5SE4

CRYSTAL STRUCTURE OF HUMAN PHOSPHODIESTERASE 10 IN COMPLEX WITH c1(cc(nc2nc(nn12)CCc3nc(cn3C)c4ccccc4)C5CC5)C, micromolar IC50=0.001357

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SLS BEAMLINE X10SA
Synchrotron site	SLS
Beamline	X10SA
Temperature [K]	100
Detector technology	PIXEL
Collection date	2010-06-24
Detector	PSI PILATUS 6M
Wavelength(s)	1.000000
Spacegroup name	H 3
Unit cell lengths	135.738, 135.738, 236.149
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	43.820 - 2.500
R-factor	0.1887
Rwork	0.185
R-free	0.25190
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.009
RMSD bond angle	1.722
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]	43.820	43.820	2.560
High resolution limit [Å]	2.500	11.180	2.500
Rmerge	0.165	0.061	1.417
Rmeas	0.184	0.068	1.583
Total number of observations	285035
Number of reflections	56076	618	4158
<I/σ(I)>	6.65	17.97	1.21
Completeness [%]	99.9	98.4	99.9
Redundancy	5.083	4.977	5.032
CC(1/2)	0.992	0.995	0.332

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