5WH6

Crystal structure of PDE4D2 in complex with inhibitor (S_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	58.948, 80.197, 163.670
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	30.000 - 1.600
R-factor	0.20707
Rwork	0.206
R-free	0.22430
RMSD bond length	0.005
RMSD bond angle	0.924
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]	81.000
High resolution limit [Å]	1.600
Rmerge	0.068
Number of reflections	95949
<I/σ(I)>	10.5
Completeness [%]	93.1
Redundancy	12.6

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.