5TNO

Discovery of novel aminobenzisoxazole derivatives as orally available factor IXa inhibitors

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 17-ID
Synchrotron site	APS
Beamline	17-ID
Temperature [K]	95
Detector technology	PIXEL
Collection date	2012-07-14
Detector	DECTRIS PILATUS 6M
Wavelength(s)	1.0
Spacegroup name	H 3
Unit cell lengths	98.835, 98.835, 94.252
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	22.550 - 1.540
R-factor	0.145
Rwork	0.145
R-free	0.15800
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1rfn
RMSD bond length	0.010
RMSD bond angle	1.130
Data reduction software	XDS ((VERSION December 29))
Data scaling software	autoPROC
Phasing software	MOLREP
Refinement software	BUSTER (2.11.7)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	63.360	1.542
High resolution limit [Å]	1.537	1.537
Rmerge	0.030	0.524
Number of reflections	51117
<I/σ(I)>	25.7
Completeness [%]	99.9	100
Redundancy	5.1	5.2

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	9	295	50 MM CHES, PH 9.0, 1.3 M TRI-SODIUM CITRATE AND 3 MM COMPOUND (CROSS SEEDED WITH CRYSTALS GROWN FROM REMARK 280 50 MM TRIS, PH 7.2, 1.45 M AMMONIUM SULFATE, 2.0 M SODIUM REMARK 280 CHLORIDE AND 3 MM COMPOUND)