4PUW

Human Aldose Reductase complexed with a ligand with an IDD structure (2-[5-fluoro-2-(prop-2-ynylcarbamoyl)phenoxy]acetic acid) at 1.12 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	2013-07-18
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	49.411, 66.688, 47.353
Unit cell angles	90.00, 92.02, 90.00

Refinement procedure

Resolution	18.486 - 1.120
R-factor	0.138
Rwork	0.137
R-free	0.15680
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2dux
RMSD bond length	0.006
RMSD bond angle	1.264
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	1.140
High resolution limit [Å]	1.120	1.120
Number of reflections	117148
<I/σ(I)>	15.99	2.44
Completeness [%]	99.7	100
Redundancy	2.5	2.3

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	5	291	Crystallization solution: 50 mM di-Ammoniumhydrogen citrate pH 5.0 PEG6000= 5 % (m/V) DTT= 5.15 g/L NADP+= 0.66 g/L and Human Aldose Reductase= 15 mg/ml. 9 microliter of the crystallization solution were mixed with 3 microliter of a 5 mM solution of the inhibitor in 120 mM di-Ammoniumhydrogen citrate pH 5.0 with 25 % (m/V) PEG 6000 and 5 % DMSO, VAPOR DIFFUSION, HANGING DROP, temperature 291K