4TQ8

Dual binding mode for 3-(9H-fluoren-9-ylideneaminooxy)propanoic acid binding to Human transthyretin (TTR)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID23-2
Synchrotron site	ESRF
Beamline	ID23-2
Temperature [K]	100
Detector technology	PIXEL
Collection date	2014-02-26
Detector	DECTRIS PILATUS 2M-F
Wavelength(s)	0.8729
Spacegroup name	P 21 21 2
Unit cell lengths	43.140, 86.040, 63.480
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	38.560 - 1.520
R-factor	0.18728
Rwork	0.186
R-free	0.20980
Structure solution method	FOURIER SYNTHESIS
RMSD bond length	0.022
RMSD bond angle	2.112
Data scaling software	XDS
Phasing software	MOLREP
Refinement software	REFMAC (5.7.0029)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	43.100	1.610
High resolution limit [Å]	1.520	1.520
Rmerge	0.145
Number of reflections	37078
<I/σ(I)>	11.9	1.01
Completeness [%]	99.8	98.8
Redundancy	8.73	7.3

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	5.7	293	Protein: 5 mg/ml 1 milli-M ligand Precipitant: 60% (30% PEG-4K, 0.2 M imidazole malate, pH 6.0) 40% (24% MPEG-5K, 0.1 M sodium acetate, pH 5.5) Drops: 1 micro-L protein-ligand complex 1 micro-L precipitant. Cryoprotectant:: 40% (12.5 % diethylene glycol + 12.5 % ethylene glycol + 12.5 % glycerol + 12.5 % 1,2-propanediol + 12.5 % DMSO + 12.5 % 1,4-dioxane), 25% MPEG 5K, 0.1 M sodium propionate, sodium cacodylate, Bis-Tris-propane(65% component A pH 4; 35% B pH 9.5 and 1 milli-M ligand.