3QKQ

Protein Tyrosine Phosphatase 1B - W179F mutant bound with vanadate

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU RU200
Temperature [K]	100
Detector technology	IMAGE PLATE
Collection date	2009-01-08
Detector	RIGAKU RAXIS IV++
Wavelength(s)	1.5418
Spacegroup name	P 31 2 1
Unit cell lengths	88.620, 88.620, 104.320
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	38.370 - 2.200
R-factor	0.1987
Rwork	0.196
R-free	0.25380
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2CM2 with the active site water molecules removed
RMSD bond length	0.009
RMSD bond angle	1.172
Data scaling software	d*TREK (9.4SSI)
Phasing software	PHASER (2.1.4)
Refinement software	PHENIX (1.6.4_486)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	38.370	38.370	2.280
High resolution limit [Å]	2.200	4.740	2.200
Rmerge	0.108	0.049	0.494
Total number of observations		13852	13210
Number of reflections	24220
<I/σ(I)>	7.9	19.4	2.7
Completeness [%]	98.7	99.2	97.3
Redundancy	5.51	5.22	5.61

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.5	277	2uL of protein solution, 0.5 uL sucrose 30 % (w/v) and 3 uL of precipitant solution (0.1 M Hepes pH 7.5, 0.2 M magnesium acetate and 15-20 % polyethylene glycol 8000). The protein solution was prepared with 15 uL of 12 mg/mL PTP1B W179F in 10 mM Tris pH 7.5, 25 mM NaCl, 0.2 mM EDTA and 3 mM DTT, and 0.5 uL of 60 mM of sodium vanadate. The well solution was 500 uL of precipitant solution., vapor diffusion, sitting drop, temperature 277K