3N7R

Crystal structure of the ectodomain complex of the CGRP receptor, a Class-B GPCR, reveals the site of drug antagonism

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ALS BEAMLINE 5.0.3
Synchrotron site	ALS
Beamline	5.0.3
Temperature [K]	100
Detector technology	CCD
Collection date	2007-08-18
Detector	ADSC QUANTUM 315
Wavelength(s)	1.0
Spacegroup name	C 2 2 21
Unit cell lengths	77.940, 118.200, 133.260
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.550 - 2.900
R-factor	0.2337
Rwork	0.232
R-free	0.26690
RMSD bond length	0.008
RMSD bond angle	1.030
Data reduction software	DENZO
Data scaling software	SCALEPACK
Refinement software	BUSTER-TNT (BUSTER 2.9.2)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	3.000
High resolution limit [Å]	2.900	6.240	2.900
Rmerge	0.066	0.039	0.438
Number of reflections	10420
<I/σ(I)>	14.8
Completeness [%]	73.6	97.4	12.1
Redundancy	4.1	4.2	1.3

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	6.5	298	CLR/RAMP1 complex was mixed with Olcegepant prior to crystallization in a 1:4 (protein : compound) molar ratio. Crystals were obtained by mixing 0.6uL protein with 0.3uL reservoir solution containing 1-1.3M ammonium sulfate, 6-8% dioxane, 60-80mM MES pH 6.5, plus 0.4 M potassium thiocyanate. Telcagepant was soaked into the ligand binding site. The crystal was transferred to 2.1M NaMalonate (pH 7.0) prior to freezing in liquid nitrogen., VAPOR DIFFUSION, HANGING DROP, temperature 298K