7PA4

Crystal structure of CD73 in complex with CMP in the open form

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	CCD
Collection date	2016-06-23
Detector	RAYONIX MX-225
Wavelength(s)	0.9184
Spacegroup name	P 21 21 2
Unit cell lengths	67.569, 131.676, 66.493
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	47.440 - 1.450
R-factor	0.1207
Rwork	0.118
R-free	0.16090
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	4h2g
RMSD bond length	0.015
RMSD bond angle	1.914
Data reduction software	XDS
Data scaling software	Aimless (0.7.4)
Phasing software	REFMAC
Refinement software	REFMAC (5.8.0267)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	47.440	47.390	1.480
High resolution limit [Å]	1.450	7.950	1.450
Rmerge	0.071	0.032	0.629
Rmeas	0.078	0.035	0.771
Rpim	0.031	0.015	0.428
Total number of observations		4178	10006
Number of reflections	99435	751	3323
<I/σ(I)>	16.9	48.2	1.9
Completeness [%]	94.3	99.2	64.7
Redundancy	5.9	5.6	3
CC(1/2)	0.999	0.999	0.600

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.8	292	7 mg/mL protein concentration, 100 mM Tris pH 7.8, 10 % PEG6000, equal amounts of protein and reservoir. Following crystal formation (1-2 days), the crystals were transferred to soaking solution containing reservoir solution and 100 mM CMP. Crystals were then transferred to cryo solution containing an additional 20 % glycerol, soaked for ~2-5 min, and flash frozen in liquid nitrogen.