5KYJ

Brain penetrant liver X receptor (LXR) modulators based on a 2,4,5,6-tetrahydropyrrolo[3,4-c]pyrazole core

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	NSLS BEAMLINE X29A
Synchrotron site	NSLS
Beamline	X29A
Temperature [K]	100
Detector technology	CCD
Collection date	2012-02-18
Detector	ADSC QUANTUM 315r
Wavelength(s)	1.075
Spacegroup name	P 21 21 21
Unit cell lengths	69.920, 100.930, 145.900
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	43.810 - 2.800
R-factor	0.20134
Rwork	0.199
R-free	0.25280
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	5i4v
RMSD bond length	0.011
RMSD bond angle	1.512
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	MOLREP
Refinement software	REFMAC (5.8.0071)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	43.810	2.872
High resolution limit [Å]	2.800	2.800
Number of reflections	24770
<I/σ(I)>	19.4	2.47
Completeness [%]	99.8	99.57
Redundancy	7.6	7.8

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	8	298	1uL of scLXRbeta-LBD/scRXRbeta-LBD @ 10 mg protein/ml in 20 mM Tris-HCl pH 8.0, 150 mM NaCl, 5 mM DTT containing 1mM ligand and less than 2%(v/v) DMSO was mixed with 1uL of reservoir solution (0.2M LiCl, 16-20%(w/v) PEG3350, 7-10%(v/v) ethylene glycol, 0.01M Strontium chloride) on a circular, silanized glass cover slide and inverted and sealed with silicon grease over a well of 200uL of reservoir solution. Crystallization plates were incubated at 23 deg C for 2-5 days before rods would appear measuring 50 to 100um long.