2Y82

Structure and property based design of factor Xa inhibitors: pyrrolidin-2-ones with aminoindane and phenylpyrrolidine P4 motifs

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID29
Synchrotron site	ESRF
Beamline	ID29
Temperature [K]	100
Detector technology	CCD
Collection date	2005-09-28
Detector	ADSC CCD
Spacegroup name	P 21 21 21
Unit cell lengths	56.693, 72.212, 78.759
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	20.000 - 2.200
R-factor	0.18116
Rwork	0.178
R-free	0.23332
Structure solution method	OTHER
RMSD bond length	0.010
RMSD bond angle	1.433
Data reduction software	MOSFLM
Data scaling software	SCALA
Refinement software	REFMAC (5.5.0109)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	53.220	2.310
High resolution limit [Å]	2.190	2.190
Rmerge	0.120	0.490
Number of reflections	17166
<I/σ(I)>	12.6	3.7
Completeness [%]	99.6	99.6
Redundancy	5.2	5.3

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION	5.75		CRYSTALLISATION WAS CARRIED OUT USING VAPOUR DIFFUSION IN 2UL DROPS CONTAINING A 1:1 MIXTURE OF PROTEIN AND WELL SOLUTION. WELL SOLUTION CONTAINED 16-20% PEG 6K, 50 MM MES-NAOH (PH 5.5-6), 5 MM CACL2 AND 50 MM NACL.