5TTZ

Crystal structure of Grp94 bound to isoform-selective inhibitor methyl 2-(2-(1-(4-bromobenzyl)-1H-imidazol-2-yl)ethyl)-3-chloro-4,6-dihydroxybenzoate

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 22-BM
Synchrotron site	APS
Beamline	22-BM
Temperature [K]	80
Detector technology	CCD
Collection date	2014-06-25
Detector	MARMOSAIC 300 mm CCD
Wavelength(s)	1
Spacegroup name	P 21 21 21
Unit cell lengths	65.237, 84.420, 95.473
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	47.736 - 2.707
R-factor	0.2076
Rwork	0.199
R-free	0.28550
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2gfd
RMSD bond length	0.010
RMSD bond angle	1.272
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	PHENIX (1.9_1692)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	47.740
High resolution limit [Å]	2.707
Rmerge	0.121	0.663
Number of reflections	217928
<I/σ(I)>	22.11
Completeness [%]	97.7
Redundancy	14.6

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.5	289.15	Protein at 30 mg/mL in 0.1 M Tris pH 7.5 was mixed 1:1 with mother liquor comprised of 35% PEG400, 0.1 M Tris pH 7.5, and 80 mM MgCl2. Crystals were harvested and soaked in mother liquor containing 20 mM inhibitor. A layer of glycerol was then added through which crystals were harvested and cryo-cooled in liquid nitrogen.