6RK9

Aspartyl/Asparaginyl beta-hydroxylase (AspH)oxygenase and TPR domains in complex with manganese, N-oxalylglycine and cyclic peptide substrate mimic of factor X

Replaces:  5JZZ

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU FR-E+ SUPERBRIGHT
Temperature [K]	100
Detector technology	CCD
Collection date	2014-04-04
Detector	RIGAKU SATURN 944+
Wavelength(s)	1.54
Spacegroup name	P 1
Unit cell lengths	49.472, 59.243, 95.665
Unit cell angles	103.97, 91.49, 92.70

Refinement procedure

Resolution	31.997 - 2.292
R-factor	0.2117
Rwork	0.211
R-free	0.23500
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	5jqy
Data reduction software	HKL-3000
Data scaling software	SCALEPACK
Phasing software	PHASER
Refinement software	PHENIX

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	2.380
High resolution limit [Å]	2.292	4.950	2.292
Rmerge	0.150	0.061	0.992
Rmeas	0.145	0.067
Rpim	0.069	0.028	0.466
Number of reflections	46948	4650	4743
<I/σ(I)>	6
Completeness [%]	99.9	99.6	100
Redundancy	5.6	5.8	5.5
CC(1/2)		0.997	0.671

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	6.5	277	100 mM Bis-tris propane, 200 mM potassium thiocyanate, 20% PEG 3350, 2 mM N-oxalylglycine, 1 mM manganese chloride, 3.3 mM cyclic peptide, 18 mg/ml asph protein