6UPE

Structure of trehalose-6-phosphate phosphatase from Salmonella typhimurium inhibited by 4-n-octylphenyl alpha-D-glucopyranoside-6-sulfate

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SSRL BEAMLINE BL14-1
Synchrotron site	SSRL
Beamline	BL14-1
Temperature [K]	290
Detector technology	CCD
Collection date	2016-05-23
Detector	MARMOSAIC 325 mm CCD
Wavelength(s)	1.378
Spacegroup name	P 1 21 1
Unit cell lengths	46.159, 52.419, 108.615
Unit cell angles	90.00, 100.58, 90.00

Refinement procedure

Resolution	37.402 - 2.244
R-factor	0.19
Rwork	0.186
R-free	0.23200
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	6upb
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	PHASER (2.6.0)
Refinement software	PHENIX (1.13_2998)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	2.280
High resolution limit [Å]	2.240	6.080	2.240
Rmerge	0.107	0.087	0.422
Rmeas	0.123	0.100	0.505
Rpim	0.060	0.048	0.273
Number of reflections	24547	1303	1124
<I/σ(I)>	9.3
Completeness [%]	99.3	99.6	90.6
Redundancy	4	4	3.1
CC(1/2)	0.978	0.987	0.840

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP		290	Drop contained: 1.5 uL 40 mg/mL protein, 2 uL reservoir solution (15% PEG 3350, 400 mM lithium citrate, 30 mM magnesium chloride, 40 mM mixture of MES, MOPS, and TAPS at pH 7.5), and 0.5 uL 1:10^3 dilution of seed stock prepared according to Seed Bead protocol. Crystals were transferred to drop containing 18% PEG 3350, 400mM lithium citrate, 40 mM magnesium chloride, 10% ethylene glycol, and 1mM OGS for 24 prior to cryocooling