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