The methods of synthesis of trans-bis(ethylamine)dichloro platinum(II) (trans-[Pt(C2H5NH2)(2)Cl-2]) and palladium(II) (trans-[Pd(C2H5NH2)(2)Cl-2]) complexes for obtaining monophase products were developed. For substance characterizations FTIR spectroscopy, thermogravimetric and X-ray diffraction analysis were used. The crystal structures of the synthesized compounds were determined using X-ray powder diffraction technique. The neutral complexes had specific system of intermolecular contacts in the crystals that allowed distinguishing two forms, A and B. Despite of the similar structure and sizes, trans[Pt(C2H5NH2)(2)Cl-2] and trans-[Pd(C2H5NH2)(2)Cl-2] complexes created different hydrogen bond networks and crystal structures. The first had a grid topology of 3(6) with the cells from three and the second - 4(4) from four complexes. It resulted in different thermal behavior. Trans- [Pt(C2H5NH2)(2)Cl-2]-A demonstrated irreversible solid state transition into B-form at 165 degrees C and got new H-bond system with the topology similar to the palladium analog (4 4 ), however, the realized complex arrangement was significantly different. The structure of B-form was stable until the decomposition at 220 degrees C. High-temperature X-ray diffraction demonstrated high elasticity of the H-bond network in trans-[Pd(C2H5NH2)(2)Cl-2]-A. Notwithstanding significant alterations during heating, the H-bond system returns the structure to its initial state. The interpretation of structural transformation was proposed. The H-bond network formation was influenced by the dynamic properties of the molecules. For the platinum compound, the option with more dense molecular packing occurred. For palladium, the atomic mass distribution was responsible for a larger molecular volume and for a more symmetrical packing. Thermal decomposition of both compounds occurred with simultaneous separation of the halogen and amminoalkyl particles resulting in a low-temperature reduction of the metal and the formation of nanoparticles with sizes in the range of 5 -10 nm. For the palladium compound, the decay in vacuum had a noticeable rate already at 100 degrees C. (C) 2019 Elsevier B.V. All rights reserved.
Crystal structure models of complex compounds [Pd(CH3NH2)4][PdBr4] (sp.gr.P4/mnc (128), a=10.6866(7)Å, c=6.7262(3)Å, V=768.16(10)Å3) and [Pt(NH3)5Cl]Br3 (sp.gr.I41/a (88), a=17.2587(5)Å; c=15.1164(3)Å, V=4502,61(10) Å3) has been determined by using the developed multipopulational parallel genetic algorithm (MPGA) and x-ray powder diffraction data.This paper presents the methodology and results of the structural analysis of these compounds obtained by application of the MPGA.
In the paper seven new ionic complex compounds were obtained by chemical reaction of H 2 [PtCl 6 l with trans-1,2-dl-diammoniumcyclohexane. The phase variety was achieved by changing acidity, crystallization rate, temperature, solvent type and the molecular ratio of reagents. The compounds were characterized by thermal and chemical analysis, IR and 1H NMR spectroscopy. Crystal structures of the five compounds were determined by X-ray powder diffraction analysis. All phases have ionic structures. In some cases H2O or HCl molecules were involved in crystal lattice. It was shown that hydrogen bonding played an important role in the variety of crystal phase formation. The crystal structures reflect precrystallizational situation in solution and especially the ion association into larger aggregates due to the formation of hydrogen bonds.
The analysis of accessible data on synthesis and crystal structure of palladium acetate is carried out. The chemical circuit of reception of palladium acetate from its nitrate solution is offered. The schemes of production of palladium acetate compounds are offered.
AbstractChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.