3PA4

X-ray crystal structure of compound 2a bound to human CHK1 kinase domain

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	CHESS BEAMLINE A1
Synchrotron site	CHESS
Beamline	A1
Temperature [K]	100
Detector technology	CCD
Collection date	2006-05-15
Detector	ADSC QUANTUM 210
Wavelength(s)	0.97900
Spacegroup name	P 1 21 1
Unit cell lengths	44.920, 65.850, 58.270
Unit cell angles	90.00, 94.93, 90.00

Refinement procedure

Resolution	28.000 - 1.590
Rwork	0.225
R-free	0.25000
Structure solution method	FOURIER SYNTHESIS
Data reduction software	DENZO
Data scaling software	SCALEPACK
Refinement software	BUSTER-TNT

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	1.630
High resolution limit [Å]	1.590	4.340	1.590
Rmerge	0.066	0.048	0.418
Number of reflections	44486
<I/σ(I)>	11.9
Completeness [%]	98.3	93.1	98.1
Redundancy	2.9	2.8	2.8

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	hanging drop	7.5	298	0.1 M Tris-Cl pH 7.5, 1% v/v n-butanol, 2.5% v/v DMSO, 25% v/v Glycerol, 6-12% PEG 3.25K, 2.5 mM TCEP-Cl, 10 mM Na2-Dithionite, hanging drop, temperature 298K