3H0B

Discovery of aminoheterocycles as a novel beta-secretase inhibitor class

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ALS BEAMLINE 5.0.2
Synchrotron site	ALS
Beamline	5.0.2
Temperature [K]	100
Detector technology	CCD
Collection date	2004-09-14
Detector	ADSC QUANTUM 4r
Wavelength(s)	1.0000
Spacegroup name	C 1 2 1
Unit cell lengths	221.178, 107.440, 65.084
Unit cell angles	90.00, 99.47, 90.00

Refinement procedure

Resolution	47.250 - 2.700
R-factor	0.222
Rwork	0.220
R-free	0.25100
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1tqf
RMSD bond length	0.004
RMSD bond angle	0.850
Data reduction software	DENZO
Data scaling software	SCALEPACK
Refinement software	REFMAC

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	47.250	50.000	2.800
High resolution limit [Å]	2.700	5.810	2.700
Rmerge	0.078	0.033	0.526
Number of reflections	41217
<I/σ(I)>	17.402
Completeness [%]	99.9	99.5	99.8
Redundancy	3.8	3.7	3.7

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.5	293	1.5M Lithium Sulfate, 0.1M HEPES pH 7.5; crystals were soaked in 1.5M Lithium Sulfate, 0.1M Na Citrate, pH 5.0, 0.5mM inhibitor, VAPOR DIFFUSION, SITTING DROP, temperature 293K