2ORP

Murine inducible nitric oxide synthase oxygenase domain (delta 114) 2-[4-(2-Imidazol-1-yl-6-methyl-pyrimidin-4-yl)-1-isobutyryl-piperazin-2-yl]-N-[2-(4-methoxy-phenyl)-ethyl]-acetamide complex

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SSRL BEAMLINE BL7-1
Synchrotron site	SSRL
Beamline	BL7-1
Temperature [K]	100
Detector technology	IMAGE PLATE
Collection date	1998-04-09
Detector	MAR scanner 345 mm plate
Wavelength(s)	1.08
Spacegroup name	P 21 21 21
Unit cell lengths	63.230, 73.750, 93.560
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	19.750 - 1.970
Rwork	0.217
R-free	0.25200
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	1nos
RMSD bond length	0.007
RMSD bond angle	0.900
Data reduction software	MOSFLM
Data scaling software	CCP4 ((SCALA))
Phasing software	X-PLOR
Refinement software	CNS (1.1)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	19.750	2.080
High resolution limit [Å]	1.970	1.970
Rmerge	0.090	0.289
Number of reflections	21034
<I/σ(I)>	5.4	2.5
Completeness [%]	95.3	95.3
Redundancy	3.6	3.1

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	4.7	308	CRYSTALS OF MURINE DELTA114 INOS WERE PREPARED IN THE PRESENCE OF IMIDAZOLE FOLLOWING THE PROCEDURES OF CRANE ET AL. (REFERENCE 1) AS FOLLOWS: THE 6 UL CRYSTALLIZATION DROPS CONTAINED 20 MG/ML MURINE DELTA114 INOS, 20 MM HEPES PH 7.6, 5 % GLYCEROL, 0.5 MM DTT, 6.8 % PEG-3350, 60 MM NA2SO3, AND 50 MM IMIDAZOLE/ MALATE BUFFER PH 4.7 WERE PLACED OVER A 1 ML RESERVOIR CONTAINING 13.6 % PEG-3350, 120 MM NA2SO3, AND 100 MM IMIDAZOLE/MALATE BUFFER PH 4.7. THESE CRYSTALS WERE SOAKED FOR 25 HOURS IN 5 UM 2-[4-(2-Imidazol-1-yl-6- methyl-pyrimidin-4-yl)-1-isobutyryl-piperazin-2-yl]-N- [2-(4-methoxy-phenyl)-ethyl]-acetamide, 14 % PEG-3350, 1 MM NAN3, 50 MM MES PH 6.5 AND 50 MM NA2SO3. THE, pH 4.70, VAPOR DIFFUSION, HANGING DROP, temperature 308K