4P7E

Triazolopyridine compounds as selective JAK1 inhibitors: from hit identification to GLPG0634

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID23-1
Synchrotron site	ESRF
Beamline	ID23-1
Temperature [K]	100
Detector technology	CCD
Collection date	2010-07-17
Detector	MARRESEARCH
Wavelength(s)	0.976
Spacegroup name	P 41
Unit cell lengths	111.390, 111.390, 71.080
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	111.390 - 2.400
R-factor	0.20773
Rwork	0.205
R-free	0.26680
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2b7a
RMSD bond length	0.010
RMSD bond angle	1.327
Data reduction software	iMOSFLM (7.0.6)
Data scaling software	SCALA (3.3.16)
Phasing software	PHASER (2.1.4)
Refinement software	REFMAC (5.2.0019)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	30.000	3.000
High resolution limit [Å]	2.400	2.400
Rmerge		0.379
Number of reflections	34206
<I/σ(I)>	5.4	1.6
Completeness [%]	99.5
Redundancy	7.1	6.9

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	6	277	20% PEG 6000, 100 mM MES pH6, 0.2M LiCl