3DUY

Crystal structure of human beta-secretase in complex with NVP-AFJ144

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU FR-E SUPERBRIGHT
Temperature [K]	100
Detector technology	CCD
Collection date	2005-11-18
Detector	RIGAKU SATURN 92
Wavelength(s)	1.54178
Spacegroup name	P 1 21 1
Unit cell lengths	82.537, 103.062, 100.602
Unit cell angles	90.00, 103.64, 90.00

Refinement procedure

Resolution	70.930 - 1.970
R-factor	0.204
Rwork	0.202
R-free	0.22300
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1fkn
RMSD bond length	0.005
RMSD bond angle	0.800
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	CNX
Refinement software	CNS

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	70.930	2.030
High resolution limit [Å]	1.970	1.970
Rmerge	0.068	0.395
Number of reflections	107931	6065
<I/σ(I)>	22.55	3.8
Completeness [%]	93.5	61.7
Redundancy	10.2	4.7

Crystallization Conditions

crystal ID	method	pH	temperature	details
1				1.0M Ammonium sulfate in water, pH 5.5, VAPOR DIFFUSION, HANGING DROP, temperature 292K. Protein stock was BACE MUT46B batch XII 8.5 mg/mL in 10mM Tris-HCl pH 7.4, 25mM NaCl, with a 5-fold excess of NVP-AFJ144-NX-2 added from a 50mM stock solution in 90% DMSO-D6 (1.8% DMSO in drop). A solution containing 1.2M Ammonium sulfate, 25% Glycerol, 1mM NVP-AFJ144-NX-2 and 1.8% DMSO was used as cryo-protectant