2VH6
Structure and property based design of factor Xa inhibitors: pyrrolidin-2-ones with biaryl P4 motifs
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | SYNCHROTRON |
| Source details | SRS BEAMLINE PX14.2 |
| Synchrotron site | SRS |
| Beamline | PX14.2 |
| Temperature [K] | 100 |
| Detector technology | CCD |
| Collection date | 2002-01-24 |
| Detector | ADSC CCD |
| Spacegroup name | P 21 21 21 |
| Unit cell lengths | 55.959, 72.309, 78.976 |
| Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
| Resolution | 20.000 - 1.950 |
| R-factor | 0.19906 |
| Rwork | 0.197 |
| R-free | 0.24163 |
| Structure solution method | MOLECULAR REPLACEMENT |
| RMSD bond length | 0.014 |
| RMSD bond angle | 1.625 |
| Data reduction software | DENZO |
| Data scaling software | SCALEPACK |
| Phasing software | REFMAC |
| Refinement software | REFMAC (5.3.0006) |
Data quality characteristics
| Overall | Outer shell | |
| Low resolution limit [Å] | 25.000 | 2.020 |
| High resolution limit [Å] | 1.930 | 1.950 |
| Rmerge | 0.050 | 0.450 |
| Number of reflections | 22951 | |
| Completeness [%] | 93.1 | |
| Redundancy | 3.6 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | VAPOR DIFFUSION, HANGING DROP | 5.85 | CRYSTALLISATION WAS CARRIED OUT USING THE HANGING DROP VAPOUR DIFFUSION METHOD IN 2UL DROPS CONTAINING A 1:1 MIXTURE OF PROTEIN AND WELL SOLUTION. WELL SOLUTION CONTAINED 16-20% PEG 6K, 50MM MES-NAOH (PH5.7-6.0), 5MM CACL2 AND 50MM NACL, pH 5.85 |
