5P2Q

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 143

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	2014-02-15
Detector	MAR CCD 165 mm
Wavelength(s)	0.8944
Spacegroup name	P 1 21 1
Unit cell lengths	45.230, 72.880, 52.720
Unit cell angles	90.00, 109.20, 90.00

Refinement procedure

Resolution	17.575 - 1.350
R-factor	0.1383
Rwork	0.137
R-free	0.16150
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.184
Data reduction software	iMOSFLM
Data scaling software	SCALA
Phasing software	PHASER (2.5.7)
Refinement software	PHENIX

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	17.640	17.575	1.420
High resolution limit [Å]	1.350	4.270	1.350
Rmerge	0.070	0.039	0.451
Rmeas	0.080	0.044	0.519
Rpim	0.039	0.022	0.255
Total number of observations	281359	9275	38302
Number of reflections	69212
<I/σ(I)>	11.1	28.2	2.9
Completeness [%]	97.7	98	95
Redundancy	4.1	4.1	3.9

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 143 with the SMILES code CC1=CSC(=O)N1CCCC(=O)NC1=NC=CS1