4Z0L

The murine cyclooxygenase-2 complexed with a nido-dicarbaborate-containing indomethacin derivative

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 24-ID-C
Synchrotron site	APS
Beamline	24-ID-C
Temperature [K]	100
Detector technology	PIXEL
Collection date	2014-02-05
Detector	PSI PILATUS 6M
Wavelength(s)	0.97918
Spacegroup name	P 21 21 2
Unit cell lengths	180.944, 135.011, 124.195
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	49.600 - 2.290
R-factor	0.212
Rwork	0.210
R-free	0.25000
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3nt1
RMSD bond length	0.008
RMSD bond angle	0.946
Data reduction software	XDS
Data scaling software	XDS
Phasing software	PHASER
Refinement software	PHENIX (1.9_1692)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	2.370
High resolution limit [Å]	2.290	2.290
Rmerge	0.061	0.195
Number of reflections	135815
<I/σ(I)>	17.7	5.7
Completeness [%]	98.7	91
Redundancy	4.3	4.8

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	8	291	mCOX-2 protein reconstituted with a 2-fold molar excess of heme in phosphtate buffer, pH 6.7, 100 mM NaCl, 1.2% (w/v) -OG, and 0.1% NaN3, and 10-fold molar excess of inhibitors from 25 mM DMSO stocks were added to protein samples. Mixing 3 uL of the protein-inhibitor complex with 3 uL crystallization solution containing 50 mM EPPS, pH 8.0, 120 mM MgCl2, 22-26% PEG MME-550 against reservoir solutions comprised of 50 mM EPPS pH 8.0, 120 mM MgCl2, 22-26% PEG MME-550