Thermal behavior of the saccharinates of K+, Na+, Rb+, Cs+ and NH4+: structural inferences
TL;DR: In this paper, four alkali saccharinates: K 3 (sac) 3 ·2H 2 O (KSac), Rb 2(sac) 2 ·H 2O (RbSac), ammonium saccharinate (AmmSac), Cs(Hsac)(sac)·H2O (CsSac)) and CsSac were synthesized and their thermal decomposition was investigated in the temperature interval 293-873 K by means of thermogravimetric methods (TG, DTG, DTA) in static atmosphere of helium and
About: This article is published in Thermochimica Acta.The article was published on 2000-08-28. It has received 17 citations till now. The article focuses on the topics: Thermal decomposition.
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TL;DR: In this paper, a wide variety of metal species based on mononuclear, binuclear, polynuclear complexes and extended coordination polymers are discussed in relation to the coordination modes of the anion, i.e., monodentate (through the N-atom or the carbonylic O-atom), bidentate, tridentate or bridge forming.
180 citations
TL;DR: In this paper, the authors trace the evolution of supramolecular chemistry and crystal engineering starting from the early nineties and projects a center stage for chemistry in the natural sciences.
Abstract: Advances in supramolecular chemistry and crystal engineering reported from India within the last decade are highlighted in the categories of new intermolecular interactions, designed supramolecular architectures, network structures, multi-component host-guest systems, cocrystals, and polymorphs. Understanding self-assembly and crystallization through X-ray crystal structures is illustrated by two important prototypes — the large unit cell of elusive saccharin hydrate, Na16(sac)16 · 30H2O, which contains regular and irregular domains in the same structure, and by the Aufbau build up of zinc phosphate framework structures, e.g. ladder motif in [C3N2H12][Zn(HPO4)2] to layer structure in [C3N2H12][Zn2(HPO4)3] upon prolonged hydrothermal conditions. The pivotal role of accurate X-ray diffraction in supramolecular and structural studies is evident in many examples. Application of the bottomup approach to make powerful NLO and magnetic materials, design of efficient organogelators, and crystallization of novel pharmaceutical polymorphs and cocrystals show possible future directions for interdisciplinary research in chemistry with materials and pharmaceutical scientists. This article traces the evolution of supramolecular chemistry and crystal engineering starting from the early nineties and projects a center stage for chemistry in the natural sciences.
74 citations
TL;DR: Not far from a crystal nucleus?
Abstract: Not far from a crystal nucleus? The complex crystal structure of sodium saccharin "dihydrate"could be a good model for nucleation (see graphic). The asymmetric unit contains 362 atoms and much water, and the crystal contains ordered and disordered regions. Amazingly, the crystal structure of this metastable compound was not determined for 125 years following its isolation, although it is manufactured in bulk.
55 citations
TL;DR: The thermal decomposition behavior of triethanolamine (TEA) and monoethanolethylenediamine (me-en) complexes was studied under non-isothermal conditions by TG, DTA and DTG in dynamic nitrogen atmosphere as discussed by the authors.
28 citations
TL;DR: In this paper, a literature survey of the infrared carbonyl stretching bands of 73 solid saccharinates, saccharin and the saccharini nitranion (the latter in diluted DMSO solution) is presented.
27 citations
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TL;DR: In this article, the thermal decomposition of saccharin was studied in static air atmosphere and the final decomposition products were identified by XRPD as the respective metal oxides and the kinetic parameters, such as the order of reaction and energy of activation for the dehydration stage, were evaluated and the thermal stabilities of the complexes were discussed.
Abstract: The thermal decompositions of Mn(II), Fe(II), Co(II), Ni(II), Cu(II) and Zn(II) complexes of saccharin were studied in static air atmosphere. All of the complexes contain four molecules of coordination water and two molecules of crystallization water. The water molecules were removed in a single stage, except from the Zn(II) complex, which exhibited two endothermic effects. The dehydration process was usually accompanied by a sharp colour change. The anhydrous complexes exhibited a phase transition and the decomposition or combustion of saccharin occurred in the second and subsequent stages. The final decomposition products were identified by XRPD as the respective metal oxides. The kinetic parameters, such as the order of reaction and energy of activation for the dehydration stage, were evaluated and the thermal stabilities of the complexes are discussed.
59 citations
TL;DR: The results concerning the number of bands attributable to the abovementioned vibrations, their frequencies and intensities were correlated with the crystallographically determined type of metal-to-ligand bonding, on the one hand, and the structurally different SO2 groups as mentioned in this paper.
Abstract: The infrared spectra of a series of metal saccharinates (those of Na, Mg, Mn Fe, Co; Ni, Zn, Cd, Pb as well as mercury(II) saccharinate and chloromercury(II) saccharinate) were studied in the region of the antisymmetric and symmetric SO2 stretching vibrations [vas(SO2) and vs(SO2) hereafter]. The results concerning the number of bands attributable to the abovementioned vibrations, their frequencies and intensities were correlated with the crystallographically determined type of metal-to-ligand bonding, on the one hand, and the number of the structurally different SO2 groups, on the other. It was shown that, irrespective on whether the sulphonyl oxygen atoms do or do not participate in bonding to the metal atom and/or in hydrogen bonding and irrespective on the type of the metal-to-saccharin bond (from covalent to purely ionic), the frequencies of both vas(SO2) and vs(SO2) modes are lower for the metal saccharinates than for saccharin itself, the effect being more pronounced in the case of the vas...
52 citations
TL;DR: In this paper, the frequency of the stretching vibrations in a number of metal saccharinates with known structues (Na, Mg, Mn, Fe, Co, Ni, Zn, Cd and Hg compounds were studied) are lower than in saccharine itself.
43 citations
TL;DR: The FT IR spectra, at temperatures from liquid-nitrogen boiling (LNT) up to room temperature (RT), as well as the RT Raman solid-state spectra of protonated and deuterated ammonium saccharinate and of a series of alkali (Na, K, Rb, Cs) saccharinates are studied.
32 citations
TL;DR: In this paper, the synthesis of a vanadyl(IV)/saccharin complex is reported, which differs considerably from all known divalent metal-saccharinates and its bonding characteristics.
Abstract: The synthesis of a new vanadyl(IV)/saccharin complex is reported. Its bonding characteristics differ considerably from all known divalent metal-saccharinates. In this complex a VO(OH)+ moiety is coordinated to a saccharin molecule through its carbonyl oxygen and to a saccharinate ion through its deprotonated nitrogen. Two water molecules complete the coordination sphere. X-ray powder diagrams, infrared- and electronic absorption-spectra were recorded and analyzed for the characterization of the compound and its coordination properties. Besides, the magnetic susceptibility and the thermal behaviour were also investigated.
31 citations