4Y86

Crystal structure of PDE9 in complex with racemic inhibitor C33

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	2014-08-22
Detector	ADSC QUANTUM 315
Wavelength(s)	1
Spacegroup name	P 41 21 2
Unit cell lengths	104.135, 104.135, 269.536
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	97.140 - 2.010
R-factor	0.22395
Rwork	0.223
R-free	0.24725
RMSD bond length	0.007
RMSD bond angle	1.067
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	AMoRE
Refinement software	REFMAC (5.8.0073)

Data quality characteristics

	Overall
Low resolution limit [Å]	100.000
High resolution limit [Å]	2.000
Number of reflections	96827
<I/σ(I)>	20.8
Completeness [%]	97.2
Redundancy	12.6

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.4	277	The PDE9A2 (8-10 mg/mL) in a buffer of 50 mM NaCl, 20 mM Tris-HCl, pH 7.5, 1 mM mercaptoethanol, and 1 mM EDTA was mixed with 2 mM C33 and crystallized against a well buffer of 1.8 - 2.0 M sodium formate.