2Y80

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	APS BEAMLINE 14-BM-D
Synchrotron site	APS
Beamline	14-BM-D
Temperature [K]	100
Detector technology	CCD
Collection date	2004-11-19
Detector	ADSC QUANTUM 4
Spacegroup name	P 21 21 21
Unit cell lengths	56.727, 72.012, 78.689
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	20.000 - 1.900
R-factor	0.1916
Rwork	0.189
R-free	0.24123
Structure solution method	OTHER
Starting model (for MR)	NONE
RMSD bond length	0.010
RMSD bond angle	1.395
Data reduction software	DENZO
Data scaling software	SCALEPACK
Refinement software	REFMAC (5.5.0109)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	25.000	1.930
High resolution limit [Å]	1.900	1.900
Rmerge	0.060	0.440
Number of reflections	25983
<I/σ(I)>	20.91	3.19
Completeness [%]	99.8	99.8
Redundancy	5.3	5.1

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.