hours. The glycerol concentration was then raised to 30% over 30 minutes, prior to flash freezing., VAPOR DIFFUSION, HANGING DROP, temperature 293K |