5TH9

Structure determination of a potent, selective antibody inhibitor of human MMP9 (GS-5745 bound to MMP-9)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ALS BEAMLINE 5.0.1
Synchrotron site	ALS
Beamline	5.0.1
Temperature [K]	100
Detector technology	CCD
Collection date	2013-05-16
Detector	ADSC QUANTUM 315
Wavelength(s)	0.979
Spacegroup name	P 43 21 2
Unit cell lengths	168.167, 168.167, 234.735
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.641 - 2.999
R-factor	0.2193
Rwork	0.218
R-free	0.25700
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1L6J (MMP9) 1F8T (GS-5745 Fab)
RMSD bond length	0.013
RMSD bond angle	1.068
Data reduction software	HKL-2000
Data scaling software	SCALEPACK
Phasing software	PHASER
Refinement software	PHENIX (1.10.1_2155)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	3.090
High resolution limit [Å]	3.000	6.860	3.000
Rmerge	0.098	0.027	0.465
Total number of observations	412284
Number of reflections	67959
<I/σ(I)>	8.9
Completeness [%]	100.0	99.8	100
Redundancy	6.1	5.8	6.2

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.5	293	Drop: 8% (w/v) PEG 8000 0.1 M HEPES, pH 7.5 50% (v/v) Silver Bullet 21 (Hampton Research) Reservoir: 22.5% (w/v) PEG 8000 0.1 M HEPES, pH 7.5