4TQI

Human transthyretin (TTR) complexed with 3-(9H-fluoren-9-ylideneaminooxy)propanoic acid in a dual binding mode

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SOLEIL BEAMLINE PROXIMA 2
Synchrotron site	SOLEIL
Beamline	PROXIMA 2
Temperature [K]	100
Detector technology	CCD
Collection date	2013-11-20
Detector	ADSC QUANTUM 315r
Wavelength(s)	0.9801
Spacegroup name	P 21 21 2
Unit cell lengths	43.250, 86.370, 63.340
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	35.720 - 1.250
R-factor	0.174
Rwork	0.173
R-free	0.20800
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3gs0
RMSD bond length	0.006
RMSD bond angle	1.060
Data scaling software	XDS
Refinement software	PHENIX ((PHENIX.REFINE: 1.8.4_1496))

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	43.200	1.320
High resolution limit [Å]	1.250	1.250
Rmerge	0.151
Number of reflections	63728
<I/σ(I)>	11.11	1.64
Completeness [%]	95.7	91.5
Redundancy	8.04	7.2

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	5.7	293	protein: TTR 10 mg/ml + ligand 0.66 milli-M in 0.1 M NaCl, 0.05 M Na acetate, pH 5.5. Precipitant: 70% (30% PEG-4K, 0.2 M imidazole malate, pH 6.0) and 30% (12% MPEG-5K, 0.1 M sodium acetate, pH 5.5). Cryoprotectant: 40% (25 % diethylene glycol, 12.5 % MPD, 37.5 % 2,3-butanediol, 12.5 % 1,4-dioxane), 10% PEG 10K, 0.1 M (mixed sodium propionate, sodium cacodylate, Bis-Tris-propane) (65% component A pH 4; 35% B pH 9.5)