4PM1

Human transthyretin (TTR) complexed with 16-alpha-bromo-estradiol

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID23-1
Synchrotron site	ESRF
Beamline	ID23-1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2014-01-30
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.87
Spacegroup name	P 21 21 2
Unit cell lengths	43.202, 86.134, 63.395
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	43.067 - 1.230
R-factor	0.1784
Rwork	0.177
R-free	0.21060
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3gs4
RMSD bond length	0.007
RMSD bond angle	1.304
Data scaling software	XDS
Refinement software	PHENIX ((phenix.refine: 1.8.4_1496))

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	43.067	1.270
High resolution limit [Å]	1.230	1.230
Rmerge	0.118	1.220
Number of reflections	68116
<I/σ(I)>	11.73	1.88
Completeness [%]	98.0	96.4
Redundancy	9.32	9.58

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	6.2	293	Protein: 5 mg/ml TTR dialysed against 0.1 M NaCl, 0.05M Na acetate, pH 5.5. Precipitant:: 70% (30% PEG 4000, 0.2M imidazole malate, pH 6.0) 30% (18% monomethyl PEG 2000, 0.1 M sodium cacodylate, pH 6.5). Cryoprotectant: 40% (25 % diethylene glycol + 12.5 % MPD + 37.5 % 2,3-butanediol + 12.5 % 1,4-dioxane) 50% (12.5% MPEG 5K, 25% MPEG 550) 0.1 M (mixed Na propionate, Na cacodylate, Bis-Tris-propane 50% at pH 4.0 and 50% pH 9.5)