1NCE

Crystal structure of a ternary complex of E. coli thymidylate synthase D169C with dUMP and the antifolate CB3717

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU RU200
Temperature [K]	298
Detector technology	IMAGE PLATE
Collection date	1998-12-21
Detector	RIGAKU RAXIS II
Spacegroup name	P 63
Unit cell lengths	127.100, 127.100, 68.100
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	36.690 - 2.400
R-factor	0.187
Rwork	0.187
R-free	0.24600
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	1KCE with waters and ligands removed
RMSD bond length	0.008
RMSD bond angle	24.300 *
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	CNS
Refinement software	CNS

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	40.000	2.550
High resolution limit [Å]	2.400	2.400
Rmerge	0.174
Number of reflections	24679
<I/σ(I)>	8.1	1.9
Completeness [%]	100.0	100
Redundancy	8.7

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	9.1	298	potassium phosphate, EDTA, ammonium sulfate, DTT, pH 9.1, VAPOR DIFFUSION, HANGING DROP, temperature 298.0K

Crystallization Reagents in Literatures

ID	crystal ID	solution	reagent name	concentration (unit)	details
1	1	drop	protein	13 (mg/ml)
10	1	reservoir	dithiothreitol	10 (mM)
11	1	reservoir	ammonium sulfate	2.4 (M)
2	1	drop	potassium phosphate	10 (mM)
3	1	drop	EDTA	50000 (mM)
4	1	drop	ammonium sulfate	1.2 (M)
5	1	drop	dithiothreitol	10 (mM)
6	1	drop	dUMP	6 (mM)
7	1	drop	CB3717	40000 (mM)
8	1	reservoir	potassium phosphate	20 (mM)
9	1	reservoir	EDTA	100000 (mM)