5SK1

CRYSTAL STRUCTURE OF HUMAN PHOSPHODIESTERASE 10 IN COMPLEX WITH c12nc(cn1ccc(n2)NC(c3c(C(=O)NC)cnn3C)=O)c4ccccc4, micromolar IC50=0.01331975

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	2009-04-03
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	1.007500
Spacegroup name	H 3
Unit cell lengths	134.851, 134.851, 234.435
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	41.370 - 2.300
R-factor	0.1874
Rwork	0.185
R-free	0.23840
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.008
RMSD bond angle	1.505
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]	41.370	41.370	2.360
High resolution limit [Å]	2.300	10.290	2.300
Rmerge	0.072	0.022	0.972
Rmeas	0.083	0.026	1.130
Total number of observations	274205
Number of reflections	70543	752	5220
<I/σ(I)>	13.72	51.63	1.46
Completeness [%]	99.9	94.5	100
Redundancy	3.887	3.632	3.865
CC(1/2)	0.999	0.999	0.520

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