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