4XYC

NANOMOLAR INHIBITORS OF MYCOBACTERIUM TUBERCULOSIS GLUTAMINE SYNTHETASE 1: SYNTHESIS, BIOLOGICAL EVALUATION AND X-RAY CRYSTALLOGRAPHIC STUDIES

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID14-2
Synchrotron site	ESRF
Beamline	ID14-2
Temperature [K]	200
Detector technology	CCD
Collection date	2011-12-25
Detector	ADSC QUANTUM 4r
Wavelength(s)	0.933
Spacegroup name	P 21 21 21
Unit cell lengths	260.112, 273.497, 207.634
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	50.000 - 3.300
R-factor	0.203
Rwork	0.200
R-free	0.26500
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2wgs
RMSD bond length	0.010
RMSD bond angle	1.354
Data reduction software	MOSFLM
Data scaling software	SCALA
Phasing software	AMoRE
Refinement software	REFMAC (5.5.0109)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	3.500
High resolution limit [Å]	3.300	3.300
Rmerge	0.190	0.790
Number of reflections	221564
<I/σ(I)>	9.3	3
Completeness [%]	99.9	100
Redundancy	6.6	6.4

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.5	298	24% PEG3350, 0.2 M KSCN, PH 7.5, VAPOR DIFFUSION, HANGING DROP, TEMPERATURE 298K