4J5P

Crystal Structure of a Covalently Bound alpha-Ketoheterocycle Inhibitor (Phenhexyl/Oxadiazole/Pyridine) to a Humanized Variant of Fatty Acid Amide Hydrolase

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SSRL BEAMLINE BL11-1
Synchrotron site	SSRL
Beamline	BL11-1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2011-01-19
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.979
Spacegroup name	P 32 2 1
Unit cell lengths	104.067, 104.067, 261.034
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	33.380 - 2.300
R-factor	0.22216
Rwork	0.220
R-free	0.26487
Structure solution method	MIR
Starting model (for MR)	3k84
RMSD bond length	0.016
RMSD bond angle	1.764
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	PHASER
Refinement software	REFMAC (5.7.0029)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	2.380
High resolution limit [Å]	2.300	2.300
Rmerge		0.900
Number of reflections	71819
<I/σ(I)>	11.8	1.2
Completeness [%]	97.4	88
Redundancy	6.4	2.8

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	5.5	287	50 mM MES, pH 5.5, 0.02% UM-LA, 15% PEG400, 4% polypropylene glycol P400, 13% xylitol, 1 mM DTT, 50 mM potassium chloride, 50 mM sodium fluoride, VAPOR DIFFUSION, SITTING DROP, temperature 287K