3NAL

SR Ca(2+)-ATPase in the HnE2 state complexed with the Thapsigargin derivative DTB

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID23-1
Synchrotron site	ESRF
Beamline	ID23-1
Temperature [K]	100
Detector technology	CCD
Collection date	2006-09-18
Detector	ADSC QUANTUM 315r
Wavelength(s)	1.0661
Spacegroup name	P 41 21 2
Unit cell lengths	71.330, 71.330, 591.020
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	50.000 - 2.650
Rwork	0.255
R-free	0.28300
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2c8k
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	CNS
Refinement software	CNS

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	2.750
High resolution limit [Å]	2.650	2.650
Rmerge	0.110	0.843
Number of reflections	45158	4114
<I/σ(I)>	12.78	2.5
Completeness [%]	97.4	86.9
Redundancy	9.3	8.2

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	6.8	298	14% w/v PEG 2000 MME, 10% v/v glycerol, 100-200mM MgSO4, 4% tert-butanol, pH 6.8, VAPOR DIFFUSION, HANGING DROP, temperature 298K