3NU0

Design, Synthesis, Biological Evaluation and X-ray Crystal Structure of Novel Classical 6,5,6-TricyclicBenzo[4,5]thieno[2,3-d]pyrimidines as Dual Thymidylate Synthase and Dihydrofolate Reductase Inhibitors

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SSRL BEAMLINE BL9-2
Synchrotron site	SSRL
Beamline	BL9-2
Temperature [K]	200
Detector technology	CCD
Collection date	2008-12-06
Detector	MARMOSAIC 325 mm CCD
Wavelength(s)	0.975
Spacegroup name	H 3
Unit cell lengths	84.395, 84.395, 78.193
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	33.100 - 1.350
R-factor	0.18149
Rwork	0.180
R-free	0.20927
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	u072
RMSD bond length	0.035
RMSD bond angle	2.992
Data reduction software	MOSFLM
Data scaling software	SCALA
Phasing software	MOLREP
Refinement software	REFMAC (5.5.0088)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	33.100	1.420
High resolution limit [Å]	1.350	1.350
Rmerge	0.063	0.390
Number of reflections	45587
<I/σ(I)>	27	8.6
Completeness [%]	100.0	100
Redundancy	12.5	12.1

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	6.9	293	100 mM KPO4, 69% saturated AmSO4, 3% v/v ethanol, pH 6.9, VAPOR DIFFUSION, HANGING DROP, temperature 200K, temperature 293K