5JUN

PB2 bound to an azaindole inhibitor

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SSRL BEAMLINE BL7-1
Synchrotron site	SSRL
Beamline	BL7-1
Temperature [K]	100
Detector technology	CCD
Collection date	2011-07-19
Detector	MAR CCD 165 mm
Wavelength(s)	0.979460
Spacegroup name	P 65
Unit cell lengths	81.360, 81.360, 54.820
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	29.640 - 2.690
R-factor	0.176
Rwork	0.176
R-free	0.18900
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	4nce
RMSD bond length	0.010
RMSD bond angle	1.130
Data scaling software	SCALA (3.3.15)
Refinement software	BUSTER-TNT (2.11.6)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	29.640	25.549	2.740
High resolution limit [Å]	2.598	8.210	2.600
Rmerge		0.013	0.545
Number of reflections	6190
<I/σ(I)>	23.2	45	1.4
Completeness [%]	95.4	96.4	99.9
Redundancy	4.9	4.7	4.7

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	4.7	293	1 uL protein solution (2.8 mg/mL protein, 50 mM Tris, pH 8, 200 mM sodium chloride, 2 mM dithiothreitol, 1 mM anthraquinone-2,6-disulfonic acid disodium salt, 7.5 mM GTP) + 0.4 uL well solution (1.5 M sodium formate, 100 mM sodium citrate, pH 4.7, 10 mM dithiothreitol) suspended over 1 mL of well solution, crystals transferred to a soaking solution (3.25 M sodium formate, 100 mM sodium citrate, pH 4.7) containing 1 mM inhibitor, incubated approximately 15 hours at room temperature, and then transferred to a cryo-preservative solution (soaking solution with 25% v/v glycerol) prior to freezing in liquid nitrogen