5EGM

Development of a novel tricyclic class of potent and selective FIXa inhibitors

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU FR-E+ SUPERBRIGHT
Temperature [K]	95
Detector technology	IMAGE PLATE
Collection date	2013-01-30
Detector	RIGAKU RAXIS IV++
Wavelength(s)	1.541780
Spacegroup name	H 3
Unit cell lengths	99.298, 99.298, 94.685
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	23.250 - 1.841
R-factor	0.1492
Rwork	0.148
R-free	0.17140
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1rfn
RMSD bond length	0.010
RMSD bond angle	1.100
Data reduction software	XDS (VERSION September 2)
Data scaling software	autoPROC
Phasing software	MOLREP
Refinement software	BUSTER (2.11.5)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	41.470	1.848
High resolution limit [Å]	1.841	1.841
Rmerge	0.052	0.495
Number of reflections	29836
<I/σ(I)>	16	2.7
Completeness [%]	98.9	98.2
Redundancy	3.5	3.6

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 REMARK 280 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)