4JIK

X-RAY Crystal structure of compound 22a (R)-2-(4-chlorophenyl)-8-(piperidin-3-ylamino)imidazo[1,2-c]pyrimidine-5-carboxamide bound to human chk1 kinase domain

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 17-ID
Synchrotron site	APS
Beamline	17-ID
Temperature [K]	100
Detector technology	CCD
Collection date	2008
Detector	ADSC QUANTUM 210r
Wavelength(s)	1.0
Spacegroup name	P 1 21 1
Unit cell lengths	45.110, 65.900, 54.760
Unit cell angles	90.00, 102.74, 90.00

Refinement procedure

Resolution	50.000 - 1.900
R-factor	0.211
Rwork	0.211
R-free	0.23700
Structure solution method	FOURIER SYNTHESIS
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	BUSTER
Refinement software	BUSTER

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	1.930
High resolution limit [Å]	1.900	1.900
Rmerge		0.370
Number of reflections	23586
<I/σ(I)>	20.7	3.1
Completeness [%]	95.0	85.2
Redundancy	2.9	2.5

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, 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 to 12% PEG 3.25K 2.5 mM TCEP-Cl 10 mM Na2-Dithionite, VAPOR DIFFUSION, HANGING DROP, temperature 298K