5SG3

CRYSTAL STRUCTURE OF HUMAN PHOSPHODIESTERASE 10 IN COMPLEX WITH c1(ccc(cc1)[C@@H](C(N\\N=C\\c2cc(c(Br)c(c2)OC)OC)=O)OCC)N3CCOCC3, micromolar IC50=0.0063575

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	2010-07-18
Detector	PSI PILATUS 6M
Wavelength(s)	1.000000
Spacegroup name	H 3
Unit cell lengths	135.445, 135.445, 235.303
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	43.680 - 1.980
R-factor	0.1847
Rwork	0.182
R-free	0.22790
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.015
RMSD bond angle	2.000
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]	43.680	43.680	2.030
High resolution limit [Å]	1.980	8.850	1.980
Rmerge	0.087	0.023	1.313
Rmeas	0.096	0.026	1.462
Total number of observations	580438
Number of reflections	111944	1258	8272
<I/σ(I)>	13.55	54.05	1.28
Completeness [%]	99.9	99.1	99.9
Redundancy	5.185	5.041	5.18
CC(1/2)	0.999	0.999	0.447

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