H2O Compounds Research Articles

Synthesis, structural characterization and antitumoral activity of (NH4)4Li2V10O28.10H2O compound

The decavanadate compound with inorganic cations, (NH4)4Li2V10O28.10H2O, was synthesized by slow evaporation from aqueous solution. It was characterized by Infrared (IR) spectroscopy, Scanning Electron Microscopy (SEM) with Energy Dispersive X-Ray Analysis (EDX) as well as thermal analysis such as Differential Scanning Calorimetry (DSC), differential thermal analysis (DTA) and thermogravimetry (TG). The formula unit consists of one decavanadate cluster [V10O28]6−, two lithium cations, four ammonium ions and ten water molecules. In the crystal, molecules are linked into a three-dimensional network by O-H…O and N-H…O hydrogen bonds. The prevalence of these intermolecular interactions was confirmed by an analysis of the Hirshfeld surface (HS) and fingerprint plots (FP). The relative contribution of different interactions to the HS indicates that the O…H/H…O and H…H contacts account 86.8% of the total HS area. In this study, the cytotoxic and the antiproliferative activities of (NH4)4Li2V10O28.10H2O on human cancer cells (U87, IGR39 and MDA-MB-231) were investigated. This compound demonstrated dose-dependent antiproliferative activity on U87, MDA-MB-231 and IGR39 with IC50 values of 2 µg/mL, 18 µg/mL and 12 µg /mL, respectively. These data provide evidence on the potential anticancer activity of (NH4)4Li2V10O28.10H2O.

Characterization of bioactive ceramic coatings synthesized by plasma electrolyte oxidation on AZ31 magnesium alloy having different Na2SiO3·9H2O concentrations

Surface modification of magnesium alloys by Plasma Electrolytic Oxidation (PEO) method can be a great help for the development of degradable implants in clinical applications. In this study, the aim was to investigate the effect of changing Na2SiO3·9H2O concentration (5, 10, and 15 g L−1) in a bath containing Ca2H4P2O4, Na3PO4.12H2O, NaF, and KOH compounds at pH = 12 and a conductivity of 20 mS/cm. Coating characterization was performed by Field Emission Scanning Electron Microscopy (FESEM), Energy-Dispersive X-ray Spectroscopy (EDX), X-ray Diffraction (XRD), nanoindentation, Electrochemical Impedance Spectroscopy (EIS), Fourier Transform-Infrared Spectroscopy (FTIR), and immersion in Simulated Body Fluid (SBF). The formed bioactive ceramic coating contains bioelements from the electrolyte, including Ca, P, Si, F, and Na. And, as Na2SiO3·9H2O concentration increases, it also silicon, sodium, and oxygen values in the coating, and reduces magnesium and phosphor values. Pore density decreases in the coatings by an increase in Na2SiO3·9H2O concentration. The optimum bioactive ceramic coating considering hardness and corrosion resistance contains 10 g L−1 of Na2SiO3·9H2O. The optimized bioactive ceramic coating has the ability to form carbonate hydroxyapatite after immersion in SBF at 37 °C for one and four days.

Lignin from energy plant (Arundo donax): Pyrolysis kinetics, mechanism and pathway evaluation

Pyrolysis of lignin was conducted and main decomposition temperature range was 250–500 °C and the maximum mass loss of lignin occurred at 300–350 °C (10–20 °C/min). Activation energy was ranged from 166 to 182 kJ/mol and lnA was ranged from 35 to 40. All fitting peaks described by mechanism function of random nucleation followed by growth. There was apparent infrared spectroscopy absorbance at 3565, 2950, 2367, 2182, 1775, and 1103 cm−1 because of vibrations of functional group in H2O, CH4, CO2, CO, CO and O-containing compounds. Main composition of bio-oil was phenols and main carbon distribution was ranged from C5 to C8. Ratio of p-hydroxyphenyl, guaiacyl and syringyl structures in bio-oil varied with pyrolysis temperature. Main pyrolysis mechanism of lignin was cracking of typical structure into phenols, cracking of carboxyl groups in side chains to form CO2 and carbonization of aromatic structure to biochar. Lignin showed higher biochar yield (up to 47.46%) and biochar from lignin pyrolysis have high carbon and low ash content. Comparing with direct pyrolysis, fermentation-pyrolysis pathway produced extra high-value products of ethanol (16.70%) and CO2 (8.5%). It indicated a potential and high-value pathway of lignin produced in cellulosic ethanol plants.

Study on the Kinetics and Pyrolysis Behavior of Waste Containing Urea-Formaldehyde Resins

In this work, we studied the kinetics and behavior of wood panel wastes containing ureaformaldehyde resins. For this purpose, we used a TG-FTIR coupled system to analyze the gaseous products of the pyrolysis. With the results, we obtained the models that provide theoretical evidence and data support for the studied reactions. According to our findings, the pyrolysis of the ureaformaldehyde components displayed two stages, and the second stage presented a higher intensity. At a temperature of 900 °C, the gas generation rate for hard UF (UF1) was 32.6% higher than that for soft UF (UF2). When temperature increased from 600 °C to 900 °C, the increase of the gas generation rate was relatively small. In addition, the reaction order was obtained using the CoatsRedfern method, which provided a value for the reaction order of 1.4. The activation energy of UF1 was slightly higher than that of UF2. The FTIR analysis indicated that the main gaseous products of the pyrolysis of the urea-formaldehyde resin samples were CO2, H2O, and other compounds containing the C–H and the N–H bond as well as carbonyl groups. In addition, it was determined that Nitrogen was mainly present in the form of hydronitrogen compounds but not as nitrogen oxides. These last may represent a higher degree of pollution.

Edge-Plane Exposed N-Doped Carbon Nanofibers Toward Fast K-Ion Adsorption/Diffusion Kinetics for K-Ion Capacitors

Sluggish kinetics severely limit the development of potassium-ion hybrid capacitors (PIHCs). Exposing active sites is recognized as an ideal strategy to resolve this issue, but the corresponding ma...

New Silver(I) Coordination Compound Loaded into Polymeric Nanoparticles as a Strategy to Improve In Vitro Anti-Helicobacter pylori Activity.

Helicobacter pylori inhabits the gastric epithelium and can promote the development of gastric disorders, such as peptic ulcers, acute and chronic gastritis, mucosal lymphoid tissue (MALT), and gastric adenocarcinomas. To use nanotechnology as a tool to increase the antibacterial activity of silver I [Ag(I)] compounds, this study suggests a new strategy for H. pylori infections, which have hitherto been difficult to control. [Ag (PhTSC·HCl)2] (NO3)·H2O (compound 1) was synthesized, characterized, and loaded into polymeric nanoparticles (PN1). PN1 had been developed by nanoprecipitation with poly(ε-caprolactone) polymer and poloxamer 407 surfactant. System characterization assays showed that the PNs had adequate particle sizes and ζ-potentials. Transmission electron microscopy confirmed the formation of polymeric nanoparticles (PNs). Compound 1 had a minimum inhibitory concentration for H. pylori of 3.90 μg/mL, which was potentiated to 0.781 μg/mL after loading. The minimum bactericidal concentration of 7.81 μg/mL was potentiated 5-fold to 1.56 μg/mL in PN. Compound 1 loaded in PN1 displayed better activity for H. pylori biofilm formation and mature biofilm. PN1 reduced the toxicity of compound 1 to MRC-5 cells. Loading compound 1 into PN1 inhibited the mutagenicity of the free compound. In vivo, the system allowed survival of Galleria mellonella larvae at a concentration of 200 μg/mL. This is the first demonstration of the antibacterial activity of a silver complex enclosed in polymeric nanoparticles against H. pylori.

Titaneon: the eco smart lamp to degrade cigarette smoke pollutants

The purpose of this study is to find out the results of the “TITANEON” degradation power test on hazardous CO (carbon monoxide) compounds qualitatively and quantitatively and to explain the working system of the lamp. The research methods used in this study are (a) preparation: tools and materials, design testing tools; (b) conducting research: TiO2/Co synthesis, coating, tool performance test and data processing and analysis; (c) evaluation. The test results in this study were divided into two, namely qualitative and quantitative. In the qualitative test results, the “TITANEON” lamp is able to degrade CO compounds for 20 minutes. The quantitative results from 0 minutes amounted to 15526.24 ppm, 5 minutes later the CO concentration was 6202.82, in the next 15 minutes CO concentration was 2549.98 ppm and in the last 20 minutes the CO concentration was 1871.89 ppm. The system works, namely the first light that involves TiO2 nanoparticles will excite electrons from the valence band to the conduction band while producing positive holes in the valence band and negatively charged electron pairs. After that, TiO2 nanoparticles are transformed into super oxide compounds which release active oxygen species (O2 radicals and OH radicals), these compounds will degrade cigarette smoke compounds into CO2 and H2O compounds through photocatalytic mechanisms.

In-situ synchronous carbonation and self-activation of biochar/geopolymer composite membrane: Enhanced catalyst for oxidative degradation of tetracycline in water

A new biochar/geopolymer composite membrane (BC/GM) was prepared by an in-situ synchronous carbonation and self-activation process from two sustainable materials. The monolithic geopolymer membrane (GM) served not only as a porous support, achieving good dispersion and retrieve of biochar (BC), but also as a solid base for in-situ activating BC during carbonization of lignin precursor. The obtained BC/GM contained a hierarchically porous structure (exhibiting a bi-modal pore size distribution at 3.54 and 16.53 nm, respectively), having a large specificsurface area (37.46 m2/g, 28 times of BC), containing rich functional groups (COH, CO and OCO, etc.) and a high degree of graphitization (evidenced by a lower value of ID/IG = 0.81) which exhibited a high activity in decomposing H2O2 to generate ·OH radicals for degradation of tetracycline (TC). Nearly 100% of TC (50 mg/L, 100 mL) was removed by 0.15 g BC/GM (1 mL H2O2, pH 5.0, 60 °C, 5 h). It also showed a good stability and reusability during 5 repeated cycling. EPR, XPS, FTIR and Raman analysis suggested the phenolic-OH, ketone, quinone moieties and defect structures in BC contributed to the generation of ·OH through transferring electrons to H2O2, while the graphitized carbon in BC with porous structure and large surface area provided intimate contact between catalyst and TC molecules that accordingly enhanced the electron conductivity and suppressed the decay of ·OH radicals during redox reaction, which eventually realized the efficient degradation of TC into CO2, H2O, and other inorganic compounds through ring-opening reaction, isomerization, demethylation, deamination, and dehydration reaction.

Effect of liquid smoke on surface morphology and tensile strength of Sago Fiber

This study aims to identify the effect of liquid smoke treatment on surface morphology and tensile strength of sago fiber (SF), including chemical reactions during the treatment. The proposed study is divided into two steps, fiber treatment and property tests. The first treatment, SF was immersion in the liquid smoke solution for 1, 2, 3, 4, and 5 hours, then dried for 1 hour which then characterized SEM, universal machine testing machine, X-Ray diffractometer (XRD), and Fourier transform infrared spectrometer (FTIR). The acetic acid in liquid smoke reacts with fiber to form fiber-liquid and H2O compounds. The heating process degrades H2O content in fibers and decomposes C and C elements to close together forming strong chemical bonds so that the fiber morphology become rough, porous, grooved and increasing the tensile strength of the fiber. But excessive heating treatment makes fibers more fragile because the H2O elements degrade too low. Dominant percentage of SF crystallization occurred after 4 and 5 hours, 64.7 and 66.9 %, respectively among other durations, a significant increase of tensile strength 50.813 MPa was achieved by 1-hour immersion in liquid smoke. Hence, as alternative to improve the mechanical characteristics of SF, immersion in liquid smoke should be applied. Furthermore, studies of similar treatment on other natural fibers can also be considered in the future.

Preparation of water-soluble amorphous erbium borate (ErBO3.3H2O) nanoparticles with positive charge

We report a simple one-step protocol for the preparation of nearly monodisperse and highly water-soluble erbium borate nanoparticles through a co-precipitation method. Erbium ions were precipitated by boric acid/sodium hydroxide buffer with a pH of 9.2 in the presence of polyethylene glycol (2000 gmol−1) (PEG). As a result of the X-ray diffraction analysis, it was determined that the products that were precipitated in the medium with/without PEG were amorphous and the calcined product has an appropriate pattern for the vaterite-type ErBO3 crystal structure. Infrared spectrophotometer and thermal gravimetric analysis revealed the chemical formulation of the ErBO3.3H2O compound. It was found that partially spherical nanoparticles have a size of 15 ± 6 nm according to TEM images. The average particle size was also measured in the water using dynamic light scattering method. The particles size is equal to about 100 nm in water and the zeta potential of particles is + 41 mV, which indicates a highly stable colloidal solution. Besides ErBO3.3H2O nanoparticles showed strong paramagnetism, their Bohr magnetron number was found as 9.48. Thus, these nanoparticles have promising properties for biomedical applications, such as cell targeting, drug delivery, and bioimaging.

Synthesis of a novel phosphorus-nitrogen flame retardant and its application in epoxy resin

A novel phosphorus-nitrogen flame retardant named as melamine phenyl phosphate (MAPPO) was synthesized successfully via the neutralization reaction between phenylphosphonic acid (PPOA) and melamine (MA). The chemical structure of MAPPO was characterized by Fourier transform infrared spectra (FT-IR), nuclear magnetic resonance (NMR) and element analysis (EA). MAPPO was introduced into epoxy resin by blending to improve the flame retardancy. Flame retardancy and combustion behavior of EP/MAPPO were investigated by limiting oxygen index (LOI) test, vertical burning (UL-94) test and cone calorimeter test. UL-94 and LOI tests results showed EP containing 18 wt% MAPPO passed the UL-94 V-0 rating and got a high LOI value of 33%. In the cone calorimeter test, compared with that of EP, the values of peak of heat release rate (HRR), total heat release (THR), peak of smoke production rate (PSPR) and total smoke production (TSP) of modified EP were reduced by 58.7%, 40%, 49% and 61.6%, respectively. By analyzing the volatile pyrolysis products of MAPPO, it was known that MAPPO mainly produced CO2, NH3, H2O and other nitrogen-containing compounds, which diluted the concentration of fuel gases and oxygen during combustion. Meanwhile, the char residue of EP/MAPPO system after combustion was also analyzed by scanning electron microscope (SEM), FT-IR and Raman tests, and the results showed MAPPO was able to promote the crosslinking of EP leading to the formation of compact char layer containing P–O–C, PO and CC, etc. In a word, the enhancement in flame retardancy was attributed to both dilution effect of non-combustible gases and barrier effect of compact char.

Carbon quantum dots @ Pd-SnS2 nanocomposite: The role of CQDs @ Pd nanoclusters in enhancing photocatalytic reduction of aromatic nitro compounds

2D layered SnS2 is one of the most popular semiconductor photocatalysts. However, its performance on photocatalytic reduction of aromatic nitro compounds is unsatisfactory, due to charge carrier recombination and weak adsorption of active hydrogen from the hydrolysis of NaBH4. Herein, we have prepared CQDs @ Pd nanoclusters with Pd nanoparticles below 5 nm through an in-situ reducing Pd(Ⅱ) with CQDs containing some oxygen-containing groups at first. CQDs @ Pd-SnS2 is achieved through a strong interaction of sulfur ions bonding on nanometric Pd surface. The composite shows a stable and efficient visible-light-driven catalytic reduction of aromatic nitro compounds in H2O and NaBH4. Under 40 min visible light irradiation, the conversion rate of 4-NP attains 99.7% on CQDs @ Pd-SnS2. The first order reaction rate constant is 0.0332 min−1, 586.5, 202.4 and 31.9 times that on SnS2, CQDs-SnS2 and Pd-SnS2 in the condition of 20 mg·L−1 4-NP and excess NaBH4, respectively. The significant enhancement is ascribed to CQDs @ Pd promoting the charge carrier separation on SnS2 and increasing the adsorption of active hydrogen from the hydrolysis of NaBH4.

Synthesis, crystal structure and magnetic properties of the new Cu(II)/Mn(II) coordination polymer [{Cu(cyclam)MnCl3(H2O)2}Cl

The synthesis, characterization and crystal structures of the copper complex [Cu(cyclam)Cl2]·H2O (1) and bimetallic compound [{Cu(cyclam)MnCl3(H2O)2}Cl]n (2), where cyclam = 1,4,8,11-tetraazacyclotetradecane, are reported. The crystal structure of 1 consists of complexes where Cu(II) is hexacoordinated and has elongated tetragonal-bipyramidal coordination, axial positions are occupied by the oxygen atoms from coordinated water molecules and the basal ones by the nitrogen atoms from the macrocyclic ligand. The reaction of 1 with manganese(II) chloride gives compound 2 with an ionic structure consisting of polymeric cation where Mn(II) and Cu(II) ions are bridged by chlorido ligands. Both central atoms are hexacoordinated and have distorted octahedral coordination environment. In the crystal structure, the formation of two types of chains is observed, one of them contains Cu(II) and Mn(II) ions arranged in alternating manner and perpendicular to them another type of chains consisting of chlorido-bridged Mn(II) atoms is formed. The magnetic properties are characterized by the dominant antiferromagnetic interaction forming Mn(II) chains along c-axis with JMn/kB = −3.38 K. A long-range magnetic order is formed at 4.23 K in zero magnetic field through the interaction with the Cu(II) subsystem. The analysis of the Arrott plots and critical exponent n describing the field dependence of the entropy change during adiabatic magnetization of the system revealed that the application of a weak magnetic field changes the order of the phase transition from second to the first order.

Synthesis, characterization and cytotoxic activity of tioconazole coordination compounds with nickel(II), palladium(II) and platinum(II)

Coordination compounds of nickel(II), palladium(II) and platinum(II) with tioconazole (tcnz) were synthesized and characterized by infrared, UV-Vis-NIR, elemental analysis, molar conductivity, magnetic susceptibility, mass spectrometry, NMR spectroscopy and X- ray diffraction. Tioconazole presented a monodentate coordination mode, through the nitrogen atom of the imidazolic ring. The NiII compounds stabilized an octahedral geometry. In [Ni(tcnz)2(NO3)2].H2O the coordinated nitrate presented a bidentate coordination mode, while for the [Ni(tcnz)2(OAc)2].3H2O compound, the acetate behaves as a bridging ligand. When different molar ratios were used on the reaction synthesis, three or six ligands were coordinate to the nickel(II) atom, [Ni(tcnz)3Br2(H2O)], [Ni(tcnz)6]Cl2 and [Ni(tcnz)6]Br2. The palladium(II) and platinum(II) compounds, [Pd(tcnz)2Cl2], [Pt(tcnz)2Cl2].2H2O and [Pd(tcnz)2(OAc)2], stabilized a trans-square planar geometry. The compounds [Ni(tcnz)6]X2 give place to 3D supramolecular arrangements through hydrogen bonding (X∙∙∙H, X = Cl and Br) and p∙∙∙p stacking interactions, between the six membered rings of neighbouring molecules. The in vitro cytotoxic activity of the synthesized compounds was studied in four different human carcinoma cell lines: HCT-15 (colon), HeLa (cervix-uterine), MCF-7 (breast) and PC-3 (prostate).

The mechanical activation as an efficient method for the improvement of perovskit technology

The effect of high-voltage mechanical energy of planetary mill on a solid hydrated product isolated by the treatment of perovskite with nitric acid has been established. The transformation includes several physicochemical steps such as dispersion of the particles, amorphization of their surface and formation of structural defects. It leads to approximately twofold increases in the specific surface area and porosity of the particles. The best result of mechanical activation was achieved at rotation speed of 650 rpm for 4-5 hours due to high hardness of rutile and anatase contained in hydrated products. The mechanical activation markedly increases the chemical activity of the hydrated product at the step of treatment with sulfuric acid of 700-900 g/l H2SO4. The kinetic curves show the reduction in time of the induction period due to increasing in the dissolution rate of the amorphous layer in the hydrated product particles. Also the extraction of TiO2 into sulfuric acid liquid phase up to 85 % and 76 % respectively, depending on the conditions (in air atmosphere or in an autoclave). At the concentration of 700 g/l H2SO4 a stable liquid system is observed without any sulphate precipitates. Increase in H2SO4 concentration up to 900 g/l markedly accelerates the extraction process. However, increased acidity reduces the stability of the system and promotes formation of TiOSO4•H2O compound in the. The obtained results can be used to improve the nitric-sulfuric acid technology of perovskite.

Hirshfeld surface analysis, vibrational spectra, optical, DFT studies and biological activities of (C7H12N2)2[SnCl6]Cl2·1.5H2O compound

Abstract The (C7H12N2)2[SnCl6]Cl2·1.5H2O compound was characterized by X-ray powder diffraction study to confirm the crystalline nature. The Hirshfeld surface analysis was carried out to discuss the strength and role of the hydrogen bonds and other intermolecular contacts in crystal lattice. The crystal structures, vibrational frequencies, atomic charges and the related properties were also investigated by the density functional theory (DFT) method. The HOMO-LUMO energy shows high band gap energy indicative of stability of the synthesized compound. Interestingly, the synthesized product shows a higher antioxidant activity in a dose-dependent manner evaluated through different in vitro antioxidant assays and an interesting antibacterial activity.

Titanosilicate Sitinakite Compound As a Low-Potential Anode for Sodium-Ion Battery

Sodium-ion batteries (SIBs) have been considered as a promising candidate for large-scale energy storage applications, because of the low cost of sodium element and a broad choice of cathode materials which do not contain the expensive raw materials. However, a lack of promising anode materials still hinders the development of SIBs technology. Herein, we for the first time report a one dimensional tunnel-structure titanosilicate sitinakite compound with an ideal formula of Na1.68H0.32Ti2O3SiO4·1.76H2O employed as a new type anode material in SIBs. This material can deliver a reversible capacity of 110 mAh g-1 at a current density of 20 mA g-1 and with an average working voltage of 0.4 V vs. Na+/Na. The structure changes of this material during discharge/charge processes were investigated by using in-situ laboratory X-ray diffraction. The results indicated that sodium insertion proceeds via a topotactic intercalation pathway. We also identified pre-dehydration as an effective avenue to further improve the capacity of Na1.68H0.32Ti2O3SiO4·1.76H2O anode (reversible capacity of 131 mAh g-1 at a current density of 20 mA g-1 after pre-dehydration process). In addition, cation Nb doped Na1.68H0.32Ti2O3SiO4·1.76H2O compounds have been synthesized and systematically investigated the electrochemical performances in SIBs. Reference [1] Liu, Y.; Xia, Y., Na1.68H0.32Ti2O3SiO4·1.76H2O as a Low-Potential Anode Material for Sodium-Ion Battery. ACS Applied Energy Materials 2018, doi:10.1021/acsaem.8b01412.

Cocrystallization of Chiral N7,N16-bis (S-1-Phenylethyl)-1,4,10,13-Tetraoxo-7,16-Diazacyclooctadecane-7,16-Dicarboxamide with Hydrochlorides of Methyl Ethers of Leucine and Valine Enantiomers

An attempt to co-crystallize N7,N16-bis(S-1-phenylethyl)-1,4,10,13-tetraoxo-7,16-diazacyclooctadecane-7,16-dicarboxamide (1) with hydrochlorides of methyl ethers (HCMEs) of L- and D-valine and also L- and D-leucine results in separate crystallization of diazacrown-ether 1 (or its monohydrate 1·H2O) and HCMEs of respective α-amino acids. Crystal structures of D-leucine 1·H2O (1) and HCME (2) compounds, which were not described previously, are solved by single crystal X-ray diffraction.

Influence of Composition of Technogenic Materials-sourced Alumininosilicate Binder onto Structural Formation and Performance Properties of Construction Composites

Analysis of data from studies of aluminum silicate binder-based construction composites allowed giving theoretical justification and then experimentally confirming a possibility to control synthesis of new growth to obtain composites with predefined characteristics by means of using shales of incomplete clay synthesis of various genesis. Employing aluminosilicate rocks of incomplete clay synthesis, which contain thermodynamically-unstable compounds make it possible to shift from traditional raw materials to production of composite materials on the basis of natural polyfunctional raw material, thus allowing to accelerate synthesis of new growth, change its morphology, optimize microstructure of binding materials and as a result, to improve performance properties of final products. Improvement of performance properties of silicate materials and reduction of their energy content are provided by producing hydrogarnets and other CaO–Al2O3–SiO2–H2O compounds in the binding material under condition of hydrothermal treatment without additional pressure.

Thermal properties and ion mobility in the antimony(III) fluoride complexes with DL–valine (C5H12NO2)SbF4·H2O and DL–serine (C3H8NO3)Sb2F7. Crystal structure of (C5H12NO2)SbF4·H2O compound

Fluoride complexes of antimony(III) with amino acids (DL–valine and DL–serine) of the compositions (C5H12NO2)SbF4·H2O (I) and (C3H8NO3)Sb2F7 (II) have been synthesized. The crystal structure of the (C5H12NO2)SbF4·H2O compound (monoclinic syngony, Z = 4, space group P21/c) has been determined for the first time. The structure of I is composed of cations of DL-valinium ((C5H12NO2)+), complex [SbF4]nn– anions having a polymeric chain structure, and crystallization water molecules. Thermal properties and ionic mobility in fluoroantimonates I and II were studied by the DSC and NMR (1H, 19F) methods. It has been established that irreversible endo-effects on DSC curves at 351 and 385 K for the compounds I and II, respectively, are related to formation of X-ray-amorphous phases. In the complex I, ionic mobilities in fluoride and proton sublattices with frequencies above 104 Hz are absent in the studied temperature range (150–420 K), whereas the ions diffusion is observed in both sublattices of II at 320 K. The mechanisms of emergence of ions diffusion in sublattices of the compound II were suggested.