4FI8

Kinetic Stabilization of transthyretin through covalent modification of K15 by 4-bromo-3-(5-(3,5-dichloro-4-hydroxyphenyl)-1,3,4-oxadiazol-2-yl)-benzenesulfonamide

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SSRL BEAMLINE BL12-2
Synchrotron site	SSRL
Beamline	BL12-2
Temperature [K]	100
Detector technology	PIXEL
Collection date	2011-06-24
Detector	PSI PILATUS 6M
Wavelength(s)	0.9795
Spacegroup name	P 21 21 2
Unit cell lengths	43.185, 86.143, 63.693
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	86.140 - 1.220
R-factor	0.1691
Rwork	0.168
R-free	0.19660
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2fbr
RMSD bond length	0.018
RMSD bond angle	1.771
Data reduction software	DENZO
Data scaling software	SCALEPACK
Refinement software	REFMAC

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	86.143	50.000	1.260
High resolution limit [Å]	1.220	2.630	1.220
Rmerge		0.074	0.647
Number of reflections	70853
<I/σ(I)>	10.7
Completeness [%]	99.2	98	99.6
Redundancy	5.7	5.4	4.8

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	5.5	298	The wt-TTR was concentrated to 4 mg/ml in 10 mM NaPi, 100 mM KCl, at pH 7.6 and co-crystallized at room temperature with inhibitors using the vapor-diffusion sitting drop method, crystals were grown from 1.395 M sodium citrate, 3.5% v/v glycerol at ph 5.5. The crystals were frozen using a cryo-protectant solution of 1.395 m sodium citrate, ph 5.5, containing 10% v/v glycerol, vapor diffusion, sitting drop, temperature 298.0, VAPOR DIFFUSION, SITTING DROP