1FJS

CRYSTAL STRUCTURE OF THE INHIBITOR ZK-807834 (CI-1031) COMPLEXED WITH FACTOR XA

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SSRL BEAMLINE BL9-2
Synchrotron site	SSRL
Beamline	BL9-2
Temperature [K]	100
Detector technology	CCD
Collection date	1999-11-19
Detector	ADSC QUANTUM 4
Spacegroup name	P 21 21 21
Unit cell lengths	55.770, 71.960, 80.230
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	8.000 - 1.920
R-factor	0.196 *
Rwork	0.196
R-free	0.25600
Structure solution method	DIRECT REPLACEMENT
Starting model (for MR)	1xka
RMSD bond length	0.011
RMSD bond angle	1.777 *
Data reduction software	X-GEN
Data scaling software	X-GEN
Phasing software	X-PLOR (3.1)
Refinement software	X-PLOR (3.1)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	26.100	1.930
High resolution limit [Å]	1.920 *	1.920 *
Rmerge	0.054 *	0.260 *
Total number of observations	104166 *
Number of reflections	29450
<I/σ(I)>	12.6	1.33
Completeness [%]	99.7 *	99.9 *
Redundancy	3.6 *	3.7 *

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	Vapor diffusion, hanging drop *	8	295	Drop; 2 microliter, 12 mg/ml Factor Xa, 50 mM Tris pH 8.0, 75 mM NaCl + 2 microlter reservoir: Reservoir; 15-21% PEG-1500 and 10mM CaCl2, VAPOR DIFFUSION, temperature 295K

Crystallization Reagents in Literatures

ID	crystal ID	solution	reagent name	concentration (unit)	details
1	1	drop	inhibitor		3-fold excess
2	1	drop			1 equiv
3	1	drop	protein	12 (mg/ml)
4	1	reservoir	PEG1500	15-21 (%)
5	1	reservoir		10 (mM)