2WYJ
Structure and property based design of factor Xa inhibitors: pyrrolidin-2-ones with monoaryl P4 motifs
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | ESRF BEAMLINE ID14-4 |
Synchrotron site | ESRF |
Beamline | ID14-4 |
Temperature [K] | 100 |
Detector technology | CCD |
Collection date | 2003-11-30 |
Detector | ADSC CCD |
Spacegroup name | P 21 21 21 |
Unit cell lengths | 56.564, 72.485, 78.177 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 28.400 - 2.380 |
R-factor | 0.19979 |
Rwork | 0.197 |
R-free | 0.25478 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | 1ezq |
RMSD bond length | 0.011 |
RMSD bond angle | 1.525 |
Data reduction software | DENZO |
Data scaling software | SCALEPACK |
Phasing software | REFMAC |
Refinement software | REFMAC (5.4.0073) |
Data quality characteristics
Overall | Outer shell | |
Low resolution limit [Å] | 30.000 | 2.490 |
High resolution limit [Å] | 2.380 | 2.380 |
Rmerge | 0.060 | 0.370 |
Number of reflections | 13086 | |
<I/σ(I)> | 22.7 | 4 |
Completeness [%] | 98.2 | 96.4 |
Redundancy | 4.3 | 4 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, HANGING DROP | 5.75 | CRYSTALLISATION WAS CARRIED OUT USING HANG DROP VAPOUR DIFFUSION METHODS IN 2UL DROPS CONTAINING 1:1 RATIO PROTEIN AND WELL SOLUTION. WELL SOLUTION CONTAINED 16-20% PEG6K, 50MM MES-NAOH (PH5.5-6), 5MM CACL2 AND 50MM NACL, pH 5.75 |