6HTY
PXR in complex with P2X4 inhibitor compound 25
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | BESSY BEAMLINE 14.1 |
Synchrotron site | BESSY |
Beamline | 14.1 |
Temperature [K] | 100 |
Detector technology | PIXEL |
Collection date | 2014-10-01 |
Detector | DECTRIS PILATUS 6M |
Wavelength(s) | 1.040432 |
Spacegroup name | P 21 21 21 |
Unit cell lengths | 85.417, 88.616, 104.929 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 45.150 - 2.220 |
R-factor | 0.18674 |
Rwork | 0.185 |
R-free | 0.22611 |
Structure solution method | FOURIER SYNTHESIS |
Starting model (for MR) | 3hvl |
RMSD bond length | 0.011 |
RMSD bond angle | 1.420 |
Data reduction software | XDS |
Data scaling software | XDS |
Phasing software | REFMAC (5.8.0049) |
Refinement software | REFMAC (5.8.0189) |
Data quality characteristics
Overall | Outer shell | |
Low resolution limit [Å] | 45.150 | 2.350 |
High resolution limit [Å] | 2.220 | 2.220 |
Rmeas | 0.065 | 0.847 |
Number of reflections | 39804 | 6262 |
<I/σ(I)> | 15.4 | 1.7 |
Completeness [%] | 99.3 | 98.6 |
Redundancy | 5 | 4.9 |
CC(1/2) | 0.999 | 0.707 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, HANGING DROP | 8 | 277 | 1 microliter protein at 12.1 mg/ml (in 20 millimolar Tris pH 7.8, 250 millimolar NaCl, 2.5 millimolar EDTA, 5% (v/v) glycerol, 5 mM DTT), preincubated with 10 millimolar compound 15 (from 200 millimolar stock in DMSO), mixed with 1 microliter of reservoir (100 mM imidazole pH 8.0, 17 % (v/v) MPD). Crystals additionally soaked in 20 millimolar compound 15 prior to data collection. cryo buffer 34% (v/v) MPD supplemented with 20 millimolar compound 15 |