1S2C

Crystal structures of prostaglandin D2 11-ketoreductase 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 ID14-2
Synchrotron site	ESRF
Beamline	ID14-2
Temperature [K]	100
Detector technology	CCD
Collection date	2002-02-09
Detector	ADSC QUANTUM 4
Wavelength(s)	0.93
Spacegroup name	P 21 21 21
Unit cell lengths	55.798, 63.000, 96.289
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.000 - 1.800
R-factor	0.16996
Rwork	0.168
R-free	0.20500 *
Structure solution method	isomorphous replacement
Starting model (for MR)	1s1p
RMSD bond length	0.007
RMSD bond angle	1.200 *
Data reduction software	MOSFLM
Data scaling software	CCP4 ((SCALA))
Phasing software	CNS
Refinement software	REFMAC (5.1.24)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	48.000 *	1.900
High resolution limit [Å]	1.800	1.800
Rmerge	0.078 *	0.256 *
Total number of observations	141396 *
Number of reflections	32084	4459 *
<I/σ(I)>	13.6	3.8
Completeness [%]	99.7	98.1
Redundancy	4.4	2.8

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)