6XUQ

Human Ecto-5'-nucleotidase (CD73) in complex with A1618 (compound 1b in publication) in the closed state in 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	2018-03-02
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.91841
Spacegroup name	C 2 2 21
Unit cell lengths	53.090, 93.850, 235.660
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.210 - 1.970
R-factor	0.213
Rwork	0.212
R-free	0.23900
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	4h2i
RMSD bond length	0.010
RMSD bond angle	1.190
Data reduction software	XDS
Data scaling software	XDS
Phasing software	BUSTER (2.10.3)
Refinement software	BUSTER (2.10.3)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	47.130	47.130	2.090
High resolution limit [Å]	1.970	5.870	1.970
Rmerge	0.120	0.032	3.381
Rmeas	0.142	0.038	3.984
Number of reflections	80202	3020	12856
<I/σ(I)>	6.81	32.26	0.37
Completeness [%]	99.6	99.5	99.2
Redundancy	3.482	3.53	3.528
CC(1/2)	0.998	0.999	0.135

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	8	291	Reservoir: 7.5 % PEG 6.000, 0.1 M MES pH 6.2. 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 and 1 mM of compound. Cryo: 20% PEG200 in crystallization drop