4JIJ

Crystal structure of an inactive mutant of MMP-9 catalytic domain in complex with a fluorogenic synthetic peptidic substrate

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SOLEIL BEAMLINE PROXIMA 1
Synchrotron site	SOLEIL
Beamline	PROXIMA 1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2012-02-17
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.9184
Spacegroup name	P 21 21 21
Unit cell lengths	34.200, 57.400, 172.030
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	40.568 - 1.698
R-factor	0.1615
Rwork	0.160
R-free	0.19540
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4h3x
RMSD bond length	0.006
RMSD bond angle	1.084
Data reduction software	XDS
Data scaling software	XDS
Phasing software	MOLREP
Refinement software	PHENIX ((phenix.refine: 1.8_1069))

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	1.800
High resolution limit [Å]	1.698	5.070	1.700
Rmerge	0.174	0.073	1.052
Number of reflections	38427
<I/σ(I)>	9.91	26.6	2.06
Completeness [%]	99.7	99.7	98.5
Redundancy	8.97	7.83	8.92

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	6	293	Protein: 6 microL hMMP9(E402A) at 181 micro-M 0.12 M acetohydroxamic acid and 0.3 microL IT34-I at 6.9 mill-M. Reservoir: 10% PEG 20K, 0.1 M MMT (L-malic acid, MES, Tris) 75% acid/25% basic, 0.8 M NaCl, 0.02 SrCl2, 0.01% azide. Cryoprotectant: CryoProtX CM2, 0.8 M Li formate, 0.1 M (MMT 75% acid/25% basic), 9% PEG 10K, pH 6.0, VAPOR DIFFUSION, SITTING DROP, temperature 293K