5SIB
Crystal Structure of human phosphodiesterase 10 in complex with 3-methyl-6-[2-(2-methyl-5-pyrrolidin-1-yl-1,2,4-triazol-3-yl)ethyl]-2-(trifluoromethyl)imidazo[1,2-b]pyridazine
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 | 2012-01-31 |
Detector | PSI PILATUS 6M |
Wavelength(s) | 0.700010 |
Spacegroup name | H 3 |
Unit cell lengths | 135.556, 135.556, 235.636 |
Unit cell angles | 90.00, 90.00, 120.00 |
Refinement procedure
Resolution | 43.730 - 2.540 |
R-factor | 0.1753 |
Rwork | 0.172 |
R-free | 0.24860 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | inhouse model |
RMSD bond length | 0.009 |
RMSD bond angle | 1.614 |
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] | 43.730 | 43.730 | 2.610 |
High resolution limit [Å] | 2.540 | 11.360 | 2.540 |
Rmerge | 0.150 | 0.026 | 1.293 |
Rmeas | 0.167 | 0.029 | 1.434 |
Total number of observations | 281927 | ||
Number of reflections | 53250 | 589 | 3945 |
<I/σ(I)> | 8.64 | 47.07 | 1.11 |
Completeness [%] | 100.0 | 98.5 | 100 |
Redundancy | 5.294 | 5.389 | 5.376 |
CC(1/2) | 0.996 | 0.999 | 0.399 |
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 |