6DFO

Crystal structure of human GRP78 in complex with 8-bromoadenosine

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 23-ID-D
Synchrotron site	APS
Beamline	23-ID-D
Temperature [K]	173
Detector technology	PIXEL
Collection date	2017-06-16
Detector	DECTRIS PILATUS 6M
Wavelength(s)	1.03327
Spacegroup name	P 1 21 1
Unit cell lengths	55.556, 74.734, 89.670
Unit cell angles	90.00, 98.78, 90.00

Refinement procedure

Resolution	28.690 - 2.540
R-factor	0.19
Rwork	0.187
R-free	0.25100
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.010
RMSD bond angle	1.150
Data reduction software	XDS (INTEL64_Linux_x86_64)
Data scaling software	SCALA (3.3.21)
Phasing software	MOLREP
Refinement software	BUSTER (2.10.2)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	88.620	44.310	2.680
High resolution limit [Å]	2.540	8.050	2.540
Rmerge		0.056	0.566
Rmeas	0.133	0.062	0.613
Rpim	0.051	0.024	0.233
Number of reflections	23826	792	3319
<I/σ(I)>	11.3	9.8	1.4
Completeness [%]	99.2	99.4	95.1
Redundancy	6.7	6.3	6.7

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	8.5	298	Triclinic crystals of apo GRP78 were observed in 0.1 M Tris-HCl, 25% PEG3350, 0.1 M sodium/potassium tartrate. Initial crystals were then microseeded in 25% PEG3350, 0.1 M Tris-HCl, 0.2 M sodium chloride. These new apo monoclinic crystals were soaked with 5 mM 8-bromoadenosine for one week.