7PBB
Crystal structure of CD73 in complex with caffeine in the open form
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | SYNCHROTRON |
| Source details | BESSY BEAMLINE 14.1 |
| Synchrotron site | BESSY |
| Beamline | 14.1 |
| Temperature [K] | 100 |
| Detector technology | PIXEL |
| Collection date | 2016-12-02 |
| Detector | DECTRIS PILATUS 6M |
| Wavelength(s) | 0.9184 |
| Spacegroup name | P 21 21 2 |
| Unit cell lengths | 67.243, 131.799, 66.316 |
| Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
| Resolution | 47.260 - 1.470 |
| R-factor | 0.1738 |
| Rwork | 0.173 |
| R-free | 0.19560 |
| Structure solution method | FOURIER SYNTHESIS |
| Starting model (for MR) | 4h2g |
| RMSD bond length | 0.016 |
| RMSD bond angle | 1.966 |
| Data reduction software | XDS |
| Data scaling software | Aimless (0.7.4) |
| Phasing software | REFMAC |
| Refinement software | REFMAC (5.8.0267) |
Data quality characteristics
| Overall | Inner shell | Outer shell | |
| Low resolution limit [Å] | 47.260 | 47.220 | 1.500 |
| High resolution limit [Å] | 1.470 | 8.060 | 1.470 |
| Rmerge | 0.172 | 0.066 | 1.443 |
| Rmeas | 0.187 | 0.074 | 1.566 |
| Rpim | 0.072 | 0.032 | 0.597 |
| Total number of observations | 4061 | 30755 | |
| Number of reflections | 99458 | 719 | 4699 |
| <I/σ(I)> | 7.6 | 23.5 | 1.4 |
| Completeness [%] | 99.0 | 99.1 | 95.4 |
| Redundancy | 6.6 | 5.6 | 6.5 |
| CC(1/2) | 0.995 | 0.994 | 0.348 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | VAPOR DIFFUSION, HANGING DROP | 292 | 7 mg/mL protein concentration, 100 mM Tris pH 7.8, 10 % PEG6000, equal amounts of protein and reservoir. Following crystal formation (1-2 days), the crystals were transferred to soaking solution containing reservoir solution and 50 mM caffeine. Crystals were then transferred to cryo solution containing an additional 20 % glycerol, soaked for ~2-5 min, and flash frozen in liquid nitrogen. |
