4PUU

Human Aldose Reductase complexed with a ligand with an IDD structure (2-(2-carbamoyl-5-fluoro-phenoxy)acetic acid) at 1.14 A

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.2
Synchrotron site	BESSY
Beamline	14.2
Temperature [K]	100
Detector technology	CCD
Collection date	2013-12-13
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	49.289, 66.394, 47.245
Unit cell angles	90.00, 91.82, 90.00

Refinement procedure

Resolution	17.322 - 1.140
R-factor	0.1379
Rwork	0.137
R-free	0.15610
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2dux
RMSD bond length	0.005
RMSD bond angle	1.211
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	PHASER
Refinement software	PHENIX ((phenix.refine: 1.8.4_1496))

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	1.160
High resolution limit [Å]	1.140	1.140
Number of reflections	109695
<I/σ(I)>	19.06	2.64
Completeness [%]	99.1	99
Redundancy	2.9	2.6

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	8	291	50 mM di-Ammoniumhydrogen citrate pH 5.0, PEG6000= 5 % (m/V), DTT= 5,15 g/L, NADP+= 0,66 g/L Human Aldose Reductase= 15 mg/ml. Afterwards the crystals have been transferred into Tris 100 mM 25% (m/V) PEG6000 pH 8.0 saturated with the inhibitor, VAPOR DIFFUSION, HANGING DROP, temperature 291K