4QGE
phosphodiesterase-9A in complex with inhibitor WYQ-C36D
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | NSLS BEAMLINE X29A |
Synchrotron site | NSLS |
Beamline | X29A |
Temperature [K] | 100 |
Detector technology | CCD |
Detector | ADSC QUANTUM 315 |
Wavelength(s) | 1.05 |
Spacegroup name | P 41 21 2 |
Unit cell lengths | 103.580, 103.580, 268.657 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 30.000 - 2.000 |
Rwork | 0.241 |
R-free | 0.26800 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | PDE9 catalytic domain |
RMSD bond length | 0.006 |
RMSD bond angle | 1.200 |
Data reduction software | HKL-2000 |
Data scaling software | HKL-2000 |
Phasing software | AMoRE |
Refinement software | CNS |
Data quality characteristics
Overall | |
Low resolution limit [Å] | 30.000 |
High resolution limit [Å] | 2.000 |
Rmerge | 0.065 |
Number of reflections | 91112 |
<I/σ(I)> | 23 |
Completeness [%] | 91.5 |
Redundancy | 10.5 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, HANGING DROP | 7.5 | 277 | The crystals of PDE9A2 were grown by using hanging drop vapor diffusion method. The PDE9A2 (181 506) (8-10 mg/mL) in a buffer of 50 mM NaCl, 20 mM Tris HCl, pH 7.5, 1 mM -mercaptoethanol, and 1 mM EDTA was mixed with 2 mM IBMX overnight before setting-up of crystallization against the well buffer of 0.1 M HEPES (pH 7.5), 3.0 M sodium formate at 4 C. Crystals of the PDE9-3r complex were prepared by soaking PDE9-IBMX cocrystals in the crystallization buffer plus 2 mM 3r at 25oC for 3 days., VAPOR DIFFUSION, HANGING DROP, temperature 277K |