7JWN
Crystal structure of Human Serum Albumin in complex with ketoprofen
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | APS BEAMLINE 19-ID |
Synchrotron site | APS |
Beamline | 19-ID |
Temperature [K] | 100 |
Detector technology | PIXEL |
Collection date | 2020-02-11 |
Detector | DECTRIS PILATUS3 6M |
Wavelength(s) | 0.979 |
Spacegroup name | C 1 2 1 |
Unit cell lengths | 170.499, 38.878, 98.501 |
Unit cell angles | 90.00, 104.47, 90.00 |
Refinement procedure
Resolution | 41.920 - 2.600 |
R-factor | 0.1855 |
Rwork | 0.183 |
R-free | 0.23070 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | 4k2c |
RMSD bond length | 0.002 |
RMSD bond angle | 1.139 |
Data reduction software | HKL-3000 |
Data scaling software | HKL-3000 |
Phasing software | MOLREP |
Refinement software | REFMAC (5.8.0266) |
Data quality characteristics
Overall | Inner shell | Outer shell | |
Low resolution limit [Å] | 50.000 | 50.000 | 2.640 |
High resolution limit [Å] | 2.600 | 7.050 | 2.600 |
Rmerge | 0.080 | 0.062 | 0.803 |
Rmeas | 0.092 | 0.071 | 0.925 |
Rpim | 0.044 | 0.034 | 0.447 |
Number of reflections | 18925 | 1022 | 851 |
<I/σ(I)> | 9.3 | 1.3 | |
Completeness [%] | 96.4 | 96.3 | 88.5 |
Redundancy | 4.2 | 4.2 | 3.5 |
CC(1/2) | 0.990 | 0.612 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, SITTING DROP | 7 | 310 | Prior to crystallization, the protein at concentration of 162 mg/ml (dissolved in 50 mM Tris pH 7.4 and 20 mM NaCl) was mixed with 100 mM ketoprofen in 100% DMSO in ratio 9:1 (final ketoprofen concentration 10 mM) and incubated for several hours at 37 oC. Then, 0.2 ul of the protein solution was mixed with 0.2 ul of the well condition (24% PEG 3350, 50 mM K2HPO4 at pH 7.0). The crystallization plate was incubated at RT for 3 months, then for several days at 37 oC, and after the growth of the first HSA crystals, the plate was transferred to RT. |