4CTN
Glucopyranosylidene-spiro-iminothiazolidinone, a New Bicyclic Ring System: Synthesis, Derivatization, and Evaluation as Glycogen Phosphorylase Inhibitors by Enzyme Kinetic and Crystallographic Methods
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | SYNCHROTRON |
| Source details | SRS BEAMLINE PX10.1 |
| Synchrotron site | SRS |
| Beamline | PX10.1 |
| Temperature [K] | 298 |
| Detector technology | CCD |
| Collection date | 2007-11-16 |
| Detector | MARRESEARCH |
| Spacegroup name | P 43 21 2 |
| Unit cell lengths | 127.760, 127.760, 116.040 |
| Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
| Resolution | 32.030 - 2.100 |
| R-factor | 0.18305 |
| Rwork | 0.181 |
| R-free | 0.21837 |
| Structure solution method | MOLECULAR REPLACEMENT |
| Starting model (for MR) | 2pyd |
| RMSD bond length | 0.006 |
| RMSD bond angle | 1.053 |
| Data reduction software | MOSFLM |
| Data scaling software | SCALA |
| Phasing software | PHASER |
| Refinement software | REFMAC (5.7.0032) |
Data quality characteristics
| Overall | Outer shell | |
| Low resolution limit [Å] | 35.700 | 32.030 |
| High resolution limit [Å] | 2.100 | 2.100 |
| Rmerge | 0.090 | 0.430 |
| Number of reflections | 55833 | |
| <I/σ(I)> | 15.9 | 4.6 |
| Completeness [%] | 99.2 | 99.8 |
| Redundancy | 5 | 4.9 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | 6.8 | 25MG/ML ENZYME, 1MM SPERMINE, 10MM BES, 3MM DTT, 0.1MM EDTA, PH 6.7, AT 16OC. |
