4Z84

PKAB3 in complex with pyrrolidine inhibitor 34a

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.1
Synchrotron site	BESSY
Beamline	14.1
Temperature [K]	100
Detector technology	CCD
Collection date	2012-11-24
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 21 21 21
Unit cell lengths	61.852, 78.431, 79.506
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	19.608 - 1.554
R-factor	0.209273093362
Rwork	0.208
R-free	0.23430
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1q61
RMSD bond length	0.010
RMSD bond angle	1.101
Data reduction software	XDS (January 10, 2014)
Data scaling software	XDS (January 10, 2014)
Phasing software	PHASER (2.5.5)
Refinement software	PHENIX (1.9_1692)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	19.608	1.593
High resolution limit [Å]	1.554	1.554
Rmerge	0.127
Number of reflections	51501
<I/σ(I)>	5.94
Completeness [%]	91.5	0.49
Redundancy	3.4

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7	277	The droplets, containing 16 mg/ml protein 25 mM Bis-Tris-HCl, pH 7.0, 150 mM KCl, 1.5mM octanoyl-N-methylglucamide, 0.8 mM PKI peptide and 1mM of the pyrrolidine inhibitor 34a, were equilibrated against 12-26 % (v/v) methanol.