1SIH

AGAO in covalent complex with the inhibitor MOBA ("4-(4-methylphenoxy)-2-butyn-1-amine")

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU RU200
Temperature [K]	100
Detector technology	IMAGE PLATE
Collection date	2003-08-01
Detector	MAR scanner 345 mm plate
Spacegroup name	C 1 2 1
Unit cell lengths	157.645, 62.787, 91.657
Unit cell angles	90.00, 112.18, 90.00

Refinement procedure

Resolution	22.810 - 1.730
R-factor	0.14963
Rwork	0.149
R-free	0.16837
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.010
RMSD bond angle	1.367
Data reduction software	MOSFLM
Data scaling software	CCP4 ((SCALA)
Refinement software	REFMAC (5.1.24)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	22.810	1.770
High resolution limit [Å]	1.730	1.730
Rmerge	0.031	0.200
Number of reflections	80205
<I/σ(I)>	29	7.4
Completeness [%]	92.3	71.2
Redundancy	5.5

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	6.5	293	2 microlitres of (AGAO 10 mg/ml, 50mM HEPES pH 7.0) plus 2 microlitres of the reservoir solution (1.1M (NH4)2SO4, 150mM Na-citrate pH 6.5) Crystals were cryoprotected and soaked with MOBA. Crystals were soaked in well solution plus 20% glycerol plus 10-fold excess of MOBA., for 48 hours. The glycerol concentration was then raised to 30% over 30 minutes, prior to flash freezing., VAPOR DIFFUSION, HANGING DROP, temperature 293K