3PA3

X-ray crystal structure of compound 70 bound to human CHK1 kinase domain

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU FR-E SUPERBRIGHT
Temperature [K]	100
Detector technology	IMAGE PLATE
Collection date	2006-02-15
Detector	RIGAKU RAXIS IV
Wavelength(s)	1.54578
Spacegroup name	P 1 21 1
Unit cell lengths	44.910, 65.890, 58.180
Unit cell angles	90.00, 94.26, 90.00

Refinement procedure

Resolution	19.000 - 1.400
Rwork	0.193
R-free	0.21300
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	1.420
High resolution limit [Å]	1.400	3.802	1.400
Rmerge	0.050	0.052	0.306
Number of reflections	60050
<I/σ(I)>	28.1
Completeness [%]	90.2	87.4	36.2
Redundancy	2.4	2.7	1.4

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