5LH4

Trypsin inhibitors for the treatment of pancreatitis - cpd 1

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SLS BEAMLINE X10SA
Synchrotron site	SLS
Beamline	X10SA
Temperature [K]	100
Detector technology	CCD
Collection date	2007-12-14
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.99184
Spacegroup name	P 21 21 21
Unit cell lengths	54.585, 58.235, 66.666
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	20.060 - 1.370
R-factor	0.1537
Rwork	0.152
R-free	0.17890
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	inhouse
RMSD bond length	0.010
RMSD bond angle	1.200
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	BUSTER (2.9.6)

Data quality characteristics

	Overall
Low resolution limit [Å]	66.680
High resolution limit [Å]	1.370
Number of reflections	42363
<I/σ(I)>	19.34
Completeness [%]	93.4
Redundancy	5.76

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION	7.5	298	Crystallization Reservoir Solution: 25 % PEG3350, 0.2 M LISO4, 100 MM HEPES PH 7.5 Crystallization Protein Solution: 100 MG/ML IN 50MM TRIS PH 7.5, 150MM NACL, 5 MM CACL2. Complex Formation Method = Soaking Crystallization Protocol = equal volumes (2ul+2um) Crystallization Method = Vapor diffusion - Hanging drop Cryo Protocol: prior to data collection the crystal was plunged into liquid nitrogen.