3IJ8

Directed 'in situ' Elongation as a Strategy to Characterize the Covalent Glycosyl-Enzyme Catalytic Intermediate of Human Pancreatic a-Amylase

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SSRL BEAMLINE BL11-1
Synchrotron site	SSRL
Beamline	BL11-1
Temperature [K]	100
Detector technology	CCD
Detector	ADSC QUANTUM 315r
Wavelength(s)	0.98
Spacegroup name	P 21 21 21
Unit cell lengths	52.000, 68.470, 129.860
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	29.330 - 1.430
Rwork	0.197
R-free	0.21300
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.005
RMSD bond angle	1.010
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	CNS
Refinement software	CNS

Data quality characteristics

	Overall
Low resolution limit [Å]	29.330
High resolution limit [Å]	1.430
Rmerge	0.030
Number of reflections	85356
Completeness [%]	98.8

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.5	298	60% 2-methylpentane-2, 4-diol and 100 mM cacodylate, pH 7.5, VAPOR DIFFUSION, HANGING DROP, temperature 298.0K