7QBM

Structure of the activation intermediate of cathepsin K in complex with the 3-cyano-3-aza-beta-amino acid inhibitor Gu2602

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	PIXEL
Collection date	2018-05-03
Detector	DECTRIS PILATUS3 6M
Wavelength(s)	0.9184
Spacegroup name	P 43 21 2
Unit cell lengths	103.283, 103.283, 55.464
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.910 - 1.880
R-factor	0.1926
Rwork	0.190
R-free	0.23400
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	7nxm
RMSD bond length	0.009
RMSD bond angle	1.426
Data reduction software	XDS
Data scaling software	XDS
Phasing software	BUCCANEER
Refinement software	REFMAC (5.8.0267)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	48.910	48.910	1.900
High resolution limit [Å]	1.790	5.330	1.790
Rmerge	0.128	0.118	1.650
Rmeas	0.135	0.124	1.916
Total number of observations	260542
Number of reflections	27424	1231	3559
<I/σ(I)>	10.69	21.51	1.01
Completeness [%]	94.5	99.7	77.3
Redundancy	9.501	11.18	3.696
CC(1/2)	0.993	0.989	0.517

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP		290	10% PEG 8000, 20% ethylene glycol, 0.02 M sodium formate, 0.02 M ammonium acetate, 0.02 M trisodium citrate, 0.02 M sodium potassium L-tartrate, 0.02 M sodium oxamate, 0.1 M MES/imidazole pH 6.5