6RQ7

Gadolinium MRI contrast compound binding in human plasma glycoprotein afamin - resurrection of highly anisotropic data

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE MASSIF-1
Synchrotron site	ESRF
Beamline	MASSIF-1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2018-05-15
Detector	DECTRIS PILATUS3 2M
Wavelength(s)	0.96598
Spacegroup name	P 21 21 2
Unit cell lengths	103.352, 109.734, 48.381
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	75.240 - 2.690
R-factor	0.26629
Rwork	0.263
R-free	0.33544
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	5OKL_B
RMSD bond length	0.002
RMSD bond angle	1.191
Data reduction software	XDS
Data scaling software	pointless
Phasing software	PHASER
Refinement software	REFMAC (5.8.0238)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	75.240	3.020
High resolution limit [Å]	2.690	2.700
Rmerge	0.180	0.540
Rmeas	0.200	0.680
Number of reflections	9591	486
<I/σ(I)>	5.6	1.7
Completeness [%]	85.2	62
Redundancy	4.7	2.1
CC(1/2)	0.990	0.800

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	5.5	293	Stock: 5 mg/ml AFM in 20mM HEPES pH 7.5, 150mM NaCl, incubated with 10mM Gd-DO3A Drop: 200 nL AFM stock + 200 nL of precipitate in hanging drop vapor diffusion (EMBL HTX) Precipitant: 23 to 28% PEG4k, 0.2M NH4SO4, 0.1 M CH3COONH4, pH 5.5