Reaction Of Sulfide Research Articles

Experimental and theoretical investigation on pre-deposited precursor as growth sites for monolayer MoS2 growth by supercritical fluid deposition

The assistance of promoters, Molybdates or alkali metal salts can regulate the nucleation site of MoS2 in chemical vapor deposition. However, the introduction of impurities inevitably reduces the MoS2 quality. Here, we present the growth of monolayer MoS2 by supercritical fluid deposition to pre-deposit Mo(CO)6 precursors as nucleation sites, replacing difficult to clean conventional promoters. Domain-limited homogeneous and heterogeneous reactions occur at nucleation sites, and through optimization of sulfurization parameters, high-quality monolayer MoS2 with about 20 μm domain size can be obtained by growing at 760 °C and 40 sccm argon for 20 min. Monolayer MoS2 coverage ranged from 2.6 % to 39.1 % by regulating dissolution mass in range of 100–400 mg, utilizing the highly soluble Mo(CO)6 in supercritical CO2. Density functional theory calculations show that decarbonylated Mo(CO)6 possesses higher sulfide reactivity. This study provides new insights into the impurity-free controlled site growth of two-dimensional materials.

An efficient catalytic method for the Suzuki reaction and oxidation of sulfides by using novel magnetic nanoparticles (SnFe2O4) as a reusable catalyst

In this study, we focused on the deposition of copper nanoparticles onto Cinchonine-functionalized SnFe2O4 magnetic nanoparticles. This environmentally friendly heterogeneous catalyst was thoroughly analyzed using a variety of techniques including SEM, EDS, TGA, TEM, VSM, XRD, ICP, XPS and FT-IR. In addition, it demonstrated outstanding performance as a catalyst for Suzuki reactions and the oxidation of sulfides in environmentally sustainable conditions. The catalyst could be effortlessly separated from the mixture and reused for up to four cycles without any decrease in its catalytic efficacy. This method provides the advantages of a simple procedure, high yields of products, convenient handling, environmentally friendly conditions, and short reaction times.

The enhanced properties of ZnCoNi-S electrode by magnetron sputtering of Au nanoparticles for high performance supercapacitors

In this work, the distinctive effect of Au nanoparticles on shape preservation and properties enhancement during the preparation of transition metal sulfides is explored for the first time. After zeolitic imidazolate framework-67 (ZIF-67) is uniformly covered on nickel foam (NF), ZnCo layered double hydroxides (ZnCo-LDH) are compounded with ZIF-67 via hydrothermal method. The surface of compound is then coated with Au by magnetron sputtering. The final electrode is produced through sulfidation reaction. Benefiting from the excellent inertness and electrical conductivity of Au, the flake structure remains stable during the following sulfidation, and transfer impedance of the obtained Au/ZnS@Co3S4@Ni3S2 (Au/ZCN-S) electrode decreases significantly. In contrast, magnetron sputtered Ag or Cu nanoparticles react to Ag2S or CuS2 and cannot protect the refined structure of electrode as Au does. The Au/ZCN-S electrode shows a low transfer impedance of 0.0785 Ω and enables a specific capacity of 302.6 mAh g−1. Furthermore, the asymmetric supercapacitor constructed by Au/ZCN-S and activated carbon (AC) achieves a remarkable energy density of 104.09 Wh kg−1 with a high capacitance retention rate of 91.184 % after 10000 cycles. This work provides a new approach to optimize the morphology and performance of transition metal sulfides electrode for supercapacitors.

Evaluating the efficacy of biogeochemical cover system in mitigating landfill gas emissions: A large-scale laboratory simulation.

Municipal solid waste (MSW) landfills are a significant source of methane (CH4) emissions in the United States, contributing to global warming. Current landfill gas (LFG) management methods, like the landfill cover system and LFG collection system, do not entirely prevent LFG release. Biocovers have the potential to reduce CH4 emissions through microbial oxidation. However, LFG also contains carbon dioxide (CO2) and trace hydrogen sulfide (H2S) depending on waste composition, temperature, moisture content, and age of waste. An innovative biogeochemical cover (BGCC) was developed to tackle these concerns. This cover comprises a biochar-based biocover layer overlaid with a basic oxygen furnace (BOF) steel slag layer. The biochar-based biocover layer oxidizes CH4 emissions, while the BOF slag layer reduces CO2 and H2S through carbonation and sulfidation reaction mechanisms. The BGCC system's field performance remains unexamined. Therefore, a large-scale tank setup simulating near-field conditions was developed to evaluate the BGCC system's ability to mitigate CH4, CO2, and H2S from LFG simultaneously. Synthetic LFG was passed through the BGCC in five distinct phases, each designed to simulate the varying gas compositions and flux rates typical of MSW landfill. Gas profiles along the depth were monitored during each phase, and gas removal efficiency was measured. After testing, biocover and BOF slag samples were extracted to analyze physico-chemical properties. Batch tests were also conducted on samples extracted from the biocover and BOF slag layers to determine potential CH4 oxidation rates and residual CO2 sequestration capacity. The results showed that the BGCC system's CH4 removal efficiency decreased with higher CH4 flux rates, achieving its highest removal (74.7-79.7%) at moderate influx rates (23.9-25.5g CH4/m2-day) and reducing to its lowest removal (27.4%) at the highest influx rate (57.5g CH4/m2-day). Complete H2S removal occurred during Phase 3 in the biocover layer of BGCC system. CH4 oxidation rates were highest near the upper (277.9µg CH4/g-day) and lowest in the deeper region of the biocover layer. In the tank experiment, CO2 breakthrough occurred after 156days due to drying of the BOF slag layer, with an average residual carbonation capacity of 46 gCO2/kg slag after moisture adjustment. Overall, the BGCC system effectively mitigated LFG emissions, including CH4, CO2, and H2S, at moderate flux rates, showing promise as a comprehensive solution for LFG management.

Al2O3-MnS Inclusions and Pitting Corrosion in the Weld Heat-Affected Zone

Manganese sulfide inclusions have been identified as a key factor contributing to the degradation of pitting corrosion resistance in both carbon and stainless steels. However, the precise reasons behind the differential reactivity of various sulfides, with some serving as active sites for pitting while others remain inactive, are not yet fully understood. The effect of debonding occurring at the interface between these inclusions and the steel matrix in relation to pitting corrosion has not been extensively investigated. In this study, an examination of a service-exposed pipeline girth weld was conducted. Immersion testing in blowdown water and multiscale characterization techniques investigated the inclusion-matrix interface debonding within the heat-affected zone. Our findings suggest that interfacial debonding is more likely at the Al2O3- MnS cluster interface. This observation offers a rationale for the selective reactivity of sulfides that form clusters with oxides, highlighting the likelihood that only sulfides clustering with oxides act as active pitting initiation sites.

Pt nanoclusters confined in the pores of hollow carbon spheres boost adsorption and electrochemical redox reaction for lithium-sulfur batteries

Sulfur (S) cathode is considered an ideal energy storage material for secondary batteries due to the high specific capacity and energy density. However, the insulating nature of S and lithium sulfide and slow electrochemical reaction kinetics, among many other issues, limit its power and energy output. Precious metals are vigorous catalytic materials and have been applied in various fields. However, the investigation of small-sized precious metal nanoclusters as the catalytic for polysulfide conversion in lithium-sulfur (Li-S) batteries has yet to be deepened. Herein, small-sized Pt nanoclusters are successfully synthesized and confined in the pores of hollow carbon spheres as the host for Li-S batteries cathode. The resultant PtNC@HCS provides the space for storing S and the electron transport network. Meanwhile, the Pt nanoclusters in the pores serve as catalytic sites for adsorbing and accelerating polysulfide conversion, thus effectively suppressing the shuttle effect. As a result, PtNC@HCS exhibits an initial capacity of 1460 mAh g−1 and a reversible capacity of 1316 mAh g−1 at 0.2C, with outstanding capacity retention, which confirms that such precious metal nanocluster catalytic material design effectively can optimize the electrochemical performance of Li-S batteries.

Atmospheric Influences on Li6PS5Cl Separators and the Resulting Ionic Conductivity for All-Solid-State Batteries

All-solid-state batteries (ASSBs), defined through a solid electrolyte, are emerging as a promising solution to address current challenges in energy and power density demands for electromobility. Within the various possible types of solid electrolytes, sulfide-based materials exhibit advantageous high ionic conductivities. However, due to the strong reactivity of sulfides, atmospheric exposure can lead to the formation of toxic hydrogen sulfide and additionally negatively impact the resulting battery performance. Both factors present key challenges for ASSB production, as they necessitate the development of a material-adapted, economically viable and safe process atmosphere. In the present study, the influence of different production atmospheres on sulfide-based solid electrolytes is experimentally investigated. For this purpose, sulfide sheets are exposed to defined atmospheres with dynamic air fluctuations at dew points ranging from −60 °C to 0 °C. The resulting ionic conductivities indicate a dependency on the prevailing dew point and exposure time with a discernible impact on performance even at dew points of −60 °C within atmospheres with constant air circulation. With the acquired results, a detailed and knowledge-based selection and design of dry room production atmospheres for ASSB cell assembly is possible, which is a necessary step for further industrialization.

Enhanced Triethylamine Detection at Room Temperature Using a Layered MoS2 Nanosheet-Coated PPy Nanorod: A Comprehensive Study.

The rapid and reliable detection of triethylamine (TEA), a toxic, explosive, volatile organic compound at room temperature, is highly significant for food safety, environmental, and human health monitoring. This manuscript reports a layered molybdenum disulfide (MoS2) nanosheet-coated polypyrrole (PPy) nanorod-based heterostructure sensor (MsPy) which offers superior sensing properties toward TEA at room temperature (25 °C). Herein, different MsPy nanocomposites were synthesized, followed by a controlled sulfidation reaction through dissolution, diffusion, and regrowth mechanisms. Optimizing the ratio of the precursor of molybdenum trioxide (MoO3/PPy) is crucial for achieving effective deposition of a layered MoS2 nanosheet on the PPy surface. The as-prepared MoS2 nanosheet-coated PPy sensor (MsPy_40) enables one to selectively detect trace TEA vapor at 25 °C with a detection lower limit of 0.5 ppm. The MsPy_40 sensor exhibits 17 times higher response than the pristine MoS2 nanosheet to 50 ppm TEA, with rapid response (∼3.9 s) and recovery (∼19.6 s), along with better stability, good selectivity, and remarkable repeatability. The significantly enhanced sensing performance is attributed to the unique surface morphology of the layered MoS2 nanosheet-coated PPy nanorod and the formation of a p-n heterojunction between PPy and MoS2.

SUPPORTED COBALT OXIDE NANOPARTICLES: THE INFLUENCE OF MESOPOROUS MATERIALS AND THEIR ROLE IMETHYL PHENYL SULFIDE OXIDATION REACTIONS.

The effect of the support in the incorporation of cobalt oxide nanoparticles on mesoporous materials (SBA‐15) and mesoporous cellular foam (MCF) was investigated. The materials were characterized using various techniques. The XRD diffraction patterns showed that the porous structures remained after cobalt incorporation, while high‐angle XRD of the MCF showed CoO peaks, in contrast to Co‐SBA‐15 which exhibited Co3O4. This was confirmed by XPS technique. The SEM‐EDS and HRTEM‐STEM microscopy indicate a distribution of cobalt oxides uniform in the samples synthesized and the average size of the particles is 1.88 nm. H2‐TPR analysis highlighted the interaction between the support surfaces and the metal oxide (SMSI). It was observed that in the SBA‐15 structure, small clusters of cobalt oxide formed with a strong interaction with silica, leading to high reduction temperatures. The catalysts activity was characterized in oxidation reactions of Methyl Phenyl Sulfide and a correlation was observed between the characterization results and the enhanced selectivity and yield towards sulfone exhibited by Co‐MCF.

Spectroscopic Characterization and Photochemistry of the Atmospherically Relevant Methanesulfenic Acid.

Methanesulfenic acid, CH3SOH, is a fleeting intermediate in the ·OH-initiated oxidation reactions of dimethyl sulfide (DMS) and dimethyl disulfide (DMDS) in the atmosphere. Herein, we report the characterization and photochemistry of CH3SOH in Ar- and N2-matrices at 10 K. The characterization of CH3SOH with matrix-isolation IR and UV-vis spectroscopy is supported by D and 13C isotope labeling experiments and quantum chemical calculations. In line with the observed absorption at 260 nm for CH3SOH, its photolysis at 254 nm leads to dissociation by yielding the novel water complex H2CS···H2O, which exhibits a five-membered ring structure with intermolecular S···HO and CH···O hydrogen bonding interactions. Upon further irradiation at 193 nm, the H2CS···H2O complex undergoes dehydrogenation to form CS···H2O, which can further convert to HC(O)SH under irradiation at 254 nm. When the photolysis of CH3SOH was performed in an O2-doped Ar-matrix, methanesulfonic acid (MSA, CH3SO3H) was obtained as the oxidation product.

Heterogeneous Reaction of Dimethyl Sulfide with a Chlorine Atom

Heterogeneous Reaction of Dimethyl Sulfide with a Chlorine Atom

Selective separation and recovery of valuable metals through directional vulcanization of black copper sludge

The recovery of copper (Cu) from secondary sources has emerged as a promising trend in the copper industry’s advancement. Black copper sludge (BCS), a valuable hazardous waste produced during Cu electrolytic refining, contains various precious metals, including Cu3As. This study investigates theoretical and experimental aspects using BCS as a raw material to mitigate solid waste emissions and retrieve valuable metals. The proposed method for separating Cu from As through directional sulfidation offers an environmentally friendly solution. Gibbs free energies of the sulfidation reaction between BCS and S were calculated using HSC Chemistry 9.0, with experimental validation confirming the method’s feasibility. The study explores the effects of vulcanization temperature, holding time, and S content during the vulcanization reaction. Under optimal conditions of 873 K temperature, 60 min holding time, and 20 % excess S, Cu existed as Cu2S in the sulfide residue, while As2O3 was observed as a condensate. Cu and As recovery rates were 98.38 % and 84.62 % respectively, with a 99.98 % removal efficiency for Cu volatiles and 94.36 % for As residue. This method effectively separates Cu and As from solid wastes containing As, offering a simpler and more environmentally friendly alternative to traditional pyrometallurgical and hydrometallurgical methods. The study presents a novel, eco-friendly, and highly efficient approach for the safe disposal of As-containing solid waste.

Separation of V(Ⅴ) and Cr(Ⅵ) from vanadium-containing solutions based on E-pH diagrams of V-Cr-S-H2O system

The extremely similar physicochemical properties of vanadium and chromium lead to the difficulty in separating from each other. In this study, a novel hydrometallurgical process was devised to selectively precipitate chromium from vanadium-containing solutions, facilitating the efficient separation of V(V) and Cr(VI) while enabling the recovery of both vanadium and chromium species. The speciation of vanadium and chromium in solutions was investigated through the construction of E-pH diagrams for V-Cr-S-H2O system at 298 K, 363 K, and 453 K. The results revealed that under conditions of pH approximately 12 and temperature 363 K, the reduction potential of SO42-/S2- was found to lie between that of CrO42-/Cr(OH)3 and VO43-/V2O3. This suggests that selective reduction of Cr(VI) could be achieved using S2- as reducing agent. In order to validate the theoretical findings, single-factor experiments were conducted on a laboratory scale. The effects of various parameters including initial pH, sodium sulfide dosage, reaction time, temperature, and initial concentration of vanadium-containing solutions on the chromium precipitation ratio and vanadium loss ratio were investigated. The experimental outcomes showed that the chromium precipitation ratio reached 99.8 % while the vanadium loss rate was only 3.5 % when the experiment was conducted at the optimal conditions: the initial pH was set to 12, sodium sulfide dosage was 2.0 times of the theoretical dosage, reaction time was 60 min and the temperature was 363 K. Then, the chromium concentration in the solution decreased from 2407 mg/L to 3.3 mg/L. Ultimately, V2O5 with a purity of 99.0 % and Cr2O3 with a purity of 97.2 % were successfully obtained.

Enhanced interfacial polarization through the conversion of Co@C into Co@Co1−xS@C nanocapsules utilizing a facile sulfidation process

The design and development of efficient Co-based electromagnetic (EM) absorbents with double-shell structures have received relatively less attention in the literature. The construction of multiple heterointerfaces gives rise to a unique morphology that holds significant potential in expanding the absorbing frequency range. Co@Co1−xS@C nanocapsules (NCs) with Co as the cores, Co1−xSx and C as the middle and outside shells separately, were successfully prepared using a facile two step process: synthesizing Co@C core–shell NCs by arc-discharge method and subsequently converting them into Co@Co1−xS@C NCs through chemical sulfidation reaction. The experimental results indicate that the thickness of the carbon shell exhibits a decreasing trend (from 1 ± 0.1 nm to 0.6 ± 0.02 nm) following the post-sulfidation process, lasting for approximately two hours. The defect density of the carbon shell also declines from 1.88 × 1011 cm−2 to 1.14 × 1011 cm−2. The reduction in thickness of the carbon shell and the formation of new Co1-xS not only enable efficient manipulation of impedance matching between the dielectric shells and magnetic cores but also facilitate the construction of multiple interfacial polarizations. The study provides evidence that the multi-interfacial Co@Co1−xS@C nanocomposite serves as an effective EM absorbent achieving a minimum reflection loss (RL) up to –78.6 dB at a thickness of merely 1.52 mm within the frequency range of 2~18 GHz.

Engineering Detrimental Functional Groups in Conductive Additives Toward High-Performance All-Solid-State Batteries.

Conductive additives are of great importance for the adequate utilization of active materials in all-solid-state lithium batteries by establishing conductive networks in the composite cathode. However, it usually causes severe interfacial side reactions with solid electrolytes, especially sulfide electrolytes, leading to sluggish ion transportation and accelerated performance degradation. Herein, a simple hydrogen thermal reduction process is proposed on a commonly used conductive additive Super P, which effectively removes the surface oxygen functional groups and weakens the interfacial side reactions with sulfide. With a small amount of 1 wt % reduced Super P, ASSLBs demonstrates a competitive capacity of 180.2 mAh g-1 , which is much higher than the 130.8 mAh g-1 of untreated Super P. Impressively, reduced Super P based ASSLBs also exhibit a higher capacity retention of 81.8 % than 64.6 % of untreated Super P. The cathode interfacial chemical evolutions reveal that reduced Super P could effectively alleviate the side reactions of sulfide. Reduced Super P shows better reversible capacity compared to reduced carbon nanofiber with almost no loss of capacity retention, due to its more complete conductive network. Our results highlight the importance of oxygen-containing functional groups for conductive additives, lightening the prospect of low-cost 0D conductive additives for practical ASSLBs.

Metabolomics reveals factors affecting the radical reaction of sulfides during thermal processing for meaty aroma

The effects of cysteine (Cys), glutathione (GSH) and cystine (GCys) on sulfides and meaty aroma were studied based on concentration monitoring and metabolomics. In multi-component models, Cys and GSH demonstrated a greater capacity to decrease dimethyl trisulfide (DMTS) levels and increase the proportion of 2-methyl-3-furanthiol (MFT), compared with GCys. Moreover, no discernible difference between Cys and GSH in dynamic profiles of volatiles to further analyze the synergistic effect of both. Results of single factor experiment and optimization revealed that the optimal thermal processing was a second-order thermal procedure. Aroma profiles revealed that the addition of Cys and GSH mixture increased the meaty intensity during the optimal thermal processing. Metabolomics based on Encyclopedia of Genes and Genomes pathway annotation confirmed that Cys and GSH significantly affected the degradation of methionine and thiamine in amino acid and protein metabolic pathways, resulting in various amounts of DMTS and MFT. Research on effect and potentially metabolic mechanisms revealed that the combination of Cys and GSH at ratio of 3:7 had higher and more effective control capacity for free radical reaction of sulfides than either one alone during second-order thermal processing, which would lay theoretical foundation for the development of high-quality thermal process products.

The sulfidation behavior of zinc during microwave hydrothermal sulfidation of heavy metal-containing sludge

ABSTRACT The heavy metals present in the sludge can undergo a reaction with sulfur, leading to their conversion into metal sulfides through hydrothermal sulfidation. Sulfur ions, possessing a strong sulfidation capability, can operate within a wider pH range at elevated temperatures. The high temperature environment promotes the sulfidation process of zinc within heavy metal-laden sludge. Increasing the temperature of microwave hydrothermal sulfidation and extending the sulfidation duration for heavy metal-containing sludge can enhance the growth of crystal size in the artificially synthesized zinc sulfide. Zinc sulfide predominantly takes the form of ZnS, which facilitates the subsequent flotation recovery of zinc.

Geochemical transformations of sulfur and their role in the formation of different types and subtypes of saline lakes in Southeastern Transbaikalia

This study focused on the chemistry and isotopes of sulfur in lakes. The bottom sediments and water columns of lakes were found to contain reduced forms of sulfur, including hydrogen sulfide ions, elemental sulfur, and thiosulfate ions, along with sulfate ions. It was determined that elemental sulfur in lakes is present mainly in the form of suspensions and colloids, and the proportion of elemental sulfur in polysulfides increases with increasing water pH. It was shown that sulfate reduction results in the greatest isotope fractionation, with a light sulfur isotope accumulating in hydrogen sulfide ions and a heavy sulfur isotope accumulating in sulfate ions. It was confirmed that the abiotic reaction of hydrogen sulfide with oxygen yields a mixture of products that are depleted in 34S and enriched in 34S in hydrogen sulfide. In contrast, the microbial oxidation of HS− → S0 yields zerovalent sulfur, which is 2–4‰ heavier than the initial product. It was shown that the loss of sulfate ions due to bacterial reduction is most significant in subtype-I and subtype-III chloride and soda lakes. In contrast, in subtype-II sulfate and soda lakes, an increase in sulfate ions was noted due to the oxidation of hydrogen sulfides in water-bearing rocks and bacterial hydrogen sulfide. This finding indicated that in addition to evaporation, the formation of a particular type and subtype of saline lake involves the processes of aluminosilicate hydrolysis, sulfate reduction and hydrogen sulfide oxidation.

Ultralong Nanowires of Cadmium Phosphate Hydroxide Synthesized Using a Cadmium Oleate Precursor Hydrothermal Method and Sulfidation Conversion to Ultralong CdS Nanowires.

Ultralong nanowires with ultrahigh aspect ratios exhibit high flexibility, and they are promising for applications in various fields. Herein, a cadmium oleate precursor hydrothermal method is developed for the synthesis of ultralong nanowires of cadmium phosphate hydroxide. In this method, water-soluble cadmium salt is used as the cadmium source, water-soluble phosphate is used as the phosphorus source, and sodium oleate is adopted as a reactant to form cadmium oleate precursor and as a structure-directing agent. By using this method, ultralong nanowires of cadmium phosphate hydroxide are successfully synthesized using CdCl2, sodium oleate, and NaH2PO4 as reactants in an aqueous solution by hydrothermal treatment at 180 °C for 24 h. In addition, a new type of flexible fire-resistant inorganic paper with good electrical insulation performance is fabricated using ultralong nanowires of cadmium phosphate hydroxide. As an example of the extended application of this synthetic method, ultralong nanowires of cadmium phosphate hydroxide can be converted to ultralong CdS nanowires through a convenient sulfidation reaction. In this way, ultralong CdS nanowires are successfully synthesized by simple sulfidation of ultralong nanowires of cadmium phosphate hydroxide under mild conditions. The as-prepared ultralong nanowires of cadmium phosphate hydroxide are promising for applications as the precursors and templates for synthesizing other inorganic ultralong nanowires and have wide applications in various fields.

Синтез и исследование структуры иодсодержащих имидазо[2,1 b][1,3]тиазиниевых систем

Heterocyclization of S-alkenyl derivatives of 1-methylimidazole-2-thiol (1-methyl-2-prenyl-sulfanylimidazole (1), 1-methyl-2-cinnamylsulfanylimidazole (4), and 2-(3-butenyl)sulfanyl-1-methyl-imidazole (7)) has been studied for the first time under the action of iodine (iodocyclization) in various solvents (chloroform, dichloro-methane, glacial acetic acid), and at different substrate and iodine ratios (1 : 1, 1 : 2). It has been found that the interaction of compounds 1, 4, 7 with iodine proceeds regioselectively, regardless of the reaction conditions, and it is accompanied by the linear annelation of the thiazinium ring and formation of a bicyclic fused heterocyclic system. As a result, new iodine-containing imidazo[2,1 b][1,3]thiazinium systems have been synthesized – 6-iodo-1,5,5-trimethyl-6,7-dihydro-5H-imidazo[2,1-b][1,3]hiazinium polyiodide / iodide (2, 3), 6-iodo-1-methyl-5-phenyl-6,7-dihydro-5H-imidazo[2,1-b][1,3]thiazinium triiodide / iodide (5, 6), and 6-iodomethyl-1-methyl-6,7-dihydro-5H-imidazo[2,1-b][1,3]thiazinium iodide (9). The structure of the synthesized compounds has been studied and proved by 1H and 13C NMR spectroscopy. The evidence for heterocyclization reactions of alkenyl sulfides 1, 4, and 7 is the absence of signals for the alkenyl protons and the presence of a more complex splitting pattern of signals for the thiazinium ring protons in the 1H NMR spectra of heterocyclization products. The structures of polyiodide 2 and triiodide 5 have been unambiguously established and characterized by X-ray diffraction analysis. According to the X-ray analysis data, the cell of polyiodide 2 contains two heterocyclic cations, a triiodide anion, and an iodide anion. In the triiodide crystal 5 heterocyclic cations correspond to two types of crystallographically independent triiodide anions: one cell contains eight molecules of a heterocyclic cation and eight triiodide anions. The structural organization in the crystals is due to short contacts between atoms: I(4)∙∙∙H(3) (2.95 Å), I(4)∙∙∙I(1) (3.57 Å), H(8a)∙∙∙I(2) (3.13 Å) (in crystal 2), I(2)∙∙∙I(4) (3.95 Å), I(5)∙∙∙H(5) (3.14 Å), I(4)∙∙∙H(7a) (3.12 Å), I(4)∙∙∙H(7b) (3.17 Å) (in crystal 5).