5SKN

CRYSTAL STRUCTURE OF HUMAN PHOSPHODIESTERASE 10 IN COMPLEX WITH n1(nccc1C3=NN(c2cccc(c2)NC(=O)C)C=CC3=O)c4ccccc4F, micromolar IC50=0.021094

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	2009-04-14
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	1.000000
Spacegroup name	H 3
Unit cell lengths	135.480, 135.480, 235.361
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	35.030 - 1.900
R-factor	0.1928
Rwork	0.191
R-free	0.22240
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.005
RMSD bond angle	1.284
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]	35.000	35.030	1.950
High resolution limit [Å]	1.900	8.500	1.900
Rmerge	0.052	0.023	1.110
Rmeas	0.061	0.027	1.380
Total number of observations	465604
Number of reflections	125596	1191	8600
<I/σ(I)>	15.26	47.76	1.09
Completeness [%]	98.9	84.2	91.5
Redundancy	3.707	3.531	2.571
CC(1/2)	0.999	0.998	0.422

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