6S7H

Human CD73 (5'-nucleotidase) in complex with PSB12489 (an AOPCP derivative) in the closed state

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.1
Synchrotron site	BESSY
Beamline	14.1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2013-10-15
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.918409
Spacegroup name	C 2 2 21
Unit cell lengths	53.830, 95.800, 233.590
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	29.200 - 1.850
R-factor	0.1812
Rwork	0.181
R-free	0.19890
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	4h2i
RMSD bond length	0.010
RMSD bond angle	1.130
Data reduction software	XDS (November 3, 2014)
Data scaling software	Aimless (0.2.8)
Refinement software	BUSTER (2.10.1)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	29.200	29.200	1.890
High resolution limit [Å]	1.850	9.060	1.850
Rmerge	0.113	0.019	3.640
Rmeas	0.122	0.021	3.986
Rpim	0.047	0.008	1.602
Total number of observations	334547
Number of reflections	49414	500	3187
<I/σ(I)>	12.7		0.6
Completeness [%]	94.8	97.4	99.8
Redundancy	6.8	6.4	6
CC(1/2)	0.999	1.000	0.285

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP		292.15	Crystallization buffer: 5 % (w/v) polyethylene glycol 6000, 0.1 M citric acid pH 5.0-6.0. Crystallization drop:1 uL crystallization buffer + 1 uL of 3 mg/mL protein in 10 mM Tris pH 8.0, 100 uM ZnCl2, 1 mM Inhibitor. Cryobuffer: 25 % (v/v) polyethylene glycol 200, 0.1 MES pH 5.5