5SEK

CRYSTAL STRUCTURE OF HUMAN PHOSPHODIESTERASE 10 IN COMPLEX WITH c1ccc2c(c1)nc(c(n2)C)CCc3nc(cn3C)c4ccccc4, micromolar IC50=0.005172

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	2010-09-17
Detector	PSI PILATUS 6M
Wavelength(s)	0.999900
Spacegroup name	H 3
Unit cell lengths	135.629, 135.629, 236.677
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	43.630 - 2.150
R-factor	0.1652
Rwork	0.164
R-free	0.19710
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.003
RMSD bond angle	1.170
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]	43.630	43.630	2.210
High resolution limit [Å]	2.150	9.620	2.150
Rmerge	0.152	0.090	1.160
Rmeas	0.170	0.100	1.284
Total number of observations	462869
Number of reflections	88274	992	6521
<I/σ(I)>	6.9	15.64	1.43
Completeness [%]	100.0	99.1	100
Redundancy	5.244	5.299	5.433
CC(1/2)	0.989	0.987	0.398

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