4ZOT

Crystal structure of BbKI, a disulfide-free plasma kallikrein inhibitor at 1.4 A resolution

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 22-ID
Synchrotron site	APS
Beamline	22-ID
Temperature [K]	100
Detector technology	CCD
Collection date	2013-12-07
Detector	MARMOSAIC 300 mm CCD
Wavelength(s)	1.000
Spacegroup name	P 21 21 21
Unit cell lengths	46.736, 59.462, 64.011
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	43.570 - 1.400
R-factor	0.1247
Rwork	0.123
R-free	0.16650
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2go2
RMSD bond length	0.014
RMSD bond angle	1.779
Data reduction software	HKL-3000
Data scaling software	HKL-3000
Phasing software	PHASER
Refinement software	REFMAC (5.8.0107)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	1.420
High resolution limit [Å]	1.400	3.800	1.400
Rmerge	0.048	0.034	0.628
Rmeas	0.054	0.039	0.704
Rpim	0.024	0.017	0.311
Total number of observations	171809
Number of reflections	34445
<I/σ(I)>	10.2		1.9
Completeness [%]	96.1	93.9	93.3
Redundancy	5	4.8	4.8
CC(1/2)		0.997	0.752

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	4.6	293	rBbKI in 0.05 M Tris/HCl, pH 8.0, and 0.15 M NaCl was concentrated to 6.3 mg/ml and crystallized using the conditions 8% PEG 4000, 0.1 M sodium acetate, pH 4.6. Cryoprotectant solution - mother liquor with extra 25% glycerol.