3N7S

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 5.0.2
Synchrotron site	ALS
Beamline	5.0.2
Temperature [K]	100
Detector technology	CCD
Collection date	2008-01-22
Detector	ADSC QUANTUM 315
Wavelength(s)	1.0
Spacegroup name	C 2 2 21
Unit cell lengths	73.305, 119.131, 137.158
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.170 - 2.100
R-factor	0.209
Rwork	0.208
R-free	0.22600
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.008
RMSD bond angle	1.020
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]	100.000	100.000	2.180
High resolution limit [Å]	2.100	4.520	2.100
Rmerge	0.073	0.029	0.424
Number of reflections	30529
<I/σ(I)>	12.4
Completeness [%]	86.9	99.3	51.5
Redundancy	4.6	4.8	3.1

Crystallization Conditions

crystal ID	method	pH	temperature	details
1		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, 0.4 M potassium thiocyanate. The crystals were transferred to 2.1M NaMalonate (pH 7.0) prior to freezing in liquid nitrogen, hanging drop, temperature 298K