5Q0G

FACTOR XIA IN COMPLEX WITH THE INHIBITOR methyl [(3R,7S)-7-({(2E)-3-[5-chloro-2-(1H-tetrazol-1-yl)phenyl]prop-2-enoyl}amino)-3-ethyl-2-oxo-1,2,3,4,5,6,7,9-octahydro-11,8-(azeno)-1,9-benzodiazacyclotridecin-14-yl]carbamate

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU FR-E SUPERBRIGHT
Temperature [K]	100
Detector technology	CCD
Collection date	2010-04-14
Detector	RIGAKU SATURN 92
Wavelength(s)	1.54
Spacegroup name	P 32 2 1
Unit cell lengths	78.900, 78.900, 105.900
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	21.020 - 2.600
R-factor	0.1874
Rwork	0.184
R-free	0.22930
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	FACTOR XIA DOUBLE MUTANT
RMSD bond length	0.010
RMSD bond angle	1.160
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	AMoRE
Refinement software	BUSTER (2.11.4)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	2.690
High resolution limit [Å]	2.600	2.600
Number of reflections	12188
<I/σ(I)>	16.8	5.6
Completeness [%]	99.9	100
Redundancy	10.7	10.9

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7	277	100 mM sodium acetate, pH 4.6, 25% (w/v) MePEG2000, 200 mM ammonium sulfate, then transferred to 100 mM Tris-HCl, pH 7.0, 25% (w/v) MePEG2000, 200 MM ammonium sulfate