5SI4
Crystal Structure of human phosphodiesterase 10 in complex with 3-(2-naphthalen-1-ylpyrazol-3-yl)-1-[3-(trifluoromethoxy)phenyl]pyridazin-4-one
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | SLS BEAMLINE X10SA |
Synchrotron site | SLS |
Beamline | X10SA |
Temperature [K] | 100 |
Detector technology | CCD |
Collection date | 2008-07-18 |
Detector | MARMOSAIC 225 mm CCD |
Wavelength(s) | 0.650000 |
Spacegroup name | H 3 |
Unit cell lengths | 135.860, 135.860, 235.620 |
Unit cell angles | 90.00, 90.00, 120.00 |
Refinement procedure
Resolution | 43.730 - 2.390 |
R-factor | 0.178 |
Rwork | 0.175 |
R-free | 0.23800 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | inhouse model |
RMSD bond length | 0.008 |
RMSD bond angle | 1.549 |
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] | 43.750 | 43.730 | 2.450 |
High resolution limit [Å] | 2.390 | 10.690 | 2.390 |
Rmerge | 0.131 | 0.024 | 1.732 |
Rmeas | 0.144 | 0.026 | 1.912 |
Total number of observations | 371928 | ||
Number of reflections | 64217 | 721 | 4775 |
<I/σ(I)> | 11.57 | 51.35 | 0.98 |
Completeness [%] | 100.0 | 98.9 | 100 |
Redundancy | 5.792 | 5.588 | 5.593 |
CC(1/2) | 0.997 | 0.999 | 0.362 |
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 |