3N3G

4-(3-Trifluoromethylphenyl)-pyrimidine-2-carbonitrile as cathepsin S inhibitors: N3, not N1 is critically important

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU MICROMAX-007 HF
Detector technology	IMAGE PLATE
Collection date	2007-07-12
Detector	RIGAKU RAXIS IV
Wavelength(s)	1.5418
Spacegroup name	P 41 2 2
Unit cell lengths	85.757, 85.757, 150.902
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	74.560 - 1.600
R-factor	0.225
Rwork	0.223
R-free	0.26400
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.009
RMSD bond angle	1.145
Data reduction software	d*TREK
Data scaling software	d*TREK (9.5L)
Phasing software	MOLREP
Refinement software	REFMAC

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	85.750	1.660
High resolution limit [Å]	1.600	1.600
Rmerge	0.166	0.501
Total number of observations		2568
Number of reflections	65361
<I/σ(I)>	5.3	1.1
Completeness [%]	87.7	24.9
Redundancy	5.28	1.41

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	5	298	crystallisation solution: 50 mM NaAcetate, 0.25 M NaCl, 4 mM MMTS, 30% PEG 4K, 0.1 M NaCitrate, 0,2 M (NH4)2SO4, 10 mM DMSO, 10 mM DTT. Cryoprotectant composition: 30% PEG 4K, 0.1 M NaCitrate, 0.2 M (NH4)2SO4, 15% PEG 400 (+ 10% compound). Ligand was introduced by soaking crystals prepared with another compound, pH 5.0, VAPOR DIFFUSION, HANGING DROP, temperature 298K