6UL8

RIP2 kinase catalytic domain complex with (5S,6S,8R)-2-(benzo[d]thiazol-5-yl)-6-hydroxy-4,5,6,7,8,9-hexahydro-5,8-methanopyrazolo[1,5-a][1,3]diazocine-3-carboxamide

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 21-ID-D
Synchrotron site	APS
Beamline	21-ID-D
Temperature [K]	93
Detector technology	CCD
Collection date	2015-11-11
Detector	MARMOSAIC 300 mm CCD
Wavelength(s)	0.9
Spacegroup name	P 32 2 1
Unit cell lengths	125.677, 125.677, 105.760
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	75.850 - 2.680
R-factor	0.1849
Rwork	0.183
R-free	0.22000
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	5ar2
RMSD bond length	0.011
RMSD bond angle	1.391
Data reduction software	HKL-2000
Data scaling software	Aimless (0.5.17)
Phasing software	MOLREP
Refinement software	REFMAC (5.8.0158)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	105.760	2.830
High resolution limit [Å]	2.680	2.680
Rmerge	0.111	0.654
Rmeas	0.120	0.705
Rpim	0.044	0.261
Total number of observations	196550
Number of reflections	27463	3944
<I/σ(I)>	12
Completeness [%]	100.0	100
Redundancy	7.2	7.2
CC(1/2)	0.997	0.852

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.5	295	85 mM Tris, pH 7.5, 200 mM calcium chloride, 10% PEG400, 5% glycerol, in 24 well Linbro trays at 22 degrees C. Crystals were frozen directly from the tray using paraffin oil as a cryoprotectant.