5E5F
X-ray structure of the complex between RNase A and compound 4-PF6 ([(PPh3)Au(mi-pbi)Pt(Me)(DMSO)][PF6]), the heterobimetallic derivative obtained in the reaction between the organometallic compound [Pt(pbi)(Me)(DMSO)], pbi=2-(2'-pyridil)benzimidazole (compound 3) and the gold(I) compound [Au(Ph3P)][PF6]
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | ROTATING ANODE |
Source details | RIGAKU MICROMAX-007 HF |
Temperature [K] | 100 |
Detector technology | CCD |
Collection date | 2015-03-18 |
Detector | RIGAKU SATURN 944+ |
Wavelength(s) | 1.5418 |
Spacegroup name | C 1 2 1 |
Unit cell lengths | 99.487, 31.215, 69.012 |
Unit cell angles | 90.00, 90.69, 90.00 |
Refinement procedure
Resolution | 69.000 - 1.680 |
R-factor | 0.18601 |
Rwork | 0.183 |
R-free | 0.23404 |
RMSD bond length | 0.018 |
RMSD bond angle | 1.873 |
Data reduction software | HKL-2000 |
Data scaling software | HKL-2000 |
Phasing software | PHASER |
Refinement software | REFMAC (5.8.0049) |
Data quality characteristics
Overall | Outer shell | |
Low resolution limit [Å] | 69.000 | 1.710 |
High resolution limit [Å] | 1.680 | 1.680 |
Rmerge | 0.294 | |
Number of reflections | 23228 | |
<I/σ(I)> | 6.5 | 2 |
Completeness [%] | 95.0 | 88.5 |
Redundancy | 2.4 | 1.6 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, HANGING DROP | 298 | RNase A crystals were obtained using the procedure previously described by Vitagliano et al., 200028. Briefly, crystals of the protein were grown by hanging drop vapor diffusion method using a reservoir solution containing 22-24 % (w/v) PEG4K, 10 mM sodium citrate pH 5.1-5.3. The crystals are monoclinic, space group C2, with two molecules in the asymmetric unit. The adducts were prepared by a three-days soaking in a solution that comprised the standard mother liquor used for the crystal growth to which a 2.5-5 mM solution of each compound was added. Crystal soaked in this solution were mounted for the X-ray data collection without using a cryoprotectant, as done in previous studies30. |