3O57

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	APS BEAMLINE 17-ID
Synchrotron site	APS
Beamline	17-ID
Temperature [K]	100
Detector technology	CCD
Collection date	2004-11-20
Detector	ADSC QUANTUM 210
Wavelength(s)	1.0
Spacegroup name	I 21 21 21
Unit cell lengths	88.622, 94.907, 105.853
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	20.000 - 2.000
R-factor	0.1901
Rwork	0.187
R-free	0.23990
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	3d3p
RMSD bond length	0.017
RMSD bond angle	1.406
Data reduction software	MOSFLM
Data scaling software	SCALA (3.2.5)
Phasing software	REFMAC
Refinement software	REFMAC

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	29.794	52.926	2.110
High resolution limit [Å]	2.000	6.320	2.000
Rmerge	0.088	0.073	0.519
Total number of observations		4782	23834
Number of reflections	30473
<I/σ(I)>	15	7.3	1.1
Completeness [%]	99.9	98.2	99.9
Redundancy	5.4	4.7	5.4

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