4YDM

High resolution crystal structure of human transthyretin bound to ligand and conjugates of 3-(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	2014-01-08
Detector	PSI PILATUS 6M
Wavelength(s)	0.97945
Spacegroup name	P 21 21 2
Unit cell lengths	42.709, 85.420, 63.537
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	63.540 - 1.250
R-factor	0.1471
Rwork	0.146
R-free	0.17232
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2qgb
RMSD bond length	0.015
RMSD bond angle	1.738
Data scaling software	SCALA (3.3.15)
Refinement software	REFMAC (5.8.0049)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	38.200	38.200	1.320
High resolution limit [Å]	1.250	3.950	1.250
Rmerge		0.016	0.498
Rmeas	0.032
Rpim	0.013	0.007	0.215
Total number of observations	403587	13158	55367
Number of reflections	64492
<I/σ(I)>	25.5	74.9	3.4
Completeness [%]	99.1	99.7	95.8
Redundancy	6.3	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 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