5SKM

CRYSTAL STRUCTURE OF HUMAN PHOSPHODIESTERASE 10 IN COMPLEX WITH [C@H]3(CCc2nc1ccc(Cl)cc1c(n2)N(C)C)CCN(C3)c4ccccn4, micromolar IC50=0.014172

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	2011-05-14
Detector	PSI PILATUS 6M
Wavelength(s)	1.000000
Spacegroup name	H 3
Unit cell lengths	136.021, 136.021, 236.102
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	43.750 - 1.910
R-factor	0.1817
Rwork	0.180
R-free	0.22130
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.013
RMSD bond angle	1.862
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]	43.750	43.750	1.960
High resolution limit [Å]	1.910	8.540	1.910
Rmerge	0.071	0.023	1.529
Rmeas	0.079	0.025	1.697
Total number of observations	653256
Number of reflections	126375	1394	9368
<I/σ(I)>	10.79	47.79	1.08
Completeness [%]	100.0	99.3	100
Redundancy	5.21	5.496	5.311
CC(1/2)	0.999	0.999	0.438

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