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 | ||||
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ID | Method | pH | Temperature | Details |
1 | 6 | 20-22% PEG3350, 0.1M CACODYLATE PH 6.0, 150-200 MM MG ACETATE, 5 MM TCEP |
Crystal Properties | |
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Matthews coefficient | Solvent content |
2.5 | 50.7 |
Crystal Data
Unit Cell | |
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Length ( Å ) | Angle ( ˚ ) |
a = 57.709 | α = 90 |
b = 106.462 | β = 90 |
c = 156.159 | γ = 90 |
Symmetry | |
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Space Group | P 21 21 21 |
Diffraction
Diffraction Experiment | ||||||||||||||
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ID # | Crystal ID | Scattering Type | Data Collection Temperature | Detector | Detector Type | Details | Collection Date | Monochromator | Protocol | |||||
1 | 1 | x-ray | 100 | CCD | MARMOSAIC 325 mm CCD | MIRRORS | 2012-07-06 | M | SINGLE WAVELENGTH |
Radiation Source | |||||
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ID # | Source | Type | Wavelength List | Synchrotron Site | Beamline |
1 | SYNCHROTRON | SSRL BEAMLINE BL9-2 | SSRL | BL9-2 |
Data Collection
Overall | |||||||||||||||||||
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ID # | Resolution (High) | Resolution (Low) | Percent Possible (Observed) | R Merge I (Observed) | Net I Over Average Sigma (I) | Redundancy | Number Reflections (All) | Number Reflections (Observed) | Observed Criterion Sigma (F) | Observed Criterion Sigma (I) | B (Isotropic) From Wilson Plot | ||||||||
1 | 2.2 | 50 | 99.4 | 0.08 | 16.9 | 3.6 | 50206 | -3 | 32.67 |
Highest Resolution Shell | |||||||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
ID # | Resolution (High) | Resolution (Low) | Percent Possible (All) | Percent Possible (Observed) | R Merge I (Observed) | Mean I Over Sigma (Observed) | Redundancy | Number Unique Reflections (All) | |||||||||||
1 | 2.2 | 2.24 | 97.9 | 0.61 | 2.1 | 3.5 |
Refinement
Statistics | |||||||||||||||||||
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Diffraction ID | Structure Solution Method | Cross Validation method | Starting model | Resolution (High) | Resolution (Low) | Number Reflections (Observed) | Number Reflections (R-Free) | Percent Reflections (Observed) | R-Factor (Observed) | R-Work | R-Free | R-Free Selection Details | Mean Isotropic B | ||||||
X-RAY DIFFRACTION | OTHER | THROUGHOUT | NONE | 2.2 | 38.68 | 47001 | 2468 | 99.41 | 0.15711 | 0.15475 | 0.20284 | RANDOM | 38.058 |
Temperature Factor Modeling | ||||||
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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 | |
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Key | Refinement Restraint Deviation |
r_dihedral_angle_2_deg | 34.713 |
r_dihedral_angle_4_deg | 21.022 |
r_dihedral_angle_3_deg | 16.337 |
r_dihedral_angle_1_deg | 6.363 |
r_angle_refined_deg | 1.558 |
r_angle_other_deg | 0.827 |
r_chiral_restr | 0.087 |
r_bond_refined_d | 0.012 |
r_gen_planes_refined | 0.008 |
r_gen_planes_other | 0.005 |
Non-Hydrogen Atoms Used in Refinement | |
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Non-Hydrogen Atoms | Number |
Protein Atoms | 6421 |
Nucleic Acid Atoms | |
Solvent Atoms | 427 |
Heterogen Atoms | 201 |
Software
Software | |
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Software Name | Purpose |
REFMAC | refinement |
H | data reduction |
SCALEPACK | data scaling |
REFMAC | phasing |