6V9S

Structure-based development of subtype-selective orexin 1 receptor antagonists

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 23-ID-D
Synchrotron site	APS
Beamline	23-ID-D
Temperature [K]	100
Detector technology	PIXEL
Collection date	2018-11-29
Detector	DECTRIS PILATUS 6M
Wavelength(s)	1.033
Spacegroup name	P 21 21 21
Unit cell lengths	64.661, 66.341, 182.461
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	44.880 - 3.500
R-factor	0.2415
Rwork	0.239
R-free	0.27320
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4zj8 4zjc
Data reduction software	SCALEPACK
Data scaling software	SCALEPACK
Phasing software	PHASER
Refinement software	PHENIX (1.17.1_3660)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	3.560
High resolution limit [Å]	3.500	9.480	3.500
Rmerge	0.197	0.034	1.235
Rmeas	0.237	0.041	1.498
Rpim	0.129	0.022	0.827
Total number of observations	24855
Number of reflections	9356	470	490
<I/σ(I)>	4
Completeness [%]	89.2	77.8	94.4
Redundancy	2.7	2.6	2.6
CC(1/2)		0.995	0.286

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	LIPIDIC CUBIC PHASE		293	100mM Sodium Citrate pH 5.3, 31% PEG 400, 200 mM Ammonium Formate