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 |