5SH4

CRYSTAL STRUCTURE OF HUMAN PHOSPHODIESTERASE 10 IN COMPLEX WITH c13c(cc2c(c1)OCO2)nc([nH]3)SCc4nc(c(c(c4C)C)OC)C, micromolar IC50=0.631687

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	135.463, 135.463, 235.433
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	43.570 - 2.220
R-factor	0.1974
Rwork	0.195
R-free	0.24530
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.007
RMSD bond angle	1.462
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]	43.570	43.570	2.280
High resolution limit [Å]	2.220	9.930	2.220
Rmerge	0.155	0.044	1.387
Rmeas	0.173	0.049	1.539
Total number of observations	414074
Number of reflections	79553	893	5900
<I/σ(I)>	8.99	27.67	1.23
Completeness [%]	100.0	99	100
Redundancy	5.205	5.327	5.379
CC(1/2)	0.994	0.997	0.352

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