5JIM

Crystal Structure of Human Transthyretin in Complex with Perfluoroktansulfonsyra (PFOS)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID29
Synchrotron site	ESRF
Beamline	ID29
Temperature [K]	100
Detector technology	PIXEL
Collection date	2015-02-24
Detector	DECTRIS PILATUS3 6M
Wavelength(s)	0.913
Spacegroup name	P 21 21 2
Unit cell lengths	43.146, 85.413, 64.121
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	38.511 - 1.260
R-factor	0.1357
Rwork	0.135
R-free	0.15830
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1f41
RMSD bond length	0.009
RMSD bond angle	1.332
Data reduction software	XDS
Data scaling software	Aimless
Phasing software	PHASER
Refinement software	PHENIX (1.9_1692)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	40.000	1.300
High resolution limit [Å]	1.260	1.260
Rmerge	0.036	0.565
Number of reflections	64626
<I/σ(I)>	23.41	2.97
Completeness [%]	99.8	98.83
Redundancy	7.1	6.5

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.6	291	Purified TTRwt was dialyzed against 10 mM sodiumphosphate buffer with 100 mM KCl pH 7.6 and concentrated to 5 mg per ml. PFOS was added at 5 x molar excess to the protein. The reservoir contained 1.3 to 1.6 M sodium citrate and 3.5 percent glycerol at pH 5.5. Drop size 3 plus 3 microliter.