3O56

Catalytic domain of human phosphodiesterase 4b2b in complex with a 5-heterocycle pyrazolopyridine inhibitor

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID14-4
Synchrotron site	ESRF
Beamline	ID14-4
Temperature [K]	100
Detector technology	CCD
Collection date	2004-02-05
Detector	ADSC QUANTUM 4
Wavelength(s)	0.9393
Spacegroup name	I 21 21 21
Unit cell lengths	88.531, 94.592, 105.089
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	20.000 - 2.420
R-factor	0.1993
Rwork	0.196
R-free	0.26010
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	3d3p
RMSD bond length	0.014
RMSD bond angle	1.325
Data reduction software	MOSFLM
Data scaling software	SCALA (3.1.20)
Phasing software	REFMAC
Refinement software	REFMAC

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	29.703	29.703	2.480
High resolution limit [Å]	2.420	10.820	2.420
Rmerge	0.094	0.089	0.379
Total number of observations		795	9170
Number of reflections	17117
<I/σ(I)>	16.5	6.6	2
Completeness [%]	99.6	79.6	100
Redundancy	7.2	4.6	7.3

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	6.5	277	14-18% PEG 3000, 10% Glycerol, 50mM Sodium Cacodylate pH 6.5, 100mM Sodium Acetate, 1M Sodium Chloride, 1% DMF, 5mM DTT, VAPOR DIFFUSION, SITTING DROP, temperature 277K