4XUC

Synthesis and evaluation of heterocyclic catechol mimics as inhibitors of catechol-O-methyltransferase (COMT): Structure with Cmpd18 (1-(biphenyl-3-yl)-3-hydroxypyridin-4(1H)-one)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU FR-E+ SUPERBRIGHT
Temperature [K]	100
Detector technology	CCD
Collection date	2008-05-16
Detector	RIGAKU SATURN 944+
Wavelength(s)	1.54
Spacegroup name	P 21 21 21
Unit cell lengths	43.741, 57.201, 98.182
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	49.450 - 1.800
R-factor	0.1757
Rwork	0.174
R-free	0.21560
RMSD bond length	0.013
RMSD bond angle	1.443
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	1.830
High resolution limit [Å]	1.800	4.880	1.800
Rmerge	0.073	0.052	0.471
Total number of observations	160781
Number of reflections	23411
<I/σ(I)>	13.4
Completeness [%]	99.2	99.7	96.5
Redundancy	6.9	13.1	4.5

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION		298	0.1M MES, pH 6.5, 0.1M NaOAc, 30% PEG 2000MME; MA000417 (PEGsII), drop b10 :100uM ligand, 11mg/ml protein