6CPT

crystal structure of yeast caPDE2 in complex with IBMX

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 22-BM
Synchrotron site	APS
Beamline	22-BM
Temperature [K]	100
Detector technology	CCD
Collection date	2017-10-11
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	1
Spacegroup name	C 1 2 1
Unit cell lengths	138.190, 73.639, 64.954
Unit cell angles	90.00, 108.49, 90.00

Refinement procedure

Resolution	65.530 - 1.900
R-factor	0.19083
Rwork	0.190
R-free	0.21294
RMSD bond length	0.005
RMSD bond angle	0.976
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	AMoRE
Refinement software	REFMAC (5.8.0073)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	65.530	1.930
High resolution limit [Å]	1.900	1.900
Number of reflections	47636
<I/σ(I)>	14.5
Completeness [%]	97.4
Redundancy	7.2

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP		297	The 10-15 mg/ml full length caPDE2 (1-571) was stored in a buffer of 20 mM Tris.base, pH 7.5, 50 mM NaCl, 1 mM 2-mercaptoethanol, 1 mM EDTA and crystallized at room temperature by hanging drop against a well buffer of 50 mM MES, pH 6.5, 0.1 M ammonium sulfate, 6-10% PEG8000, or a buffer of 50 mM Na citrate pH 5.6, 0.1 M ammonium acetate, 5% glycerol, and 6-10% PEG3350. The caPDE2-IBMX complex was prepared by soaking the native crystal s in the crystallization buffer with 10 mM IBMX