5P2S

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 145

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	45.271, 73.064, 52.920
Unit cell angles	90.00, 109.57, 90.00

Refinement procedure

Resolution	24.932 - 1.078
R-factor	0.1309
Rwork	0.130
R-free	0.14460
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.222
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]	42.656		1.140
High resolution limit [Å]	1.080	3.230	1.080
Rmerge	0.064	0.028	0.639
Rmeas	0.073	0.032	0.743
Total number of observations	564549
Number of reflections	138598	5233	22067
<I/σ(I)>	13.42	44.36	2.23
Completeness [%]	99.5	98.3	98.2
Redundancy	4.073
CC(1/2)	0.999	0.998	0.745

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 145 with the SMILES code NNC1=CC=CC=C1Br