6NXB

ECAII IN COMPLEX WITH CITRATE AT PH 7

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU MICROMAX-007 HF
Temperature [K]	100
Detector technology	PIXEL
Collection date	2018-03-22
Detector	DECTRIS EIGER R 4M
Wavelength(s)	1.5418
Spacegroup name	C 1 2 1
Unit cell lengths	151.354, 62.354, 142.666
Unit cell angles	90.00, 118.04, 90.00

Refinement procedure

Resolution	22.850 - 1.750
R-factor	0.1418
Rwork	0.141
R-free	0.19170
Structure solution method	FOURIER SYNTHESIS
RMSD bond length	0.020
RMSD bond angle	2.205
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	REFMAC
Refinement software	REFMAC (5.8.0238)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	40.000	40.000	1.780
High resolution limit [Å]	1.750	4.750	1.750
Rmerge	0.039	0.020	0.405
Rmeas	0.048	0.024	0.502
Rpim	0.026	0.013	0.292
Total number of observations	336615
Number of reflections	116189	6033	5722
<I/σ(I)>	12.6
Completeness [%]	98.1	98.5	96.1
Redundancy	2.9	3.3	2.4
CC(1/2)		0.996	0.769

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7	293	Protein, at the concentration 15 mg/ml in 50 mM HEPES buffer pH 7 and 150 mM sodium chloride was mixed with equivolume solution of precipitant that contained, 17% (w/v) PEG3350 and 0.17 M ammonium citrate pH 7. Resulting droplets were equilibrated against the precipitant. For the data collection, crystal was briefly transferred to cryo-protecting solution, which had the same composition as precipitant, except concentration of PEG3350 was increased to 35 % (v/w/) and 10% (v/v), and also contained 15% of glycerol