6TFI

PXR IN COMPLEX WITH THROMBIN INHIBITOR COMPOUND 17

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	CCD
Collection date	2010-10-13
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 21 21 21
Unit cell lengths	85.356, 88.964, 105.658
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	44.480 - 1.850
R-factor	0.17276
Rwork	0.172
R-free	0.19932
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	3hvl
RMSD bond length	0.005
RMSD bond angle	1.308
Data reduction software	XDS (June 17, 2015)
Data scaling software	XSCALE (June 17, 2015)
Phasing software	REFMAC (5.5.0102)
Refinement software	REFMAC (5.8.0238)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	44.480	1.960
High resolution limit [Å]	1.850	1.850
Rmeas	0.059	0.977
Number of reflections	67925	10924
<I/σ(I)>	17.15	1.82
Completeness [%]	97.9	98.7
Redundancy	5.07	5
CC(1/2)	0.999	0.668

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 25 MILLIMOLAR COMPOUND 17 (FROM 500 MILLIMOLAR STOCK IN DMSO) for 24 hours at 277 K, MIXED WITH 1 MICROLITER OF RESERVOIR (100 MILLIMOLAR IMIDAZOLE PH 8.0, 20 % (V/V) MPD). CRYO BUFFER 100 MILLIMOLAR IMIDAZOLE PH 8.0, 30 % (V/V) MPD