4NY6

Neutron structure of leucine and valine methyl protonated type III antifreeze

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
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.6525
Spacegroup name	P 21 21 21
Unit cell lengths	32.730, 39.120, 46.540
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	26.772 - 1.850
R-factor	0.1782
Rwork	0.176
R-free	0.22450
RMSD bond length	0.013
RMSD bond angle	1.302
Data reduction software	LAUEGEN
Data scaling software	LSCALE
Phasing software	PHENIX
Refinement software	PHENIX ((phenix.refine: 1.8_1069))

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	1.900	1.090
High resolution limit [Å]	1.050	1.800	1.050
Rmerge	0.048	0.169	0.638
Number of reflections	28534
<I/σ(I)>	32.5	6.6	2.66
Completeness [%]	99.7	71.4	99.9
Redundancy	6.1	3.5

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	5.2	285	10mg/ml protein in 50 mM sodium acetate pD 5.2. Drops containing 20 ml protein solution and 30 ml precipitant buffer (2.1 M ammonium sulfate, 9% d8-glycerol) were equilibrated against 1 ml precipitant buffer in the reservoir, VAPOR DIFFUSION, SITTING DROP, temperature 285K
1	VAPOR DIFFUSION, SITTING DROP	5.2	285	10mg/ml protein in 50 mM sodium acetate pD 5.2. Drops containing 20 ml protein solution and 30 ml precipitant buffer (2.1 M ammonium sulfate, 9% d8-glycerol) were equilibrated against 1 ml precipitant buffer in the reservoir, VAPOR DIFFUSION, SITTING DROP, temperature 285K