5P2T

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 146

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, 73.414, 52.757
Unit cell angles	90.00, 109.38, 90.00

Refinement procedure

Resolution	28.128 - 1.098
R-factor	0.1298
Rwork	0.129
R-free	0.14510
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.208
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]	42.717		1.160
High resolution limit [Å]	1.100	3.290	1.100
Rmerge	0.060	0.028	0.567
Rmeas	0.069	0.033	0.658
Total number of observations	538712
Number of reflections	131581	4960	20897
<I/σ(I)>	13.15	40.76	2.4
Completeness [%]	99.4	98.2	97.9
Redundancy	4.094
CC(1/2)	0.999	0.998	0.769

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 146 with the SMILES code CC(C)SC1=NN\C(O1)=C1/C=CC=N1