5P2R

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 144

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.3
Synchrotron site	BESSY
Beamline	14.3
Temperature [K]	100
Detector technology	CCD
Collection date	2014-06-04
Detector	MAR CCD 165 mm
Wavelength(s)	0.895
Spacegroup name	P 1 21 1
Unit cell lengths	45.283, 72.882, 52.719
Unit cell angles	90.00, 109.46, 90.00

Refinement procedure

Resolution	28.092 - 1.169
R-factor	0.1364
Rwork	0.136
R-free	0.15300
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.302
Data reduction software	XDS
Data scaling software	XDS
Phasing software	PHASER (2.5.7)
Refinement software	PHENIX

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	42.697		1.240
High resolution limit [Å]	1.170	3.500	1.170
Rmerge	0.065	0.022	0.612
Rmeas	0.075	0.025	0.708
Total number of observations	448345
Number of reflections	108623	4129	17382
<I/σ(I)>	14.41	52.33	2.37
Completeness [%]	99.7	99.1	99.1
Redundancy	4.127
CC(1/2)	0.999	0.999	0.764

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	4.6	290	0.1 M ammonium acetate, 0.1 M sodium acetate, 24-30% PEG 4000; crystal obtained by streak-seeding and soaked with 90 mM of fragment 144 with the SMILES code C[C@H](NC(=O)C1=CC(=CN1)C(C)=O)C1CC1