5SIB

Crystal Structure of human phosphodiesterase 10 in complex with 3-methyl-6-[2-(2-methyl-5-pyrrolidin-1-yl-1,2,4-triazol-3-yl)ethyl]-2-(trifluoromethyl)imidazo[1,2-b]pyridazine

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	2012-01-31
Detector	PSI PILATUS 6M
Wavelength(s)	0.700010
Spacegroup name	H 3
Unit cell lengths	135.556, 135.556, 235.636
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	43.730 - 2.540
R-factor	0.1753
Rwork	0.172
R-free	0.24860
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.009
RMSD bond angle	1.614
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]	43.730	43.730	2.610
High resolution limit [Å]	2.540	11.360	2.540
Rmerge	0.150	0.026	1.293
Rmeas	0.167	0.029	1.434
Total number of observations	281927
Number of reflections	53250	589	3945
<I/σ(I)>	8.64	47.07	1.11
Completeness [%]	100.0	98.5	100
Redundancy	5.294	5.389	5.376
CC(1/2)	0.996	0.999	0.399

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