4X6H

Development of N-(Functionalized benzoyl)-homocycloleucyl-glycinonitriles as Potent Cathepsin K Inhibitors.

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	2014-03-24
Detector	PSI PILATUS 6M
Wavelength(s)	1.000008
Spacegroup name	P 21 21 21
Unit cell lengths	36.439, 54.551, 88.015
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	33.668 - 1.000
R-factor	0.1553
Rwork	0.155
R-free	0.16550
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1atk
RMSD bond length	0.022
RMSD bond angle	2.299
Data reduction software	PROTEUM PLUS (2011.4-1)
Data scaling software	SCALEPACK
Phasing software	PHASER (2.5.6)
Refinement software	PHENIX

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]			1.060
High resolution limit [Å]	1.000	2.990	1.000
Rmerge	0.052	0.031	0.522
Rmeas	0.057	0.034	0.593
Total number of observations	540950
Number of reflections	92375	3810	12248
<I/σ(I)>	15.89	47.98	2.22
Completeness [%]	96.8	99.3	80.4
Redundancy	5.9

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	5	295	0.1 M Tri-Sodium Citrate, 2.4 M Ammonium Sulfate