5DSG

Structure of the M4 muscarinic acetylcholine receptor (M4-mT4L) bound to tiotropium

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]	293
Detector technology	CCD
Collection date	2013-12-11
Detector	MARMOSAIC 300 mm CCD
Wavelength(s)	1.033
Spacegroup name	P 1 21 1
Unit cell lengths	48.490, 172.040, 60.660
Unit cell angles	90.00, 94.37, 90.00

Refinement procedure

Resolution	28.530 - 2.600
R-factor	0.2275
Rwork	0.227
R-free	0.24030
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.002
RMSD bond angle	0.613
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	PHENIX

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	28.990		2.670
High resolution limit [Å]	2.600	11.630	2.600
Rmerge	0.213	0.107	0.932
Rmeas	0.221	0.110	1.053
Total number of observations	397753
Number of reflections	30337	335	2200
<I/σ(I)>	8.18	19.48	1.39
Completeness [%]	99.7	92.5	97.4
Redundancy	13.1		4.9

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	LIPIDIC CUBIC PHASE		293	Reconstituted in 10:1 monoolein:cholesterol mix. Precipitant solution: 20 - 40% PEG300, 100 mM MES, pH 5.5 - 7.5, and 10 - 150 mM EDTA, pH 8.0