4JIJ
Crystal structure of an inactive mutant of MMP-9 catalytic domain in complex with a fluorogenic synthetic peptidic substrate
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | SOLEIL BEAMLINE PROXIMA 1 |
Synchrotron site | SOLEIL |
Beamline | PROXIMA 1 |
Temperature [K] | 100 |
Detector technology | PIXEL |
Collection date | 2012-02-17 |
Detector | DECTRIS PILATUS 6M |
Wavelength(s) | 0.9184 |
Spacegroup name | P 21 21 21 |
Unit cell lengths | 34.200, 57.400, 172.030 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 40.568 - 1.698 |
R-factor | 0.1615 |
Rwork | 0.160 |
R-free | 0.19540 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | 4h3x |
RMSD bond length | 0.006 |
RMSD bond angle | 1.084 |
Data reduction software | XDS |
Data scaling software | XDS |
Phasing software | MOLREP |
Refinement software | PHENIX ((phenix.refine: 1.8_1069)) |
Data quality characteristics
Overall | Inner shell | Outer shell | |
Low resolution limit [Å] | 50.000 | 50.000 | 1.800 |
High resolution limit [Å] | 1.698 | 5.070 | 1.700 |
Rmerge | 0.174 | 0.073 | 1.052 |
Number of reflections | 38427 | ||
<I/σ(I)> | 9.91 | 26.6 | 2.06 |
Completeness [%] | 99.7 | 99.7 | 98.5 |
Redundancy | 8.97 | 7.83 | 8.92 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, SITTING DROP | 6 | 293 | Protein: 6 microL hMMP9(E402A) at 181 micro-M 0.12 M acetohydroxamic acid and 0.3 microL IT34-I at 6.9 mill-M. Reservoir: 10% PEG 20K, 0.1 M MMT (L-malic acid, MES, Tris) 75% acid/25% basic, 0.8 M NaCl, 0.02 SrCl2, 0.01% azide. Cryoprotectant: CryoProtX CM2, 0.8 M Li formate, 0.1 M (MMT 75% acid/25% basic), 9% PEG 10K, pH 6.0, VAPOR DIFFUSION, SITTING DROP, temperature 293K |