5SEN

CRYSTAL STRUCTURE OF HUMAN PHOSPHODIESTERASE 10 IN COMPLEX WITH c4(c(C(=O)Nc3cn(c2nc1ccccc1cc2)cn3)n(C)nc4)C(=O)N5CCC5, micromolar IC50=0.000697

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	2009-06-02
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.999900
Spacegroup name	H 3
Unit cell lengths	135.313, 135.313, 234.965
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	28.450 - 2.040
R-factor	0.214
Rwork	0.212
R-free	0.25070
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.007
RMSD bond angle	1.417
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]	28.450	28.450	2.090
High resolution limit [Å]	2.040	9.120	2.040
Rmerge	0.076	0.030	1.079
Rmeas	0.089	0.037	1.277
Total number of observations	365549
Number of reflections	97435	948	7436
<I/σ(I)>	11.52	31.23	1.55
Completeness [%]	95.4	82.2	98
Redundancy	3.752	3.149	3.575
CC(1/2)	0.997	0.996	0.485

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