6DFM

Crystal structure of human GRP78 in complex with 8-aminoadenosine

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	55.662, 74.775, 89.485
Unit cell angles	90.00, 99.48, 90.00

Refinement procedure

Resolution	31.170 - 2.140
R-factor	0.189
Rwork	0.187
R-free	0.23100
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.010
RMSD bond angle	1.090
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]	88.263	44.254	2.260
High resolution limit [Å]	2.140	6.770	2.140
Rmerge		0.042	0.639
Rmeas	0.108	0.046	0.694
Rpim	0.041	0.018	0.268
Number of reflections	39667	1308	5550
<I/σ(I)>	12.3	13.7	1.2
Completeness [%]	99.2	99.3	95.4
Redundancy	6.8	6.3	6.5

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-aminoadenosine for one week.