3KKT
Crystal structure of human PDE4b with 5-[3-[(1S,2S,4R)-Bicyclo[2.2.1]hept-2-yloxy]-4-methoxyp henyl]tetrahydro-2(1H)-pyrimidinone reveals ordering of the C-terminal helix residues 502-509.
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | SYNCHROTRON |
| Source details | DIAMOND BEAMLINE I02 |
| Synchrotron site | Diamond |
| Beamline | I02 |
| Temperature [K] | 100 |
| Detector technology | CCD |
| Collection date | 2009-08-12 |
| Detector | ADSC QUANTUM 315 |
| Wavelength(s) | 0.9759 |
| Spacegroup name | P 65 2 2 |
| Unit cell lengths | 89.740, 89.740, 337.443 |
| Unit cell angles | 90.00, 90.00, 120.00 |
Refinement procedure
| Resolution | 70.588 - 2.480 |
| R-factor | 0.23757 |
| Rwork | 0.235 |
| R-free | 0.29473 |
| Structure solution method | MOLECULAR REPLACEMENT |
| Starting model (for MR) | 1XLZ chain A |
| RMSD bond length | 0.007 |
| RMSD bond angle | 1.071 |
| Data reduction software | CrystalClear |
| Data scaling software | SCALA |
| Phasing software | PHASER |
| Refinement software | REFMAC (5.5.0102) |
Data quality characteristics
| Overall | Outer shell | |
| Low resolution limit [Å] | 70.588 | 2.540 |
| High resolution limit [Å] | 2.475 | 2.480 |
| Rmerge | 0.366 | |
| Number of reflections | 29905 | |
| <I/σ(I)> | 5.2 | 2.1 |
| Completeness [%] | 99.8 | 99.7 |
| Redundancy | 6.2 | 6.4 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | VAPOR DIFFUSION, SITTING DROP | 7 | 294 | 1.2 M tri-Sodium citrate dihydrate, 0.1 M BisTris propane pH 7.0, VAPOR DIFFUSION, SITTING DROP, temperature 294K |
