3VFE

Virtual Screening and X-Ray Crystallography for Human Kallikrein 6 Inhibitors with an Amidinothiophene P1 Group

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID23-1
Synchrotron site	ESRF
Beamline	ID23-1
Temperature [K]	100
Detector technology	CCD
Collection date	2007-05-20
Detector	ADSC QUANTUM 4
Wavelength(s)	0.933
Spacegroup name	P 21 21 21
Unit cell lengths	43.938, 47.909, 107.553
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	28.710 - 1.880
R-factor	0.195
Rwork	0.193
R-free	0.22300
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1lo6
RMSD bond length	0.004
RMSD bond angle	1.300
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	MOLREP
Refinement software	CNS

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	40.000	40.000	1.950
High resolution limit [Å]	1.880	4.050	1.880
Rmerge	0.058	0.030	0.268
Number of reflections	18779
<I/σ(I)>	9.8
Completeness [%]	97.9	93	97.2
Redundancy	2.9	2.8	2.8

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	hanging drop	8.5	291	0.20 M trimethylamine N-oxide, 0.1 M Tris-HCl pH8.5, 20% PEG MME 2000 and 10 mM benzamidine, hanging drop, temperature 291K