5SFK

CRYSTAL STRUCTURE OF HUMAN PHOSPHODIESTERASE 10 IN COMPLEX WITH c1(nc(ccc1Nc2cncnc2)C3CC3)C(=O)Nc4nn(CC(F)(F)F)cc4, micromolar IC50=0.00639

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SLS BEAMLINE X10SA
Synchrotron site	SLS
Beamline	X10SA
Temperature [K]	100
Detector technology	CCD
Collection date	2008-08-29
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.979000
Spacegroup name	H 3
Unit cell lengths	135.550, 135.550, 233.950
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	43.480 - 2.330
R-factor	0.1876
Rwork	0.184
R-free	0.24840
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.009
RMSD bond angle	1.571
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0258)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	43.480	43.480	2.390
High resolution limit [Å]	2.330	10.430	2.330
Rmerge	0.078	0.021	1.016
Rmeas	0.097	0.026	1.265
Total number of observations	196258
Number of reflections	67835	741	4864
<I/σ(I)>	10.81	41.73	1.14
Completeness [%]	99.3	96.7	95.9
Redundancy	2.893	2.848	2.75
CC(1/2)	0.997	0.998	0.379

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.5	295	5-20 mg/mL protein in 25mM HEPES/NaOH pH7.5, 150mM NaCl, 50mM BME mixed 1:1 with reservoir 0.1M HEPES/NaOH pH7.5, 30% PEG550MME, 50mM MgCl2