6XUE

Human Ecto-5'-nucleotidase (CD73) in complex with A2396 (compound 74 in publication) in the closed form in crystal form IV

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	2017-10-06
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.91840
Spacegroup name	P 21 21 2
Unit cell lengths	94.019, 232.175, 54.830
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	28.300 - 1.940
R-factor	0.19
Rwork	0.190
R-free	0.21900
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	4h2i
RMSD bond length	0.010
RMSD bond angle	1.080
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	autoBUSTER
Refinement software	BUSTER (2.10.3)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	28.300	28.300	2.050
High resolution limit [Å]	1.940	5.770	1.940
Rmerge	0.103	0.026	2.297
Rmeas	0.109	0.029	2.373
Total number of observations	868437
Number of reflections	90087	6515	27325
<I/σ(I)>	15.27	44.8	0.96
Completeness [%]	99.6	99.6	97.8
Redundancy	9.66	5.059	9.73
CC(1/2)	0.999	1.000	0.477

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP		291	Reservoir: 13 % PEG 6000, 0.1 M MES pH 6.0. Drop: 1 micro-L crystallization buffer + 1 micro-L of 3 mg/mL CD73 in 10 mM Tris pH 8.0, 10 micro-M ZnCl2, 3 % DMSO, compound: saturated solution. Cryo: 20% PEG200 in crystallization drop.