4XXS

Crystal structure of BACE1 with a pyrazole-substituted tetrahydropyran thioamidine

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 17-ID
Synchrotron site	APS
Beamline	17-ID
Temperature [K]	83
Detector technology	PIXEL
Collection date	2012-03-29
Detector	DECTRIS PILATUS 6M
Wavelength(s)	1.0
Spacegroup name	P 61 2 2
Unit cell lengths	102.350, 102.350, 170.550
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	27.230 - 1.860
R-factor	0.1831
Rwork	0.182
R-free	0.20760
RMSD bond length	0.010
RMSD bond angle	1.080
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	BUSTER-TNT
Refinement software	BUSTER-TNT (BUSTER 2.11.2)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	1.890
High resolution limit [Å]	1.860	5.050	1.860
Rmerge	0.121	0.108
Total number of observations	770525
Number of reflections	44909
<I/σ(I)>	4.9
Completeness [%]	99.8	99.8	96.6
Redundancy	17.2	17.3	7.5

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	6.6	291	BACE1 lacking the pro-segment was concentrated to ~14 mg/mL in 20 mM Tris pH 7.4 and 250 mM NaCl. Crystallization was carried out by the vapor diffusion method against 200 mM sodium citrate tribasic dihydrate, 22% PEG 5K monomethyl ether and 200 mM ammonium iodide.