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In photocatalytic removal of organic pollutants, adsorption and degradation are two important processes that take place. Various instrumental techniques and trapping experiments have been used to identify the reactive species and the mechanism of photodegradation. The present work focuses on investigating the mechanism of photo-induced degradation from the comparative characterization of fresh and used samples, isotherm models, competitive adsorption, and desorption studies of pure and Ag+-modified TiO2 NPs. The comparative characterizations of fresh and used NPs were carried out with FT-IR, EDX, and XRF analyses after methylene blue (MB) degradation. The Ag+ doped TiO2 used in this study was fabricated using simple impregnation technique. The prepared NPs were characterized using techniques including XPS, XRD, SEM/EDX, XRF, UV-DRS, and pH point-zero charge analyses (pHPZC). The Ag+-modified TiO2 NPs showed improved efficiency compared to pure TiO2 NPs using normal compact fluorescent light (CFL). The Langmuir and Freundlich isotherm models were applied to test the adsorption behavior on the surface photocatalysts. The investigational data finest fitted to the Langmuir isotherms model compared to Freundlich model, suggesting the homogeneous monolayer adsorption followed by degradations. The competitive removal of MB in the presence of a photo-generated electrons trapper (Cd2+) was enhanced almost 3-folds (115 mg/L) compared to the removal from a single MB solution (40 mg/L). The characterization of the used samples as well as adsorption in the dark and negligible desorption of used samples support the involvement of the proposed photo-induced degradation mechanism.
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Viruses have spread throughout the world and cause acute illness or death among millions of people. There is a growing concern about methods to control and combat early-stage viral infections to prevent the significant public health problem. However, conventional detection methods like polymerase chain reaction (PCR) requires sample purification and are time-consuming for further clinical diagnosis. Hence, establishing a portable device for rapid detection with enhanced sensitivity and selectivity for the specific virus to prevent further spread becomes an urgent need. Many research groups are focusing on the potential of the electrochemical sensor to become a key for developing point-of-care (POC) technologies for clinical analysis because it can solve most of the limitations of conventional diagnostic methods. Herein, this review discusses the current development of electrochemical sensors for the detection of respiratory virus infections and flaviviruses over the past 10 years. Trends in future perspectives in rapid clinical detection sensors on viruses are also discussed. KEY POINTS: ⢠Respiratory related viruses and Flavivirus are being concerned for past decades. ⢠Important to differentiate the cross-reactivity between the virus in same family. ⢠Electrochemical biosensor as a suitable device to detect viruses with high performance.
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Técnicas Biossensoriais , Flavivirus , Vírus , HumanosRESUMO
This study aimed to work out a simple and high-yield procedure for the immobilization of horseradish peroxidase on silver nanoparticle. Ultraviolet-visible (UV-vis) and Fourier-transform infrared spectroscopy and transmission electron microscopy were used to characterize silver nanoparticles. Horseradish peroxidase was immobilized on ß-cyclodextrin-capped silver nanoparticles via glutaraldehyde cross-linking. Single-cell gel electrophoresis (Comet assay) was also performed to confirm the genotoxicity of silver nanoparticles. To decrease toxicity, silver nanoparticles were capped with ß-cyclodextrin. A comparative stability study of soluble and immobilized enzyme preparations was investigated against pH, temperature, and chaotropic agent, urea. The results showed that the cross-linked peroxidase was significantly more stable as compared to the soluble counterpart. The immobilized enzyme exhibited stable enzyme activities after repeated uses.
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Técnicas Biossensoriais , Enzimas Imobilizadas/metabolismo , Peroxidase do Rábano Silvestre/metabolismo , Nanopartículas Metálicas/química , Prata/química , beta-Ciclodextrinas/química , Dano ao DNA , Concentração de Íons de Hidrogênio , Microscopia Eletrônica de TransmissãoRESUMO
Horizontal subsurface-flow (HSF) constructed wetland incorporating baffles was developed to facilitate upflow and downflow conditions so that the treatment of pollutants could be achieved under multiple aerobic, anoxic and anaerobic conditions sequentially in the same wetland bed. The performances of the baffled and conventional HSF constructed wetlands, planted and unplanted, in the removal of azo dye Acid Orange 7 (AO7) were compared at the hydraulic retention times (HRT) of 5, 3 and 2 days when treating domestic wastewater spiked with AO7 concentration of 300 mg/L. The planted baffled unit was found to achieve 100%, 83% and 69% AO7 removal against 73%, 46% and 30% for the conventional unit at HRT of 5, 3 and 2 days, respectively. Longer flow path provided by baffled wetland units allowed more contact of the wastewater with the rhizomes, microbes and micro-aerobic zones resulting in relatively higher oxidation reduction potential (ORP) and enhanced performance as kinetic studies revealed faster AO7 biodegradation rate under aerobic condition. In addition, complete mineralization of AO7 was achieved in planted baffled wetland unit due to the availability of a combination of aerobic, anoxic and anaerobic conditions.
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Compostos Azo/isolamento & purificação , Benzenossulfonatos/isolamento & purificação , Poluentes Químicos da Água/isolamento & purificação , Purificação da Água/métodos , Áreas Alagadas , Aerobiose , Anaerobiose , Compostos Azo/análise , Benzenossulfonatos/análise , Biodegradação Ambiental , Corantes/análise , Corantes/isolamento & purificação , Cinética , Fatores de Tempo , Águas Residuárias/química , Poluentes Químicos da Água/análiseRESUMO
Herein, cellulose nanocrystals were synthesized from oil palm fronds (CNC-OPF) involving two pretreatment approaches, viz. autohydrolysis and soda pulping. The pretreatments were applied individually to OPF fibers to assess their influence on CNCs' physicochemical and thermal properties. CNC-OPF samples were assessed using complementary characterization techniques, which confirmed their purity and characteristics. CP/MAS 13C NMR and TEM studies revealed that autohydrolysis pretreatment yielded CNCs with effective hemicellulose and extractives removal compared to that of soda pulping. XRD analysis demonstrated that autohydrolysis-treated CNC-OPF contained a much higher crystallinity index compared to soda pulping treatment. BET measurement disclosed a relatively higher surface area and wider pore diameter of autohydrolysis-treated CNC-OPF. Autohydrolysis-treated CNCs were applied as a reinforcement filler in alginate-based hydrogel beads for the removal of 4-chlorophenol from water, which attained a qmax of 19.168 mg g-1. BET analysis revealed the less porous nature of CNC-ALG hydrogel beads which could have contributed to hydrogel beads' relatively lower adsorption capacity. The point of zero charge of CNC-ALG hydrogel beads was 4.82, suggesting their applicability only within a short solution pH range. This study directs future studies to unveil the possibilities of functionalizing CNCs in order to enhance the adsorption performance of CNC-immobilized hydrogel beads towards 4-chlorophenol and other organic contaminants.
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Clorofenóis , Nanopartículas , Celulose/química , Hidrogéis/química , Nanopartículas/químicaRESUMO
Calcium oxide (CaO) nanoparticles are known to exhibit unique property due to their high adsorption capacity and good catalytic activity. In this work the CaO nanocatalysts were prepared by hydrothermal method using anionic surfactant, sodium dodecyl sulphate (SDS), as a templating agent. The as-synthesized nanocatalysts were further used as substrate for the synthesis of alumina doped calcium oxide (Al2O3·CaO) nanocatalysts via deposition-precipitation method at the isoelectric point of CaO. The Al2O3·CaO nanocatalysts were characterized by FTIR, XRD, TGA, TEM, and FESEM techniques. The catalytic efficiencies of these nanocatalysts were studied for the photodegradation of 2,4,6-trinitrophenol (2,4,6-TNP), which is an industrial pollutant, spectrophotometrically. The effect of surfactant and temperature on size of nanocatalysts was also studied. The smallest particle size and highest percentage of degradation were observed at critical micelle concentration of the surfactant. The direct optical band gap of the Al2O3·CaO nanocatalyst was found as 3.3 eV.
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Óxido de Alumínio/química , Compostos de Cálcio/química , Óxidos/química , Picratos/química , Picratos/isolamento & purificação , Poluentes Químicos da Água/química , Poluentes Químicos da Água/isolamento & purificação , Purificação da Água/métodos , Adsorção/efeitos da radiação , Óxido de Alumínio/efeitos da radiação , Compostos de Cálcio/efeitos da radiação , Catálise , Luz , Micelas , Óxidos/efeitos da radiação , Picratos/efeitos da radiação , Dodecilsulfato de Sódio/química , Dodecilsulfato de Sódio/efeitos da radiação , Água/química , Poluentes Químicos da Água/efeitos da radiaçãoRESUMO
The purpose of this research is to synthesize environmentally friendly nanosorbents for the novel adsorption of diesel range organics (DRO) from contaminated water. Central composite design (CCD) analysis of response surface methodology (RSM) was employed in a model fitting of the variables predicting the adsorption efficiency of Moringa oleifera-functionalized zerovalent iron particles (ZINPs) for the removal of DRO. The effects of the reaction parameters on the response were screened using 24 factorial designs to determine the statistically significant independent variables. A quadratic model predicting the DRO adsorption efficiency of ZINPs with an F value of 276.84 (p value < 0.0001) was developed. Diagnostic plots show that the predicted values were in excellent agreement with actual experimental values (R2 = 0.99). The maximum percentage removal of DRO of 92.6% was achieved after optimization, using the synthesized ZINPs after 8 h of contact between DRO substrates and ZINPs at pH of 8, the temperature of 25 °C, with an adsorbent dosage of 2 g/L and at composite desirability of 1. Characterization of ZINPs revealed the formation of quasi nanospheres and nanocubes with an average particle diameter of 50.9 ± 9.7, a crystallite size of 15.31 nm, a crystallinity index of 32.47% and a pore width of 75.69-88.59 nm. The adsorption equilibrium data modelling of ZINPs for adsorption of DRO was best described by Langmuir isotherm with the maximum monolayer coverage capacity of 7.194 mg/g. The separation factor [Formula: see text], indicated favourable adsorption. The adsorption kinetic data were consistent with pseudo-second-order kinetics indicating probable chemisorption.
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Moringa oleifera , Poluentes Químicos da Água , Purificação da Água , Poluentes Químicos da Água/química , Temperatura , Adsorção , Cinética , Ferro , Água/química , Concentração de Íons de Hidrogênio , Purificação da Água/métodos , TermodinâmicaRESUMO
The primary aim of this study is to develop an economical, stable, and effective heterogeneous catalyst for wastewater remediation via the Fenton oxidation process. For this purpose, Fe3O4-montmorillonite alginate (FeMA) composite beads were synthesized by entrapping Fe3O4-montmorillonite in calcium alginate beads. The performance of the catalysts was evaluated via the Fenton degradation of ofloxacin (OFL), an antibiotic that is frequently detected in water bodies. The physiochemical properties of the FeMA composite beads were characterized using X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscope/energy dispersive X-ray (FESEM/EDX), Brunauer-Emmett-Teller (BET) analysis, Fourier transform infrared (FTIR) spectroscopy, and thermogravimetric analysis (TGA). FeMA composite beads were found to have a higher surface area, higher porosity, and better thermal stability compared to pristine alginate beads. The composite beads were subsequently used for Fenton degradation of ofloxacin (OFL) in an aqueous solution. The effects of Fe3O4-montmorillonite loading on alginate, FeMA composite beads dosage, initial solution pH, initial OFL concentration, different oxidants, H2O2 dosage, reaction temperature, and inorganic salts on Fenton degradation of OFL in aqueous solution was investigated. The results revealed that the percentage of OFL degradation reached about 80 % under optimized conditions, while the total organic carbon (TOC) removal reached about 53 %. The entrapment of Fe3O4-montmorillonite in alginate beads results in less iron ions leaching compared to previous observation, and the efficiency remains constant over the five cycles investigated. The kinetics of the Fenton degradation process are best fitted to the pseudo-first-order kinetic model. It is therefore believed that FeMA composite beads can be a promising material for wastewater remediation via the Fenton oxidation process.
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Antibacterianos , Ofloxacino , Antibacterianos/farmacologia , Bentonita , Peróxido de Hidrogênio/química , Águas Residuárias , Alginatos/química , CatáliseRESUMO
A structural study of epoxidized natural rubber (ENR-50) and its cyclic dithiocarbonate derivative was carried out using NMR spectroscopy techniques. The overlapping (1)H-NMR signals of ENR-50 at δ 1.56, 1.68-1.70, 2.06, 2.15-2.17 ppm were successfully assigned. In this work, the <(13)C-NMR chemical shift assignments of ENR-50 were consistent to the previously reported work. A cyclic dithiocarbonate derivative of ENR-50 was synthesized from the reaction of purified ENR-50 with carbon disulfide (CS(2)), in the presence of 4-dimethylaminopyridine (DMAP) as catalyst at reflux temperature. The cyclic dithiocarbonate formation involved the epoxide ring opening of the ENR-50. This was followed by insertion of the C-S moiety of CS(2) at the oxygen attached to the quaternary carbon and methine carbon of epoxidized isoprene unit, respectively. The bands due to the C=S and C-O were clearly observed in the FTIR spectrum while the (1)H-NMR spectrum of the derivative revealed the peak attributed to the methylene protons had split. The (13)C-NMR spectrum of the derivative further indicates two new carbon peaks arising from the >C=S and quaternary carbon of cyclic dithiocarbonate. All other (1)H- and (13)C-NMR chemical shifts of the derivative remain unchanged with respect to the ENR-50.
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Carbonatos/química , Compostos de Epóxi/química , Borracha/química , Catálise , Espectroscopia de Ressonância Magnética , Modelos MolecularesRESUMO
Ceramics-based filter for water treatment is an ancient technology to procure potable water at the household level. The traditional clay pots (vessels or hollow cylindrical container) have been used since long in the developing countries. The ceramic material (CaCu3Ti4O12 or CCTO) is a hetero-junction of titanium oxide, a well-known UV-active photocatalyst, and visible light absorbing CuO materials. This hetero-junction is able to overcome the limitations such as high bandgap, poor stability, low efficiency, and high photo-generated charge (e-/h+) recombination rate, associated with the other commonly used metal oxide semiconductor photocatalysts. Moreover, the low-cost, viable and facile synthesis routes for CCTO triggered its potential applications in photoelectrochemical and photocatalytic processes. This review will elaborate on the available literature demonstrating the visible light activity of CCTO photocatalysts in water treatment technologies. Furthermore, the mechanism of photocatalysis and synthesis routes are presented in this work for broader impact of the CCTO potential applications. The extended porous character and excellent surface texture have made the ceramic materials as an ideal choice to combat the bacteria, pathogens and turbidity in aqueous medium at household level. Specifically, the controlled size and shape make the CaCu3Ti4O12 (CCTO) an excellent visible light-driven photocatalyst, involving highly reactive species such as â¢OH, â¢O2- anions, h+, and e-, for the removal of organic and inorganic pollutants from water.
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Águas Residuárias , Purificação da Água , Catálise , Luz , TitânioRESUMO
The increase in new cases of drug resistance to first-line drugs such as ethambutol (ETB) makes it necessary to develop improvements for antituberculosis drugs. A new method for improving the bioavailability of active pharmaceutical ingredient (API) was investigated for preventing drug resistance and side-effects of antituberculosis drugs. In this study, an antituberculosis drug delivery system using ß-cyclodextrin (ß-CD) as the supramolecular carrier of ETB was prepared using the kneading method. The inclusion behaviour of ß-CD/ETB inclusion complex in solid and liquid state was investigated. The inclusion complex was characterized using Fourier transform infrared spectroscopy, thermogravimetric analysis, nuclear magnetic resonance (NMR) spectroscopy, and UV-visible spectroscopy. The 1H and nuclear Overhauser effect spectroscopy NMR results indicated the hydrophobic interaction between ß-CD and ETB. Meanwhile, the Benesi-Hildebrand equation was used to calculate the formation constant (K) of ß-CD/ETB complex in natural condition, pH4, and pH9, which were 105.43, 107.06, and 119.11, respectively. The stoichiometry ratio of ß-CD/ETB complex was proven to be 1:1.
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A series of Zn(II)-Schiff bases I, II and III complexes were synthesized by reaction of o-phenylenediamine with 3-methylsalicylaldehyde, 4-methylsalicylaldehyde and 5-methylsalicylaldehyde. These complexes were characterized using FT-IR, UV-Vis, Diffuse reflectance UV-Vis, elemental analysis and conductivity. Complex III was characterized by XRD single crystal, which crystallizes in the triclinic system, space group P-1, with lattice parameters a=9.5444(2) Å, b=11.9407(2) Å, c=21.1732(3) Å, V=2390.24(7) Å(3), D ( c )=1.408 Mg m(-3), Z=4, F(000)=1050, GOF=0.981, R1=0.0502, wR2=0.1205. Luminescence property of these complexes was investigated in DMF solution and in the solid state. Computational study of the electronic properties of complex III showed good agreement with the experimental data.
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Luminescência , Compostos Organometálicos/química , Compostos Organometálicos/síntese química , Teoria Quântica , Bases de Schiff/química , Zinco/química , Cristalografia por Raios X , Modelos Moleculares , Estrutura Molecular , Espectrometria de Fluorescência , Espectrofotometria UltravioletaRESUMO
Plasticised poly(vinyl chloride)-based membranes containing the ionophores (α-, ß- and γ-cyclodextrins (CD), dibenzo-18-crown-6 (DB18C6) and dibenzo-30-crown-10 (DB30C10) were evaluated for their potentiometric response towards promethazine (PM) in a flow injection analysis (FIA) set-up. Good responses were obtained when ß- and γ-CDs, and DB30C10 were used. The performance characteristics were further improved when tetrakis(4-chlorophenyl) borate (KTPB) was added to the membrane. The sensor based on ß-CD, bis(2-ethylhexyl) adipate (BEHA) and KTPB exhibited the best performance among the eighteen sensor compositions that were tested. The response was linear from 1 × 10(-5) to 1 × 10(-2) M, slope was 61.3 mV decade(-1), the pH independent region ranged from 4.5 to 7.0, a limit of detection of 5.3 × 10(-6) M was possible and a lifetime of more than a month was observed when used in the FIA system. Other plasticisers such as dioctyl phenylphosphonate and tributyl phosphate do not show significant improvements in the quality of the sensors. The promising sensors were further tested for the effects of foreign ions (Li(+), Na(+), K(+), Mg(2+), Ca(2+), Co(2+), Cu(2+), Cr(3+), Fe(3+), glucose, fructose). FIA conditions (e.g., effects of flow rate, injection volume, pH of the carrier stream) were also studied when the best sensor was used (based on ß-CD). The sensor was applied to the determination of PM in four pharmaceutical preparations and human urine that were spiked with different levels of PM. Good agreement between the sensor and the manufacturer's claimed values (for pharmaceutical preparations) was obtained, while mean recoveries of 98.6% were obtained for spiked urine samples. The molecular recognition features of the sensors as revealed by molecular modelling were rationalised by the nature of the interactions and complexation energies between the host and guest molecules.
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Ionóforos/química , Preparações Farmacêuticas/química , Potenciometria , Prometazina/urina , Éteres de Coroa/química , Eletrodos , Análise de Injeção de Fluxo , Humanos , Concentração de Íons de Hidrogênio , Íons/química , Membranas Artificiais , Metais/química , alfa-Ciclodextrinas/química , beta-Ciclodextrinas/química , gama-Ciclodextrinas/químicaRESUMO
The influence of variable reaction time (tr) on surface/textural properties (surface area, total pore volume, and pore diameter) of carbon-encapsulated magnetite (Fe3O4@C) nanocomposites fabricated by a hydrothermal process at 190 °C for 3, 4, and 5 h was studied. The properties were calculated using the Brunauer-Emmett-Teller (BET) isotherms data. The nanocomposites were characterised using Fourier transform infrared spectroscopy, X-ray diffraction analysis, thermogravimetry, and scanning and transmission electron microscopies. Analysis of variance shows tr has the largest effect on pore volume (F value = 1117.6, p value < 0.0001), followed by the surface area (F value = 54.8, p value < 0.0001) and pore diameter (F value = 10.4, p value < 0.001) with R2-adjusted values of 99.5%, 88.5% and 63.1%, respectively. Tukey and Fisher tests confirmed tr rise to have caused increased variations in mean particle sizes (11-91 nm), crystallite sizes (5-21 nm), pore diameters (9-16 nm), pore volume (0.017-0.089 cm3 g-1) and surface area (7.6-22.4 m2 g-1) of the nanocomposites with individual and simultaneous confidence limits of 97.9 and 84.4 (p-adj < 0.05). The nanocomposites' retained Fe-O vibrations at octahedral (436 cm-1) and tetrahedral (570 cm-1) cubic ferrite sites, modest thermal stability (37-60 % weight loss), and large volume-specific surface area with potential for catalytic application in advanced oxidation processes.
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Sustainable water processing techniques have been extensively investigated and are capable of improving water quality. Among the techniques, photocatalytic technology has shown great potential in recent years as a low cost, environmentally friendly and sustainable technology. However, the major challenge in the industrial development of photocatalyst technology is to develop an ideal photocatalyst which must have high photocatalytic activity, a large specific surface area, harvest sunlight and shows recyclability. Keeping these views, the present review highlighted the synthesis approaches of graphene/metal oxide nanocomposite, characterization techniques and their prominent applications in photocatalysis. Various parameters such as photocatalyst loading, structure of photocatalyst, temperature, pH, effect of oxidizing species and wavelength of light were addressed which could affect the rate of degradation. Moreover, the formation of intermediates during photo-oxidation of organic pollutants using these photocatalysts is also discussed. The analysis concluded with a synopsis of the importance of graphene-based materials in pollutant removal. Finally, a brief overview of the problems and future approaches in the field is also presented.
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In the title compound, C(15)H(14)N(2)O(4), the N=C double bond has an E configuration. The two benzene rings make a dihedral angle of 28.59â (6)°. In the crystal, mol-ecules are linked into a three-dimensional network by inter-molecular N-Hâ¯O, O-Hâ¯O and C-Hâ¯O hydrogen bonds and stabilized by weak C-Hâ¯π inter-actions.
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Herein, the role of metal-based nanoparticles (NPs) in biomedical analysis and the treatment of critical deceases been highlighted. In the world of nanotechnology, noble elements such as the gold/silver/palladium (Au/Ag/Pd) NPs are the most promising emerging trend to design bioengineering materials that could to be employed as modern diagnostic tools and devices to combat serious diseases. NPs are considered a powerful and advanced chemical tool to diagnose and to cure critical ailments such as HIV, cancer, and other types of infectious illnesses. The treatment of cancer is the most significant application of nanotechnology which is based on premature tumor detection and analysis of cancer cells through Nano-devices. The fascinating characteristic properties of NPs-such as high surface area, high surface Plasmon resonance, multi-functionalization, highly stable nature, and easy processing-make them more prolific for nanotechnology. In this review article, the multifunctional roles of Au/Ag/Pd NPs in the field of medical science, the physicochemical toxicity dependent properties, and the interaction mechanism is highlighted. Due to the cytotoxicity of Ag/Au/Pd NPs, the conclusion and future remarks emphasize the need for further research to minimize the toxicity of NPs in the bio-medicinal field.
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We study the influence of the bulky aromatic rings, e.g. anthracence-9-carboxylic acid (9-ACA) with a large conjugated pi-system on the structure and spectroscopic properties of [Er(2)(9-AC)(6)(DMF)(2)(H(2)O)(2)] complex where 9-AC=anthracence-9-carboxylato and DMF=N,N'-dimethylformamide. The complex has been prepared from the erbium chloride and 9-ACA in the mixture of H(2)O:DMF solution (4:1, v/v) followed by pH adjustment to 6. The complex is crystallized in a monoclinic system with space group P2(1)/n. The two Er(III) ions are double bridged by the deprotonated carboxyl groups of two 9-AC anions (O1 and O1A), forming an eight-coordination number. The chelating bidentate (O,O), chelating-bridging tridentate (O,O,O') and monodentate of 9-AC anions are observed in the dinuclear [Er(2)(9-AC)(6)(DMF)(2)(H(2)O)(2)] complex. The Er-Er distance is 4.015A in the dimeric unit. Intramolecular O-Hcdots, three dots, centeredO and C-Hcdots, three dots, centeredO hydrogen bonds as well as numerous of intermolecular C-Hcdots, three dots, centeredpi interactions between the anthracene rings by edge-to-face interactions linked the dinuclear dimeric units into two-dimensional supramolecular network in a propeller-arrangement. Electronic absorption spectra of the Er(III) complex and its salt were measured. The emission spectrum of the complex is composed of a broad band due to the emission of intraligand pi*-->pi transition from the 9-AC anions and a shoulder peak originating from the 4f-4f emission transition of the Er(III) ions. The complex has a high thermal stability which can be attributed to the effectively increase the rigidity of the 9-AC anions.
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Antracenos/química , Ácidos Carboxílicos/química , Érbio/química , Conformação Molecular , Cristalização , Cristalografia por Raios X , Dimerização , Modelos Moleculares , Estrutura MolecularRESUMO
In the title compound, {[Nd(C(8)H(3)NO(6))(C(8)H(4)NO(6))(H(2)O)(2)]·2.5H(2)O}(n), the Nd(II) ion is nine-coordinated by seven O atoms from five carboxyl-ate groups and two water mol-ecules. The [Nd(C(8)H(3)NO(6))(H(2)O)(2)](2+) units are bridged by 5-nitro-isophthalate dianions, forming polymeric sheets parallel to the ab plane. The polymeric sheets are linked into a three-dimensional network by O-Hâ¯O and C-Hâ¯O hydrogen bonds, and π-π inter-actions [centroid-centroid distance = 3.5533â (11)â Å]. The 5-nitro-isophthalate(1-) anion is disordered over three positions with an occupancy ratio of 0.68:0.23:0.09. Two of the uncoordinated water mol-ecules are disordered over two positions, with occupancy ratios of 0.722â (15):0.278â (15) and 0.279â (6):0.221â (6), respectively.
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The asymmetric unit of the title Schiff base compound, C(21)H(18)N(2)O(4), consists of four independent zwitterions (A, B, C and D) with similar conformations. In each independent mol-ecule, the methyl group is disordered over two positions; the occupancies of the two positions are 0.819â (5) and 0.181â (5) in mol-ecule A, 0.912â (5) and 0.088â (5) in B, 0.734â (5) and 0.266â (5) in C, and 0.940â (6) and 0.060â (6) in D. The dihydroxy-phenyl and the hydroxy-phenolate rings in mol-ecule A form dihedral angles of 17.36â (12) and 13.30â (12)°, respectively, with the central benzene ring, whereas the respective angles for mol-ecules B, C and D are 30.22â (11)/7.46â (11), 35.26â (12)/11.01â (12) and 39.89â (12)/4.29â (12)°. In all independent mol-ecules, intra-molecular N-Hâ¯O and O-Hâ¯N hydrogen bonds generate S(6) ring motifs. The four independent mol-ecules are linked into two pairs, viz. A-B and C-D, by inter-molecular O-Hâ¯O hydrogen bonds. These pairs are linked into a two-dimensional network parallel to the ab plane by C-Hâ¯O hydrogen bonds. In addition, C-Hâ¯π and π-π [centroid-centroid distance = 3.5153â (14)-3.7810â (15)â Å] inter-actions stabilize the crystal structure.