1NL9

Potent, Selective Protein Tyrosine Phosphatase 1B Inhibitor Compound 12 Using a Linked-Fragment Strategy

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU RU300
Temperature [K]	100
Detector technology	CCD
Collection date	2002-07-04
Detector	MARRESEARCH
Wavelength(s)	1.5418
Spacegroup name	P 31 2 1
Unit cell lengths	88.730, 88.730, 105.910
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	19.770 - 2.400
R-factor	0.208
Rwork	0.192
R-free	0.24700
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1TYR and initial internal refinement
RMSD bond length	0.006
RMSD bond angle	21.700 *
Data scaling software	HKL-2000
Phasing software	CNX (2000)
Refinement software	CNX (2000)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	2.490
High resolution limit [Å]	2.300	2.400
Rmerge	0.070	0.258
Number of reflections	19212
<I/σ(I)>	15.2	4.06
Completeness [%]	92.1	77.5
Redundancy	4.4	3.3

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	unknown *	7.1	277	Precipitation buffer 100 mM Hepes, 0.2 M Magnesium Acetate, 14% PEG8000, pH 7.1, VAPOR DIFFUSION, HANGING DROP, temperature 277K

Crystallization Reagents in Literatures

ID	crystal ID	solution	reagent name	concentration (unit)	details
1	1	1	protein	3-4 (mg/ml)
2	1	1	dithiothreitol	2-4 (mM)