3NC4
The binding of beta-D-glucopyranosyl-thiosemicarbazone derivatives to glycogen phosphorylase: a new class of inhibitors
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | SYNCHROTRON |
| Source details | EMBL/DESY, HAMBURG BEAMLINE X13 |
| Synchrotron site | EMBL/DESY, HAMBURG |
| Beamline | X13 |
| Temperature [K] | 298 |
| Detector technology | CCD |
| Collection date | 2009-02-22 |
| Detector | ADSC QUANTUM 4 |
| Wavelength(s) | 0.815 |
| Spacegroup name | P 43 21 2 |
| Unit cell lengths | 128.517, 128.517, 115.843 |
| Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
| Resolution | 27.990 - 2.070 |
| R-factor | 0.18176 |
| Rwork | 0.180 |
| R-free | 0.21972 |
| Structure solution method | FOURIER SYNTHESIS |
| Starting model (for MR) | 2prj |
| RMSD bond length | 0.009 |
| RMSD bond angle | 1.152 |
| Data reduction software | DENZO |
| Data scaling software | SCALEPACK |
| Phasing software | CNS |
| Refinement software | REFMAC (5.3.0037) |
Data quality characteristics
| Overall | Outer shell | |
| Low resolution limit [Å] | 30.000 | 2.110 |
| High resolution limit [Å] | 2.070 | 2.070 |
| Rmerge | 0.084 | 0.435 |
| Number of reflections | 48018 | |
| <I/σ(I)> | 9.59 | 3.72 |
| Completeness [%] | 80.4 | 83.1 |
| Redundancy | 2.5 | 2.3 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | SMALL TUBES | 6.7 | 289 | Crystals grown from 20 mg/ml of protein in a buffer solution containing 10 mM BES pH 6.7, 1 mM EDTA, 3 mM DTT. Crystals were soaked with 20mM inhibitor in 20% DMSO for 21 hrs 10 mins, pH 6.7, SMALL TUBES, temperature 289K |
