5SHJ
Crystal Structure of human phosphodiesterase 10 in complex with 4-(azetidine-1-carbonyl)-2-methyl-N-[3-(phenylcarbamoyl)phenyl]pyrazole-3-carboxamide
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 | 2009-03-30 |
Detector | MARMOSAIC 225 mm CCD |
Wavelength(s) | 1.000000 |
Spacegroup name | H 3 |
Unit cell lengths | 136.287, 136.287, 235.915 |
Unit cell angles | 90.00, 90.00, 120.00 |
Refinement procedure
Resolution | 43.830 - 2.300 |
R-factor | 0.1914 |
Rwork | 0.189 |
R-free | 0.24370 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | inhouse model |
RMSD bond length | 0.008 |
RMSD bond angle | 1.556 |
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] | 43.830 | 43.830 | 2.360 |
High resolution limit [Å] | 2.300 | 10.290 | 2.300 |
Rmerge | 0.115 | 0.043 | 0.793 |
Rmeas | 0.135 | 0.050 | 0.958 |
Total number of observations | 241659 | ||
Number of reflections | 71069 | 805 | 4989 |
<I/σ(I)> | 7.61 | 24.1 | 1.28 |
Completeness [%] | 97.9 | 98.1 | 93.1 |
Redundancy | 3.4 | 3.804 | 2.784 |
CC(1/2) | 0.993 | 0.996 | 0.499 |
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 |