6BOJ

Crystal Structure of the PDE4D Catalytic Domain and UCR2 Regulatory Helix with BPN5004

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 21-ID-F
Synchrotron site	APS
Beamline	21-ID-F
Temperature [K]	100
Detector technology	CCD
Collection date	2012-10-24
Detector	MARMOSAIC 300 mm CCD
Wavelength(s)	0.97872
Spacegroup name	P 1 21 1
Unit cell lengths	81.780, 81.890, 116.790
Unit cell angles	90.00, 110.41, 90.00

Refinement procedure

Resolution	45.500 - 1.700
R-factor	0.162
Rwork	0.161
R-free	0.18600
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.014
RMSD bond angle	1.408
Data reduction software	XDS
Data scaling software	XSCALE
Refinement software	REFMAC (5.7.0029)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	1.740
High resolution limit [Å]	1.700	1.700
Rmerge	0.085	0.499
Number of reflections	154546	11253
<I/σ(I)>	11.85	3
Completeness [%]	97.3	95.8
Redundancy	5.2	5.1

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.5	289	5.0mg/ml of PDE4D-UCR2 (CID7620) + 0.5mM BPN5004 against 8.75% w/v PEG1,000, 6.25% w/v PEG3,350, 6.25% w/v MPD, 0.015M NPS (sodium nitrate, disodium hydrogen phosphate, ammonium sulfate), 0.05M MOPS/HEPES-Na pH 7.5, 20% v/v ethanol, 0.05M Phosphate-citrate pH 4.2