3QD3

Phosphoinositide-Dependent Kinase-1 (PDK1) kinase domain with 1,1-Dimethylethyl {(3R,6S)-1-[2-amino-6-(3-amino-1H-indazol-6-yl)-4-pyrimidinyl]-6-methyl-3-piperidinyl}carbamate

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 21-ID-F
Synchrotron site	APS
Beamline	21-ID-F
Detector technology	CCD
Collection date	2009-07-08
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.97872
Spacegroup name	P 32 2 1
Unit cell lengths	123.533, 123.533, 46.870
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	29.672 - 2.000
R-factor	0.1847
Rwork	0.183
R-free	0.21140
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.007
RMSD bond angle	1.171
Data scaling software	SCALEPACK
Refinement software	PHENIX (1.4_87)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	30.000	30.000	2.070
High resolution limit [Å]	2.000	4.310	2.000
Rmerge	0.101	0.043	0.573
Number of reflections	28038
<I/σ(I)>	9.4
Completeness [%]	100.0	100	100
Redundancy	7.4	7.2	7.1

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	9	293	1.9-2 M ammonium sulfate,0.1 M tris pH 9. and 5mM ATP; 15-30% glycerol plus mother liquor mixed with inhibitor served as the cryo-protectant before being frozen in liquid nitrogen, Vapor diffusion. sitting drop, temperature 293K