4QGG

TMK in complex with compound 46, 2-(3-CHLOROPHENOXY)-3-FLUORO-4-{(1R)-3-METHYL-1-[(3S)-3-(5-METHYL-2,4-DIOXO-3,4-DIHYDROPYRIMIDIN-1(2H)-YL)PIPERIDIN-1-YL]BUTYL}BENZOIC ACID

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 17-ID
Synchrotron site	APS
Beamline	17-ID
Temperature [K]	140
Detector technology	PIXEL
Collection date	2010-08-16
Detector	DECTRIS PILATUS 6M
Wavelength(s)	1.0
Spacegroup name	P 1 21 1
Unit cell lengths	46.996, 91.042, 48.504
Unit cell angles	90.00, 100.63, 90.00

Refinement procedure

Resolution	47.670 - 1.620
R-factor	0.2087
Rwork	0.208
R-free	0.22220
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.010
RMSD bond angle	1.060
Data reduction software	PROCESS
Data scaling software	SCALA (3.3.16)
Phasing software	AMoRE
Refinement software	BUSTER-TNT (BUSTER 2.11.5)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	91.042	91.042	1.710
High resolution limit [Å]	1.621	5.130	1.620
Rmerge		0.020	0.483
Total number of observations		5270	24954
Number of reflections	49913
<I/σ(I)>	15.7	26.1	1.6
Completeness [%]	98.4	98.2	98.2
Redundancy	3.4	3.2	3.4

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