5SIX

CRYSTAL STRUCTURE OF HUMAN PHOSPHODIESTERASE 10 IN COMPLEX WITH c1(cc(nc2cc(nn12)c3c(nc4c(n3)cccc4)C)N5CC[C@H](C5)F)NC6CCOCC6, micromolar IC50=0.007291

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	2013-05-04
Detector	PSI PILATUS 6M
Wavelength(s)	0.999960
Spacegroup name	I 2 3
Unit cell lengths	141.343, 141.343, 141.343
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	44.700 - 2.290
R-factor	0.1841
Rwork	0.182
R-free	0.21890
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.007
RMSD bond angle	1.423
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]	44.700	44.700	2.350
High resolution limit [Å]	2.290	10.240	2.290
Rmerge	0.099	0.029	2.062
Rmeas	0.101	0.030	2.114
Total number of observations	428846
Number of reflections	21279	264	1593
<I/σ(I)>	24.97	105.24	1.75
Completeness [%]	100.0	98.5	100
Redundancy	20.153	18.795	20.653
CC(1/2)	1.000	1.000	0.700

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