4QGF
S.aureus TMK in complex with the potent inhibitor compound 38, 2-(3-CHLOROPHENOXY)-3-METHOXY-4-{(1R)-1-[(3S)-3-(5-METHYL-2,4-DIOXO-3,4-DIHYDROPYRIMIDIN-1(2H)-YL)PIPERIDIN-1-YL]PROPYL}BENZOIC ACID
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | ROTATING ANODE |
Source details | RIGAKU FR-E+ SUPERBRIGHT |
Temperature [K] | 140 |
Detector technology | CCD |
Collection date | 2010-08-17 |
Detector | RIGAKU SATURN 944+ |
Wavelength(s) | 1.54 |
Spacegroup name | P 1 21 1 |
Unit cell lengths | 46.188, 90.557, 48.448 |
Unit cell angles | 90.00, 101.92, 90.00 |
Refinement procedure
Resolution | 32.940 - 1.830 |
R-factor | 0.169 |
Rwork | 0.167 |
R-free | 0.20320 |
Structure solution method | MOLECULAR REPLACEMENT |
RMSD bond length | 0.010 |
RMSD bond angle | 1.020 |
Data reduction software | PROCESS |
Data scaling software | SCALA (3.3.15) |
Phasing software | AMoRE |
Refinement software | BUSTER-TNT (BUSTER 2.11.5) |
Data quality characteristics
Overall | Inner shell | Outer shell | |
Low resolution limit [Å] | 90.557 | 90.557 | 1.930 |
High resolution limit [Å] | 1.827 | 5.780 | 1.830 |
Rmerge | 0.026 | 0.481 | |
Total number of observations | 3852 | 7273 | |
Number of reflections | 32586 | ||
<I/σ(I)> | 14.3 | 16.7 | 1.5 |
Completeness [%] | 94.3 | 96.7 | 72 |
Redundancy | 3.3 | 3.5 | 2 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, SITTING DROP | 293 | To obtain the inhibitor bound crystal form of TMK-S.aureus crystals were initially grown in the absence of compound using the sitting drop method at 293 K with a reservoir solution of 100 mM PCPT (propionate-cacodylate-bistris propane buffer) pH 7-8, 21-24% PEG 3350, 200 mM Mg2Cl using 1:1 protein:reservoir solution with the protein solution at 13 mg/mL. Crystals were harvested and soaked overnight in a solution containing 100 mM PCPT, 35% PEG 3350, 200 mM Mg2Cl and 1-2 mM or compound from a 100 mM DMSO stock. After soaking the crystals were cryoprotected by soaking for 15 minutes in compound-soak solution supplemented with 20% ethylene glycol., VAPOR DIFFUSION, SITTING DROP |