6Z9B

Human Ecto-5'-nucleotidase (CD73) in complex with AOPCP derivative A830 (compound 16 in publication) in the closed form (crystal form III)

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	2016-06-24
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.91840
Spacegroup name	C 2 2 21
Unit cell lengths	53.240, 96.450, 235.170
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.230 - 2.170
R-factor	0.21
Rwork	0.208
R-free	0.26300
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	pdbid 4H2I
RMSD bond length	0.010
RMSD bond angle	1.160
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	BUSTER
Refinement software	BUSTER (2.10.3)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	48.230	48.230	2.300
High resolution limit [Å]	2.170	6.450	2.170
Rmerge	0.223	0.072	0.836
Rmeas	0.243	0.079	0.915
Number of reflections	32496	1359	5072
<I/σ(I)>	8.61	28.9	1.8
Completeness [%]	99.2	99.3	96.4
Redundancy	6.425	6.121	6.038
CC(1/2)	0.990	0.998	0.837

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	5.5	291	CD73 at 7 mg/mL was incubated on ice for one hour with 1mM of the inhibitor and 0.1 mM ZnCl2. 1 uL of protein was mixed with 1 uL of 11-14% PEG6000 and 100 mM sodium citrate pH 5.4-5.6. For cryoprotection glycerol was added to a final concentration of 15 % to the reservoir buffer.