6ASQ

Structure of Grp94 bound to methyl 2-[2-(2-benzylpyridin-3-yl)ethyl]-3-chloro-4,6-dihydroxybenzoate, a pan-Hsp90 inhibitor

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 22-BM
Synchrotron site	APS
Beamline	22-BM
Temperature [K]	197.5
Detector technology	CCD
Collection date	2016-10-21
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	1.00000
Spacegroup name	P 21 21 21
Unit cell lengths	65.431, 84.717, 95.759
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	42.359 - 2.350
R-factor	0.2001
Rwork	0.197
R-free	0.23670
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2gfd
RMSD bond length	0.004
RMSD bond angle	0.800
Data reduction software	HKL-3000
Data scaling software	HKL-3000
Phasing software	PHASER
Refinement software	PHENIX ((1.10.1_2155: ???))

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	42.360	2.434
High resolution limit [Å]	2.350	2.350
Rmerge	0.094	0.477
Number of reflections	22770
<I/σ(I)>	24.75
Completeness [%]	100.0
Redundancy	14.3

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.8	289.2	1:1 30 mg/mL protein in 100 mM bicine, pH 7.8 against mother liquor (37% PEG400, 5% glycerol, 100 mM bicine, pH 7.8, 75 mM magnesium chloride). Crystals were harvested, and soaked for 48 hours in mother liquor containing 2.5 mM inhibitor. After soaking, glycerol was added to ~25% final concentration.