3SX4

Crystal structure of human dpp-iv in complex with sa-(+)-3-(aminomethyl)-4-(2,4-dichlorophenyl)-6-(2-methoxyphenyl)- 2-methyl-5h-pyrrolo[3,4-b]pyridin-7(6h)-one

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	2005-06-08
Detector	ADSC Q315
Spacegroup name	P 21 21 21
Unit cell lengths	65.905, 67.854, 422.095
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.096 - 2.600
R-factor	0.2061
Rwork	0.203
R-free	0.27500
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3NOX.PDB
RMSD bond length	0.008
RMSD bond angle	1.189
Data reduction software	HKL-2000 ((DENZO))
Data scaling software	HKL-2000 ((SCALEPACK))
Phasing software	AMoRE
Refinement software	PHENIX (dev_780)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	2.690
High resolution limit [Å]	2.600	2.600
Rmerge	0.097	0.539
Number of reflections	57759
<I/σ(I)>	19.4	1.8
Completeness [%]	96.5	74.5
Redundancy	7.7	4.3

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	8.5	298	CRYSTALS GROWN IN 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-STORED IN LN2. 2. For crystal 2: