4CX0

Structure of bovine endothelial nitric oxide synthase Y477A mutant heme domain in complex with 6-((((3S, 5R)-5-(((6-AMINO-4- METHYLPYRIDIN-2-YL)METHOXY)METHYL)PYRROLIDIN-3-YL)OXY)METHYL)-4- METHYLPYRIDIN-2-AMINE


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1620-22% PEG3350, 0.1M CACODYLATE PH 6.0, 150-200 MM MG ACETATE, 5 MM TCEP
Crystal Properties
Matthews coefficientSolvent content
2.550.7

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 57.709α = 90
b = 106.462β = 90
c = 156.159γ = 90
Symmetry
Space GroupP 21 21 21

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDMARMOSAIC 325 mm CCDMIRRORS2012-07-06MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONSSRL BEAMLINE BL9-2SSRLBL9-2

Data Collection

Overall
ID #Resolution (High)Resolution (Low)Percent Possible (Observed)R Merge I (Observed)Net I Over Average Sigma (I)RedundancyNumber Reflections (All)Number Reflections (Observed)Observed Criterion Sigma (F)Observed Criterion Sigma (I)B (Isotropic) From Wilson Plot
12.25099.40.0816.93.650206-332.67
Highest Resolution Shell
ID #Resolution (High)Resolution (Low)Percent Possible (All)Percent Possible (Observed)R Merge I (Observed)Mean I Over Sigma (Observed)RedundancyNumber Unique Reflections (All)
12.22.2497.90.612.13.5

Refinement

Statistics
Diffraction IDStructure Solution MethodCross Validation methodStarting modelResolution (High)Resolution (Low)Number Reflections (Observed)Number Reflections (R-Free)Percent Reflections (Observed)R-Factor (Observed)R-WorkR-FreeR-Free Selection DetailsMean Isotropic B
X-RAY DIFFRACTIONOTHERTHROUGHOUTNONE2.238.6847001246899.410.157110.154750.20284RANDOM38.058
Temperature Factor Modeling
Anisotropic B[1][1]Anisotropic B[1][2]Anisotropic B[1][3]Anisotropic B[2][2]Anisotropic B[2][3]Anisotropic B[3][3]
2.94-1.82-1.12
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg34.713
r_dihedral_angle_4_deg21.022
r_dihedral_angle_3_deg16.337
r_dihedral_angle_1_deg6.363
r_angle_refined_deg1.558
r_angle_other_deg0.827
r_chiral_restr0.087
r_bond_refined_d0.012
r_gen_planes_refined0.008
r_gen_planes_other0.005
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg34.713
r_dihedral_angle_4_deg21.022
r_dihedral_angle_3_deg16.337
r_dihedral_angle_1_deg6.363
r_angle_refined_deg1.558
r_angle_other_deg0.827
r_chiral_restr0.087
r_bond_refined_d0.012
r_gen_planes_refined0.008
r_gen_planes_other0.005
r_bond_other_d0.002
r_nbd_refined
r_nbd_other
r_nbtor_refined
r_nbtor_other
r_xyhbond_nbd_refined
r_xyhbond_nbd_other
r_metal_ion_refined
r_metal_ion_other
r_symmetry_vdw_refined
r_symmetry_vdw_other
r_symmetry_hbond_refined
r_symmetry_hbond_other
r_symmetry_metal_ion_refined
r_symmetry_metal_ion_other
r_mcbond_it
r_mcbond_other
r_mcangle_it
r_mcangle_other
r_scbond_it
r_scbond_other
r_scangle_it
r_scangle_other
r_long_range_B_refined
r_long_range_B_other
r_rigid_bond_restr
r_sphericity_free
r_sphericity_bonded
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms6421
Nucleic Acid Atoms
Solvent Atoms427
Heterogen Atoms201

Software

Software
Software NamePurpose
REFMACrefinement
Hdata reduction
SCALEPACKdata scaling
REFMACphasing