3PA5

X-ray crystal structure of compound 1 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	44.840, 65.850, 58.250
Unit cell angles	90.00, 94.68, 90.00

Refinement procedure

Resolution	19.000 - 1.700
Rwork	0.185
R-free	0.20400
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	1.730
High resolution limit [Å]	1.700	4.610	1.700
Rmerge	0.075	0.063	0.439
Rmeas	0.075
Total number of observations	120752
Number of reflections	37091
<I/σ(I)>	17.8
Completeness [%]	99.8	98.6	99.9
Redundancy	3.3	3.2	2.9

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