4Y3U

The structure of phospholamban bound to the calcium pump SERCA1a

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 19-ID
Synchrotron site	APS
Beamline	19-ID
Temperature [K]	100
Detector technology	CCD
Collection date	2013-08-10
Detector	ADSC QUANTUM 315r
Wavelength(s)	0.987
Spacegroup name	P 21 21 21
Unit cell lengths	61.745, 91.825, 316.256
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.790 - 3.510
R-factor	0.23697
Rwork	0.235
R-free	0.27735
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	4kyt
RMSD bond length	0.005
RMSD bond angle	1.021
Data reduction software	HKL-3000
Data scaling software	HKL-3000
Phasing software	MOLREP
Refinement software	REFMAC (5.7.0032)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	3.560
High resolution limit [Å]	3.500	3.500
Rmerge	0.087	0.543
Number of reflections	23282
<I/σ(I)>	16.46	2.47
Completeness [%]	99.0	100
Redundancy	4.7	4.2

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7	277	1 UL OF SERCA1A AT 15 MG/ML IN 2% N- NONYL-BETA-D-MALTOPYRANOSIDE (NONYL MALTOSIDE) (ANATRACE), 20% GLYCEROL, 100 MM MOPS (PH 7.0), 0.12 M SUCROSE, 80 MM KCL, 3 MM MGCL2, AND 2.8 MM EGTA WAS MIXED WITH 1 UL OF PHOSPHOLAMBAN AT 2.1 MG/ML IN 20 MM MOPS (PH 7.2), 20% GLYCEROL, AND 0.1 % DECYLMALTOSIDE OR 0.01% DODECYL MALTOSIDE. THIS PROTEIN MIXTURE WAS THEN ADDED TO AN EQUAL VOLUME OF CRYSTALLIZATION LIQUOR; 15 % GLYCEROL, 17% (W/V) PEG-2000, 200MM NAOAC, AND 5 MM BETA-MERCOPTOETHANOL)