2X8I

Discovery of a Novel Class of triazolones as Checkpoint Kinase Inhibitors - Hit to Lead Exploration

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	EMBL/DESY, HAMBURG BEAMLINE X13
Synchrotron site	EMBL/DESY, HAMBURG
Beamline	X13
Temperature [K]	100
Detector technology	CCD
Collection date	2002-08-20
Detector	MARRESEARCH
Spacegroup name	P 21 21 21
Unit cell lengths	41.255, 70.900, 104.241
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	31.160 - 1.920
R-factor	0.1894
Rwork	0.188
R-free	0.22368
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2x8d
RMSD bond length	0.007
RMSD bond angle	1.269
Data reduction software	MOSFLM
Data scaling software	SCALA
Phasing software	AMoRE
Refinement software	REFMAC (5.5.0102)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	31.160	2.020
High resolution limit [Å]	1.920	1.920
Rmerge	0.080	0.290
Number of reflections	22530
<I/σ(I)>	14	5.6
Completeness [%]	94.3	89.4
Redundancy	5.8	5.4

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	6.5		HANGING DROP 3 UL PLUS 3UL PROTEIN: 7MG/ML, 2MM COMPOUND, 25MM TRIS PH7.5, 500MM NACL, 5% GLYCEROL. 5MM DTT WELL: 16-22% (W/V) PEG3350, 150MM AMMONIUM SULPHATE AND 100 MM BES PH 6.5