3QD4

Phosphoinositide-Dependent Kinase-1 (PDK1) kinase domain with 1,1-Dimethylethyl{(3R,5R)-1-[2-amino-6-(3-amino-1H-indazol-6-yl)-4-pyrimidinyl]-5-methyl-3-piperidinyl}carbamate

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 21-ID-G
Synchrotron site	APS
Beamline	21-ID-G
Temperature [K]	110
Detector technology	CCD
Collection date	2009-10-12
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.97872
Spacegroup name	P 32 2 1
Unit cell lengths	124.315, 124.315, 47.017
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	29.859 - 2.300
R-factor	0.1989
Rwork	0.194
R-free	0.24390
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.008
RMSD bond angle	1.218
Data reduction software	DENZO
Data scaling software	SCALEPACK
Refinement software	PHENIX (1.5_2)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	30.000	30.000	2.380
High resolution limit [Å]	2.300	4.950	2.300
Rmerge	0.078	0.037	0.582
Number of reflections	18792
<I/σ(I)>	9.3
Completeness [%]	99.9	99.4	100
Redundancy	7.1	7.1	6.5

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