5WH5

Crystal structure of the PDE4D2 catalytic domain in complex with inhibitor (R)-Zl-n-91

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	NSLS BEAMLINE X29A
Synchrotron site	NSLS
Beamline	X29A
Temperature [K]	100
Detector technology	CCD
Collection date	2008-04-24
Detector	Bruker AXIOM 200
Wavelength(s)	1.0
Spacegroup name	P 21 21 21
Unit cell lengths	59.467, 79.883, 163.444
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	30.000 - 1.800
R-factor	0.1941
Rwork	0.193
R-free	0.21410
RMSD bond length	0.005
RMSD bond angle	0.952
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	AMoRE
Refinement software	REFMAC (5.8.0073)

Data quality characteristics

	Overall
Low resolution limit [Å]	81.720
High resolution limit [Å]	1.800
Number of reflections	69331
<I/σ(I)>	8.8
Completeness [%]	94.6
Redundancy	13.2

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	EVAPORATION	7.5	277	The ~10mg/ml PDE4D2 (86-413) was stored in a buffer of 20 mM Tris.base, pH 7.5, 50 mM NaCl, 1 mM 2-mercaptoethanol, 1 mM EDTA and mixed with 2 mM (R)- or (S)-5. They were crystallized at 4C by hanging drop against a well buffer of 0.1 M HEPES pH 7.5, 15% PEG3350, 30% ethylene glycol, and 10% isopropanol.