3NOX

Crystal structure of human DPP-IV in complex with Sa-(+)-(6-(aminomethyl)-5-(2,4-dichlorophenyl)-7-methylimidazo[1,2-a]pyrimidin-2-yl)(morpholino)methanone

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	2006-03-11
Detector	ADSC Q315
Spacegroup name	P 21 21 21
Unit cell lengths	65.451, 67.072, 420.443
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	35.624 - 2.338
R-factor	0.1977
Rwork	0.196
R-free	0.26400
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3bjm
RMSD bond length	0.008
RMSD bond angle	1.158
Data reduction software	HKL-2000 ((DENZO))
Data scaling software	HKL-2000 ((SCALEPACK))
Phasing software	AMoRE
Refinement software	PHENIX ((PHENIX.REFINE: DEV_446))

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	2.430
High resolution limit [Å]	2.350	2.350
Rmerge	0.113
Number of reflections	68839
<I/σ(I)>	14	2.6
Completeness [%]	86.5	50.9
Redundancy	6.8	3.6

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	8.5	298	CRYSTALS GROWN FROM 2 UL EQUIVOLUME MIXTURE OF PROTEIN SOLUTION (0.1 M NACL, 20 MM TRIS-HCL BUFFER PH 7.8, 9.8 MG/ML PROTEIN) AND CRYSTALLIZATION SOLUTION (17% W/V PEG 3350, 15% W/V GLYCEROL, 200 MM MGCL2, 100 MM TRIS-HCL BUFFER PH 8.5). SUFFICIENT 100 MM LIGAND STOCK SOLUTION (NEAT DMSO) ADDED TO ACHIEVE 1 MM LIGAND CONCENTRATION. SOAKED OVERNIGHT. HARVESTED DIRECTLY AND CRYO-PRESERVED IN LN2., VAPOR DIFFUSION, HANGING DROP, temperature 298K