5SIX
Crystal Structure of human phosphodiesterase 10 in complex with 5-[(3R)-3-fluoropyrrolidin-1-yl]-2-(3-methylquinoxalin-2-yl)-N-(oxan-4-yl)pyrazolo[1,5-a]pyrimidin-7-amine
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | SLS BEAMLINE X10SA |
Synchrotron site | SLS |
Beamline | X10SA |
Temperature [K] | 100 |
Detector technology | PIXEL |
Collection date | 2013-05-04 |
Detector | PSI PILATUS 6M |
Wavelength(s) | 0.999960 |
Spacegroup name | I 2 3 |
Unit cell lengths | 141.343, 141.343, 141.343 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 44.700 - 2.290 |
R-factor | 0.1841 |
Rwork | 0.182 |
R-free | 0.21890 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | inhouse model |
RMSD bond length | 0.007 |
RMSD bond angle | 1.423 |
Data reduction software | XDS |
Data scaling software | XSCALE |
Phasing software | PHASER |
Refinement software | REFMAC (5.8.0258) |
Data quality characteristics
Overall | Inner shell | Outer shell | |
Low resolution limit [Å] | 44.700 | 44.700 | 2.350 |
High resolution limit [Å] | 2.290 | 10.240 | 2.290 |
Rmerge | 0.099 | 0.029 | 2.062 |
Rmeas | 0.101 | 0.030 | 2.114 |
Total number of observations | 428846 | ||
Number of reflections | 21279 | 264 | 1593 |
<I/σ(I)> | 24.97 | 105.24 | 1.75 |
Completeness [%] | 100.0 | 98.5 | 100 |
Redundancy | 20.153 | 18.795 | 20.653 |
CC(1/2) | 1.000 | 1.000 | 0.700 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, SITTING DROP | 7.5 | 295 | 5-20 mg/mL protein in 25mM HEPES/NaOH pH7.5, 150mM NaCl, 50mM BME mixed 1:1 with reservoir 0.1M HEPES/NaOH pH7.5, 30% PEG550MME, 50mM MgCl2 |