3N4C

6-Phenyl-1H-imidazo[4,5-c]pyridine-4-carbonitrile as cathepsin S inhibitors

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU MICROMAX-007 HF
Detector technology	CCD
Collection date	2006-12-11
Detector	R-Axis IV
Wavelength(s)	1.5418
Spacegroup name	P 41 2 2
Unit cell lengths	85.629, 85.629, 150.573
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	56.540 - 1.900
R-factor	0.25091
Rwork	0.249
R-free	0.28611
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1ms6
Data reduction software	d*TREK
Data scaling software	d*TREK
Phasing software	MOLREP
Refinement software	REFMAC

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	56.540	56.540	1.970
High resolution limit [Å]	1.900	4.090	1.900
Rmerge	0.118	0.045	0.482
Number of reflections	39256
<I/σ(I)>	8	23.5	3.3
Completeness [%]	87.4	99	90.9
Redundancy	6.82	6.38	7.74

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	Hanging drop	5		Composition of crystallisation solution (including components from protein prep): 50 mM NaAcetate; 0.25 M NaCl; coconcentrated with inhibitor; 4% DMSO; 26% PEG 4K; 0.1 M NaCitrate pH=5.0; 0,2 M (NH4)2SO4. Cryoprotectant composition: 26% PEG 4K, 0.1 M NaCitrate pH=5.0; o0.2 M (NH4)2SO4; 15% PEG 400 (compound), Hanging drop, temperature room temperatureK