X-RAY DIFFRACTION
Crystallization
| Crystalization Experiments | ||||
|---|---|---|---|---|
| ID | Method | pH | Temperature | Details |
| 1 | VAPOR DIFFUSION, SITTING DROP | 6 | 293 | PROTEIN WAS CRYSTALLISED USING THE VAPOR DIFFUSION METHOD (SITTING DROP). THE WELLS CONTAINED 500 MICROLITERS OF PRECIPITANT SOLUTION AND THE DROPS WERE COMPOSED OF 1.5 MICROLITERS OF PROTEIN SOLUTION (15 MG/ML) AND 1.5 MICROLITERS OF RESERVOIR SOLUTION. THE BEST CRYSTALS WERE OBTAINED FROM A SOLUTION CONTAINING 1.6 M SODIUM MALONATE PH 6 AT 293 K. |
| Crystal Properties | |
|---|---|
| Matthews coefficient | Solvent content |
| 3.09 | 59.85 |
Crystal Data
| Unit Cell | |
|---|---|
| Length ( Å ) | Angle ( ˚ ) |
| a = 207.08 | α = 90 |
| b = 207.08 | β = 90 |
| c = 60.71 | γ = 120 |
| Symmetry | |
|---|---|
| Space Group | P 6 |
Diffraction
| Diffraction Experiment | ||||||||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| ID # | Crystal ID | Scattering Type | Data Collection Temperature | Detector | Detector Type | Details | Collection Date | Monochromator | Protocol | |||||
| 1 | 1 | x-ray | 100 | CCD | ADSC CCD | M | SINGLE WAVELENGTH | |||||||
| Radiation Source | |||||
|---|---|---|---|---|---|
| ID # | Source | Type | Wavelength List | Synchrotron Site | Beamline |
| 1 | SYNCHROTRON | ESRF BEAMLINE ID14-4 | ESRF | ID14-4 | |
Data Collection
| Overall | |||||||||||||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| 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 | 45.4 | 96.5 | 0.07 | 8.1 | 8.3 | 73593 | ||||||||||||
| 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 | 2.32 | 80 | 0.62 | 1.2 | 3.8 | |||||||||||||
Refinement
| Statistics | |||||||||||||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| Diffraction ID | Structure Solution Method | Cross Validation method | Resolution (High) | Resolution (Low) | Number Reflections (Observed) | Number Reflections (R-Free) | Percent Reflections (Observed) | R-Factor (Observed) | R-Work (Depositor) | R-Work (DCC) | R-Free (Depositor) | R-Free (DCC) | R-Free Selection Details | Mean Isotropic B | |||||
| X-RAY DIFFRACTION | SAD | THROUGHOUT | 2.2 | 179.61 | 70028 | 3705 | 97.1 | 0.209 | 0.206 | 0.27 | 0.257 | 0.3 | RANDOM | 46.22 | |||||
| Temperature Factor Modeling | ||||||
|---|---|---|---|---|---|---|
| Anisotropic B[1][1] | Anisotropic B[1][2] | Anisotropic B[2][2] | Anisotropic B[3][3] | |||
| 0.55 | 0.28 | 0.55 | -0.83 | |||
| RMS Deviations | |
|---|---|
| Key | Refinement Restraint Deviation |
| r_dihedral_angle_2_deg | 38.709 |
| r_dihedral_angle_4_deg | 19.872 |
| r_dihedral_angle_3_deg | 16.104 |
| r_dihedral_angle_1_deg | 5.958 |
| r_scangle_it | 3.011 |
| r_scbond_it | 1.995 |
| r_angle_refined_deg | 1.5 |
| r_mcangle_it | 1.165 |
| r_mcbond_it | 0.972 |
| r_angle_other_deg | 0.804 |
| Non-Hydrogen Atoms Used in Refinement | |
|---|---|
| Non-Hydrogen Atoms | Number |
| Protein Atoms | 8467 |
| Nucleic Acid Atoms | |
| Solvent Atoms | 158 |
| Heterogen Atoms | 81 |
Software
| Software | |
|---|---|
| Software Name | Purpose |
| SHARP | model building |
| SCALA | data scaling |
| SHELXCD | phasing |
| SHELXD | phasing |
| SHELXE | phasing |
| SHARP | phasing |
| REFMAC | refinement |
