4XUD

Synthesis and evaluation of heterocyclic catechol mimics as inhibitors of catechol-O-methyltransferase (COMT): Structure with Cmpd32 ([1-(biphenyl-3-yl)-5-hydroxy-4-oxo-1,4-dihydropyridin-3-yl]boronic acid)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU FR-E+ SUPERBRIGHT
Temperature [K]	100
Detector technology	IMAGE PLATE
Collection date	2008-06-25
Detector	RIGAKU RAXIS IV++
Wavelength(s)	1.54
Spacegroup name	P 21 21 21
Unit cell lengths	43.812, 57.631, 98.249
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	49.690 - 2.400
R-factor	0.1713
Rwork	0.168
R-free	0.24100
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4xuc
RMSD bond length	0.011
RMSD bond angle	1.316
Data scaling software	SCALEPACK
Phasing software	MOLREP
Refinement software	REFMAC (5.2.0019)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	2.440
High resolution limit [Å]	2.400	6.510	2.400
Rmerge	0.198	0.110	0.696
Total number of observations	79089
Number of reflections	10266
<I/σ(I)>	7.2
Completeness [%]	100.0	99.7	100
Redundancy	7.7	6.7	7.7

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION	7	298	0.1M HEPES, 30% PEG 6000; MA000474 (JCSG core IV), drop e12 :100uM ligand, 12mg/ml protein