4YDN

High resolution crystal structure of human transthyretin bound to ligand and conjugates of 4-(5-(3,5-dichloro-4-hydroxyphenyl)-1,3,4-oxadiazol-2-yl)phenyl fluorosulfate

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SSRL BEAMLINE BL11-1
Synchrotron site	SSRL
Beamline	BL11-1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2013-11-22
Detector	PSI PILATUS 6M
Wavelength(s)	0.97945
Spacegroup name	P 21 21 2
Unit cell lengths	43.093, 85.522, 64.650
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	38.484 - 1.350
R-factor	0.1591
Rwork	0.157
R-free	0.19510
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2qgb
RMSD bond length	0.015
RMSD bond angle	1.694
Data reduction software	XDS
Data scaling software	SCALA (3.3.21)
Refinement software	REFMAC (5.8.0049)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	38.484	38.484	1.420
High resolution limit [Å]	1.349	4.270	1.350
Rmerge		0.017	0.449
Rmeas	0.031
Rpim	0.012	0.008	0.194
Total number of observations	338134	10787	46783
Number of reflections	53165
<I/σ(I)>	28.4	73.7	4.8
Completeness [%]	99.5	99.5	98
Redundancy	6.4	5.8	6.2

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