5TNT

Discovery of novel aminobenzisoxazole derivatives as orally available factor IXa inhibitors

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	CLSI BEAMLINE 08ID-1
Synchrotron site	CLSI
Beamline	08ID-1
Temperature [K]	95
Detector technology	CCD
Collection date	2013-05-26
Detector	RAYONIX MX-300
Wavelength(s)	0.979490
Spacegroup name	H 3
Unit cell lengths	99.084, 99.084, 94.680
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	20.500 - 1.400
R-factor	0.147
Rwork	0.146
R-free	0.16100
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 September 2)
Data scaling software	autoPROC
Phasing software	MOLREP
Refinement software	BUSTER (2.11.7)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	28.600	1.404
High resolution limit [Å]	1.400	1.400
Rmerge	0.092	0.446
Number of reflections	68182
<I/σ(I)>	11.7	3.4
Completeness [%]	99.8	91.3
Redundancy	5.6	5.6

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 CHLORIDE AND 3 MM COMPOUND)