4AQH

Plasminogen activator inhibitor type-1 in complex with the inhibitor AZ3976

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID23-2
Synchrotron site	ESRF
Beamline	ID23-2
Temperature [K]	100
Detector technology	CCD
Collection date	2010-06-11
Detector	MARMOSAIC 225 mm CCD
Spacegroup name	P 31
Unit cell lengths	119.399, 119.399, 99.691
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	60.010 - 2.400
R-factor	0.15867
Rwork	0.157
R-free	0.18138
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1dvn
RMSD bond length	0.014
RMSD bond angle	1.485
Data reduction software	MOSFLM
Data scaling software	SCALA
Phasing software	MOLREP
Refinement software	REFMAC (5.5.0066)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	49.900	2.460
High resolution limit [Å]	2.400	2.400
Rmerge	0.100	0.700
Number of reflections	62179
<I/σ(I)>	16	2.4
Completeness [%]	100.0	100
Redundancy	5.9	5.9

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	5.6		PAI-1 WAS CONCENTRATED TO ABOUT 4 G/L IN A BUFFER CONTAINING 10 MM SODIUM ACETATE PH 5.6, 150 MM SODIUM CHLORIDE AND 1 MM EDTA. AZ3976 WAS DISSOLVED IN DEUTERATED DMSO AND ADDED TO THE PROTEIN SAMPLE TO A FINAL CONCENTRATION OF 0.3 MM. CRYSTALS WERE OBTAINED BY THE HANGING DROP VAPOR DIFFUSION TECHNIQUE: 2.5 UL PROTEIN SAMPLE WAS MIXED WITH 1 UL OF A WELL SOLUTION CONTAINING 2.0 M SODIUM CHLORIDE, 100 MM BIS-TRIS PH 6.8