3QI1

Design and synthesis of hydroxyethylamine (hea) BACE-1 inhibitors: prime side chromane-containing inhibitors

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU MICROMAX-007
Temperature [K]	100
Detector technology	IMAGE PLATE
Collection date	2010-07-30
Detector	RIGAKU RAXIS HTC
Spacegroup name	P 21 21 21
Unit cell lengths	72.174, 75.506, 80.236
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	25.690 - 2.300
R-factor	0.20191
Rwork	0.198
R-free	0.26878
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.022
RMSD bond angle	1.867
Data reduction software	CrystalClear
Data scaling software	CrystalClear
Phasing software	MOLREP
Refinement software	REFMAC (5.5.0109)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	25.690	2.380
High resolution limit [Å]	2.300	2.300
Rmerge	0.086	0.406
Number of reflections	19292
<I/σ(I)>	9.2	2.3
Completeness [%]	96.2	99.8
Redundancy	3.89	3.86

Crystallization Conditions

crystal ID	method	pH	temperature	details
1		4.6	295	BACE PROTEIN AT 10MG/ML IN 100MM SODIUM BORATE BUFFER PH 8.5. 1MM COMPOUND ADDED TO PROTEIN AND INCUBATED AT 4 C FOR 3 HOURS. HANGING DROP PLATES SET UP WITH RESERVOIR SOLUTION CONTAINING 4% PEG 8000, 100MM SODIUM ACETATE PH 4.6 THE DROPS WERE MIXED WITH 1:1 (V/V) RATIO OF PROTEIN/COMPOUND TO RESERVOIR AND INCUBATED AT ROOM TEMPERATURE FOR 2 WEEKS. VAPOR DIFFUSION, HANGING DROP, TEMPERATURE 295K