5M4V

X-ray structure of the mambaquaretin-1, a selective antagonist of the vasopressin type 2 receptor

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID29
Synchrotron site	ESRF
Beamline	ID29
Temperature [K]	100
Detector technology	PIXEL
Collection date	2012-11-11
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.976251
Spacegroup name	P 4 21 2
Unit cell lengths	63.840, 63.840, 32.960
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.140 - 1.060
R-factor	0.13195
Rwork	0.131
R-free	0.15574
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1b0c
RMSD bond length	0.029
RMSD bond angle	2.709
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0155)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	45.140	1.090
High resolution limit [Å]	1.060	1.060
Rmerge	0.080	2.840
Number of reflections	31490
<I/σ(I)>	19.36	1.22
Completeness [%]	99.9	99.3
Redundancy	23.75	19.16
CC(1/2)	1.000	0.618

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.5	293	Protein: 7 mg/mL in 50mM sodium Acetate pH 5.5 Precipitant: 36% MPEG 2K, 0.45 M NaCl, 0.9 M KSCN, 0.1 M imidazole HCl, pH 7.5. Cryoprotectant: 5 % diethylene glycol, 5 % ethylene glycol, 5 % MPD, 5 % glycerol, 5 % 1,2-propanediol, 5 % DMSO, 18% MPEG-2K, 100 mM linear mixed buffer 1: sodium acetate, ADA, and bicine, 20% at pH 4 and 80% at pH 10.