7P9T

Crystal structure of CD73 in complex with dCMP 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	2016-10-04
Detector	RAYONIX MX-225
Wavelength(s)	0.8943
Spacegroup name	P 21 21 2
Unit cell lengths	68.104, 132.846, 67.404
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	47.950 - 1.790
R-factor	0.1868
Rwork	0.185
R-free	0.21680
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	4h2g
RMSD bond length	0.013
RMSD bond angle	1.900
Data reduction software	XDS
Data scaling software	Aimless (0.7.7)
Phasing software	REFMAC
Refinement software	REFMAC (5.8.0267)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	47.950	47.910	1.820
High resolution limit [Å]	1.790	9.120	1.790
Rmerge	0.107	0.025	0.994
Rmeas	0.122	0.029	1.140
Rpim	0.059	0.015	0.551
Number of reflections	58377	489	3288
<I/σ(I)>	11.1
Completeness [%]	99.7	94.6	99.1
Redundancy	4.1	3.4	4.1
CC(1/2)	0.997	0.999	0.546

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP		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 50 mM dCMP. Crystals were then transferred to cryo solution containing an additional 20 % glycerol, soaked for ~2-5 min, and flash frozen in liquid nitrogen.