4X1I

Discovery of cytotoxic Dolastatin 10 analogs with N-terminal modifications

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 17-ID
Synchrotron site	APS
Beamline	17-ID
Temperature [K]	100
Detector technology	PIXEL
Collection date	2012-02-09
Detector	DECTRIS PILATUS 6M
Wavelength(s)	1.0
Spacegroup name	P 21 21 21
Unit cell lengths	66.140, 128.210, 255.140
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.300 - 3.110
R-factor	0.194
Rwork	0.191
R-free	0.25290
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3hkb
RMSD bond length	0.009
RMSD bond angle	1.090
Data scaling software	SCALEPACK
Phasing software	BUSTER
Refinement software	BUSTER (2.11.5)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	3.150
High resolution limit [Å]	3.100	8.400	3.100
Rmerge	0.106	0.042
Total number of observations	258475
Number of reflections	40139
<I/σ(I)>	5.3
Completeness [%]	99.9	98.8	99.7
Redundancy	6.4	6.2	6.3

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	6.8	291	5% PEG 400, 0.1M LiSO4, 5-7% PEG 20K, 50 mM K-PIPES