3DV5

Crystal structure of human beta-secretase in complex with NVP-BAV544

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SLS BEAMLINE X06SA
Synchrotron site	SLS
Beamline	X06SA
Temperature [K]	96
Detector technology	CCD
Collection date	2004-04-15
Detector	MAR CCD 165 mm
Wavelength(s)	0.97933
Spacegroup name	P 1 21 1
Unit cell lengths	81.661, 103.353, 99.474
Unit cell angles	90.00, 103.72, 90.00

Refinement procedure

Resolution	55.230 - 2.100
R-factor	0.211
Rwork	0.192
R-free	0.22100
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	3dv1
RMSD bond length	0.007
RMSD bond angle	1.400
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	CNX
Refinement software	CNS

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	100.000	2.180
High resolution limit [Å]	2.100	2.100
Rmerge	0.068	0.402
Number of reflections	94339
<I/σ(I)>	8.5
Completeness [%]	99.5	95.7
Redundancy	6.3

Crystallization Conditions

crystal ID	method	pH	temperature	details
1				1.0M Ammonium phosphate, 0.1M Sodium citrate, VAPOR DIFFUSION, HANGING DROP, pH 5.1, temperature 292K. Protein stock was BACE 8.45 mg/mL in 10mM Tris-HCl pH 7.4, 25mM NaCl, with a 3.8-fold excess of NVP-BAV544-AA-1 added from a 50mM stock solution in DMSO (1.4% DMSO in drop). Cryo-protectant was 20% v/v 1,2-Propanediol, 80% Reservoir solution