5SK8

CRYSTAL STRUCTURE OF HUMAN PHOSPHODIESTERASE 10 IN COMPLEX WITH C(Nc1ccc2c(c1)nc([nH]2)c3ccccc3)(=O)c4c(cnn4CCC)Cl, micromolar IC50=0.388979

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	2009-02-09
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	1.001500
Spacegroup name	I 2 3
Unit cell lengths	141.187, 141.187, 141.187
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	37.760 - 2.300
R-factor	0.1785
Rwork	0.176
R-free	0.23340
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.007
RMSD bond angle	1.360
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]	44.650	37.760	2.360
High resolution limit [Å]	2.300	10.290	2.300
Rmerge	0.109	0.024	1.183
Rmeas	0.120	0.027	1.295
Total number of observations	128457
Number of reflections	20880	255	1527
<I/σ(I)>	12.69	50.33	1.51
Completeness [%]	99.7	95.9	99.7
Redundancy	6.152	5.514	6.1
CC(1/2)	0.998	1.000	0.551

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