1S1P

Crystal structures of prostaglandin D2 11-ketoreductase (AKR1C3) in complex with the non-steroidal anti-inflammatory drugs flufenamic acid and indomethacin

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID14-1
Synchrotron site	ESRF
Beamline	ID14-1
Temperature [K]	100
Detector technology	CCD
Collection date	2001-11-16
Detector	ADSC QUANTUM 4
Wavelength(s)	0.93
Spacegroup name	P 21 21 21
Unit cell lengths	55.681, 63.119, 96.113
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	38.000 - 1.200
R-factor	0.14679
Rwork	0.146
R-free	0.15600 *
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.006
RMSD bond angle	1.300 *
Data reduction software	MOSFLM
Data scaling software	CCP4 ((SCALA))
Phasing software	CNS
Refinement software	REFMAC (5.0)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	38.000 *	1.260
High resolution limit [Å]	1.200	1.200
Rmerge	0.059 *	0.242 *
Total number of observations	522433 *
Number of reflections	105032	13800 *
<I/σ(I)>	16.4	4.1
Completeness [%]	98.5	90.1
Redundancy	5	2.6

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7 *	291	PEG, pH 4.6, VAPOR DIFFUSION, HANGING DROP, temperature 291K

Crystallization Reagents in Literatures

ID	crystal ID	solution	reagent name	concentration (unit)	details
1	1	drop	protein	6 (mg/ml)
2	1	drop	potassium phosphate	10 (mM)	pH7.0
3	1	drop	dithiothreitol	1 (mM)
4	1	drop	EDTA	1 (mM)
5	1	drop	NADP+	2 (mM)
6	1	reservoir	PEG4000	25 (%(w/v))
7	1	reservoir	sodium citrate	100 (mM)	pH6.0
8	1	reservoir	MPD	2.5 (%(v/v))
9	1	reservoir	ammonium acetate	800 (mM)