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Inorganics
Volume 10
Issue 8
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Inorganics, Volume 10, Issue 8 (August 2022) – 19 articles

Cover Story (view full-size image): Iridium oxide (IrO2) displays appealing characteristics that make it the ideal candidate for specific applications. As for other metal oxides, controlling its architecture at the nanoscale can consent to boost the efficiency of the exhibited properties. Nanostructuration of IrO2 can be achieved through dedicated methodologies and techniques which allow obtaining metal oxide under different shapes, ranging from nanopowders to nanorods, nanotubes, nanofibers, and nanostructured thin films. The present review is dedicated to the state of the art of nanostructured IrO2, showing in each case the improvements in performances in particular for the most frequently reported applications of this material, such as oxygen evolution reaction (OER), electrochromic devices, sensing, supercapacitor, and field emission cathodes. View this paper
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8 pages, 1557 KiB  
Article
Morphology Tuned Pressure Induced Amorphization in VO2(B) Nanobelts
by Benyuan Cheng, Huafang Zhang, Quanjun Li, Jing Liu and Bingbing Liu
Inorganics 2022, 10(8), 122; https://doi.org/10.3390/inorganics10080122 - 19 Aug 2022
Cited by 3 | Viewed by 1758
Abstract
Pressure-induced amorphization (PIA) has drawn great attention since it was first observed in ice. This process depends closely on the crystal structure, the size, the morphology and the correlated pressurization environments, among which the morphology-tuned PIA remains an open question on the widely [...] Read more.
Pressure-induced amorphization (PIA) has drawn great attention since it was first observed in ice. This process depends closely on the crystal structure, the size, the morphology and the correlated pressurization environments, among which the morphology-tuned PIA remains an open question on the widely concerned mesoscale. In this work, we report the synthesis and high-pressure research of VO2(B) nanobelts. XRD and TEM were performed to investigate the amorphization process. The amorphization pressure in VO2(B) nanobelts(~30 GPa) is much higher than that in previous reported 2D VO2(B) nanosheets(~21 GPa), the mechanism is the disruption of connectivity at particular relatively weaker bonds in the (010) plane. These results suggest a morphology-tuned pressure-induced amorphization, which could promote the fundamental understanding of PIA. Full article
(This article belongs to the Special Issue Research on Synthesis, Sintering and Properties of New Inorganic Materials under High Pressure and High Temperature)
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27 pages, 7927 KiB  
Review
Uranyl Analogue Complexes—Current Progress and Synthetic Challenges
by Leonor Maria and Joaquim Marçalo
Inorganics 2022, 10(8), 121; https://doi.org/10.3390/inorganics10080121 - 18 Aug 2022
Cited by 4 | Viewed by 2688
Abstract
Uranyl ions, {UO2}n+ (n = 1, 2), display trans, strongly covalent, and chemically robust U-O multiple bonds, where 6d, 5f, and 6p orbitals play important roles. The synthesis of isoelectronic analogues of uranyl has been of interest for quite [...] Read more.
Uranyl ions, {UO2}n+ (n = 1, 2), display trans, strongly covalent, and chemically robust U-O multiple bonds, where 6d, 5f, and 6p orbitals play important roles. The synthesis of isoelectronic analogues of uranyl has been of interest for quite some time, mainly with the purpose of unveiling covalence and 5f-orbital participation in bonding. Significant advances have occurred in the last two decades, initially marked by the synthesis of uranium(VI) bis(imido) complexes, the first analogues with a {RNUNR}2+ core, later followed by the synthesis of unique trans-{EUO}2+ (E = S, Se) complexes, and recently highlighted by the synthesis of the first complexes featuring a linear {NUN} moiety. This review covers the synthesis, structure, bonding, and reactivity of uranium complexes containing a linear {EUE}n+ core (n = 0, 1, 2), isoelectronic to uranyl ions, {OUO}n+ (n = 1, 2), incorporating σ- and π-donating ligands that can engage in uranium–ligand multiple bonding, where oxygen may be replaced by heavier chalcogenido, imido, nitride, and carbene ligands, or by a transition metal. It focuses on synthetic methods of well-defined molecular uranium species in the condensed phase but also references gas-phase and low-temperature-matrix experiments, as well as computational studies that may lead to valuable insights. Full article
(This article belongs to the Special Issue Synthesis, Properties and Applications of Lanthanide and Actinide Molecular Compounds)
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13 pages, 3182 KiB  
Article
Ab Initio Study of Structure and Transport Properties of Warm Dense Nitric Oxide
by Zhijian Fu, Xianming Zhang, Rui Wang, Huayang Sun, Yangshun Lan, Jihong Xia, Zhiguo Li and Jing Song
Inorganics 2022, 10(8), 120; https://doi.org/10.3390/inorganics10080120 - 18 Aug 2022
Viewed by 1746
Abstract
The structure, equation of state and transport properties of warm dense nitric oxide (NO) were investigated in wide density and temperature ranges by ab initio molecular dynamics simulations. Both the Perdew–Burke–Ernzerhof (PBE) and the strongly constrained and appropriately normed functional with revised Vydrov–van [...] Read more.
The structure, equation of state and transport properties of warm dense nitric oxide (NO) were investigated in wide density and temperature ranges by ab initio molecular dynamics simulations. Both the Perdew–Burke–Ernzerhof (PBE) and the strongly constrained and appropriately normed functional with revised Vydrov–van Voorhis nonlocal correlation (SCAN−rVV10) functionals were used in the simulations, and the pressures predicted by the SCAN−rVV10 functional were found to be systematically lower than those predicted using PBE and experimental data along the shock Hugoniot curve. Along the Hugoniot curve, as density increased, we found that the system transformed towards a mixture of atomic nitrogen and oxygen liquids with molecular NO that remained present up to the highest densities explored. The electrical conductivity along Hugoniot indicated that nonmetal to metal transition had taken place. We also calculated the electrical and thermal conductivities of nitric oxide in the warm dense matter regime, and used them to compute the Lorentz number. In addition, we also report the electronic density of states. Full article
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14 pages, 2272 KiB  
Article
Changes in Structural, Morphological and Optical Features of Differently Synthetized C3N4-ZnO Heterostructures: An Experimental Approach
by Arianna Actis, Francesca Sacchi, Christos Takidis, Maria Cristina Paganini and Erik Cerrato
Inorganics 2022, 10(8), 119; https://doi.org/10.3390/inorganics10080119 - 16 Aug 2022
Cited by 5 | Viewed by 2252
Abstract
C3N4 is an innovative material that has had huge success as a photocatalyst in recent years. More recently, it has been coupled to robust metal oxides to obtain more stable materials. This work is focused on the different synthesis techniques [...] Read more.
C3N4 is an innovative material that has had huge success as a photocatalyst in recent years. More recently, it has been coupled to robust metal oxides to obtain more stable materials. This work is focused on the different synthesis techniques used to prepare bare C3N4 and combined C3N4/ZnO mixed systems. Different precursors, such as pure melamine and cyanuric acid-based supramolecular complexes, were employed for the preparation of the C3N4 material. Moreover, different solvents were also used, demonstrating that the use of water leads to the formation of a more stable heterojunction. Structural (XRD), morphological (FESEM) and optical (UV-vis) measurements underlined the role of the precursors used in the preparation of the materials. A clear trend can be extrapolated from this experimental approach involving different intimate contacts between the two C3N4 and ZnO phases, strictly connected to the particular preparation method adopted. The use of the supramolecular complexes for the preparation of C3N4 leads to a tighter association between the two phases at the heterojunction, resulting in much higher visible light harvesting (connected to lower band gap values). Full article
(This article belongs to the Special Issue New Advances into Nanostructured Oxides)
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13 pages, 2424 KiB  
Article
Synthesis of a Heterometallic [Zn2Ca] Pinwheel Array Stabilized by Amide-Amide Synthons
by Daniel Ejarque, Teresa Calvet, Mercè Font-Bardia and Josefina Pons
Inorganics 2022, 10(8), 118; https://doi.org/10.3390/inorganics10080118 - 14 Aug 2022
Cited by 2 | Viewed by 2293
Abstract
The rational design of heterometallic compounds bearing s-block metal ions have been a difficult task for chemists owing to their lack of preferential geometries. However, some strategies, such as the design of coordinating pockets with different sizes and/or donor atoms, have offered great [...] Read more.
The rational design of heterometallic compounds bearing s-block metal ions have been a difficult task for chemists owing to their lack of preferential geometries. However, some strategies, such as the design of coordinating pockets with different sizes and/or donor atoms, have offered great results. In this work, this strategy has been tested using Ca(II) as an s-block metal ion and a compound previously obtained by our group with the formula [Zn3(μ-ACA)6(4-phpy)2], which contains tetrahedral N,O- and octahedral O-coordinating pockets as a model structure. From this work, the corresponding heterometallic compound with the formula [Zn2Ca(μ-ACA)6(4-phpy)2]·EtOH (1) has been successfully synthesized, and fully characterized, and its crystal structure has been elucidated. Furthermore, we have compiled all the crystal structures containing [Zn2M] pinwheel secondary building units (SBUs), where M stands for an s-block metal ion, and the observed tendencies, as well as the promising applications as template SBUs for the preparation of 1D–3D coordination polymers, have been discussed. Finally, solid-state UV-Vis and photoluminescence have been recorded and compared with the homometallic [Zn3(μ-ACA)6(4-phpy)2] compound. Full article
(This article belongs to the Special Issue Heterometallic Complexes)
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17 pages, 4519 KiB  
Article
Chiral Selectors in Voltammetric Sensors Based on Mixed Phenylalanine/Alanine Cu(II) and Zn(II) Complexes
by Rufina A. Zilberg, Tatyana V. Berestova, Ruslan R. Gizatov, Yulia B. Teres, Miras N. Galimov and Elena O. Bulysheva
Inorganics 2022, 10(8), 117; https://doi.org/10.3390/inorganics10080117 - 12 Aug 2022
Cited by 7 | Viewed by 1734
Abstract
A practical application composite based on mixed chelate complexes [M(S-Ala)2(H2O)n]–[M(S-Phe)2(H2O)n] (M = Cu(II), Zn(II); n = 0–1) as chiral selectors in enantioselective voltammetric sensors was suggested. The [...] Read more.
A practical application composite based on mixed chelate complexes [M(S-Ala)2(H2O)n]–[M(S-Phe)2(H2O)n] (M = Cu(II), Zn(II); n = 0–1) as chiral selectors in enantioselective voltammetric sensors was suggested. The structures of the resulting complexes were studied by XRD, ESI-MS, and IR- and NMR-spectroscopy methods. It was determined that enantioselectivity depends on the metal nature and on the structure of the mixed complex. The mixed complexes, which were suggested to be chiral selectors, were stable under the experimental conditions and provided greater enantioselectivity in the determination of chiral analytes, such as naproxen and propranolol, in comparison with the amino acids they comprise. The best results shown by the mixed copper complex [Cu(S-Ala)2]–[Cu(S-Phe)2] were: ipS/ipR = 1.27 and ΔEp = 30 mV for Nap; and ipS/ipR = 1.37 and ΔEp = 20 mV for Prp. The electrochemical and analytical characteristics of the sensors and conditions of voltammogram recordings were studied by differential pulse voltammetry. Linear relationships between the anodic current and the concentrations of Nap and Prp enantiomers were achieved in the range of 2.5 × 10−5 to 1.0 × 10−3 mol L−1 for GCE/PEC-[Cu(S-Ala)2]–[Cu(S-Phe)2] and 5.0 × 10−5 to 1.0 × 10−3 for GCE/PEC–[Zn(S-Ala)2(H2O)]–[Zn(S-Phe)2(H2O)], with detection limits (3 s/m) of 0.30–1.24 μM. The suggested sensor was used to analyze Nap and Prp enantiomers in urine and plasma samples. Full article
(This article belongs to the Special Issue Inorganic Chemosensors)
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18 pages, 4345 KiB  
Article
Energy Levels in Pentacoordinate d5 to d9 Complexes
by Ján Titiš, Cyril Rajnák and Roman Boča
Inorganics 2022, 10(8), 116; https://doi.org/10.3390/inorganics10080116 - 12 Aug 2022
Cited by 4 | Viewed by 1927
Abstract
Energy levels of pentacoordinate d5 to d9 complexes were evaluated according to the generalized crystal field theory at three levels of sophistication for two limiting cases of pentacoordination: trigonal bipyramid and tetragonal pyramid. The electronic crystal field terms involve the interelectron [...] Read more.
Energy levels of pentacoordinate d5 to d9 complexes were evaluated according to the generalized crystal field theory at three levels of sophistication for two limiting cases of pentacoordination: trigonal bipyramid and tetragonal pyramid. The electronic crystal field terms involve the interelectron repulsion and the crystal field potential; crystal field multiplets account for the spin–orbit interaction; and magnetic energy levels involve the orbital– and spin–Zeeman interactions with the magnetic field. The crystal field terms are labelled according to the irreducible representations of point groups D3h and C4v using Mulliken notation. The crystal field multiplets are labelled with the Bethe notations for the respective double groups D’3 and C’4. The magnetic functions, such as the temperature dependence of the effective magnetic moment and the field dependence of the magnetization, are evaluated by employing the apparatus of statistical thermodynamics as derivatives of the field-dependent partition function. When appropriate, the formalism of the spin Hamiltonian is applied, giving rise to a set of magnetic parameters, such as the zero-field splitting D and E, magnetogyric ratio tensor, and temperature-independent paramagnetism. The data calculated using GCFT were compared with the ab initio calculations at the CASSCF+NEVPT2 level and those involving the spin–orbit interaction. Full article
(This article belongs to the Special Issue Recent Progress in Coordination Chemistry)
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22 pages, 10298 KiB  
Review
Nanostructured Iridium Oxide: State of the Art
by Francesca Scarpelli, Nicolas Godbert, Alessandra Crispini and Iolinda Aiello
Inorganics 2022, 10(8), 115; https://doi.org/10.3390/inorganics10080115 - 5 Aug 2022
Cited by 8 | Viewed by 5190
Abstract
Iridium Oxide (IrO2) is a metal oxide with a rutile crystalline structure, analogous to the TiO2 rutile polymorph. Unlike other oxides of transition metals, IrO2 shows a metallic type conductivity and displays a low surface work function. IrO2 [...] Read more.
Iridium Oxide (IrO2) is a metal oxide with a rutile crystalline structure, analogous to the TiO2 rutile polymorph. Unlike other oxides of transition metals, IrO2 shows a metallic type conductivity and displays a low surface work function. IrO2 is also characterized by a high chemical stability. These highly desirable properties make IrO2 a rightful candidate for specific applications. Furthermore, IrO2 can be synthesized in the form of a wide variety of nanostructures ranging from nanopowder, nanosheets, nanotubes, nanorods, nanowires, and nanoporous thin films. IrO2 nanostructuration, which allows its attractive intrinsic properties to be enhanced, can therefore be exploited according to the pursued application. Indeed, IrO2 nanostructures have shown utility in fields that span from electrocatalysis, electrochromic devices, sensors, fuel cell and supercapacitors. After a brief description of the IrO2 structure and properties, the present review will describe the main employed synthetic methodologies that are followed to prepare selectively the various types of nanostructures, highlighting in each case the advantages brought by the nanostructuration illustrating their performances and applications. Full article
(This article belongs to the Special Issue New Advances into Nanostructured Oxides)
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9 pages, 4843 KiB  
Communication
Short-Chain Acid Additives to Control PbI2 Crystallization in Hybrid Perovskite Films
by Chiara Dionigi, Gabriele Calabrese, Giampiero Ruani and Silvia Milita
Inorganics 2022, 10(8), 114; https://doi.org/10.3390/inorganics10080114 - 5 Aug 2022
Cited by 3 | Viewed by 2048
Abstract
The quality and the performance of hybrid perovskite (HP)’s films strongly depend on the complete conversion into MAPbI3 of a spin-coated solution of methylammonium iodide (MAI) and PbI2. Highly crystalline PbI2 on a substrate limits such a conversion and, [...] Read more.
The quality and the performance of hybrid perovskite (HP)’s films strongly depend on the complete conversion into MAPbI3 of a spin-coated solution of methylammonium iodide (MAI) and PbI2. Highly crystalline PbI2 on a substrate limits such a conversion and, consequently, the HP’s solar cell performances. We investigate for the first time the use of short-chain organic acids as additives in a non-complexing solvent like γ-butyrolactone (GBL), that can retard retard the crystallization of PbI2. Based on XRD analyses of the spin coated films, the acetic acid is the most effective additive in retarding the PbI2 crystallization, making Pb2+ available for a subsequent reaction with MAI. These results open a new experimental path for fabricating perovskite films by single or sequential step methods involving acid additives. Full article
(This article belongs to the Section Inorganic Materials)
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12 pages, 3010 KiB  
Article
Green Synthesis of Silver Nanoparticles Using Artemisia vulgaris Extract and Its Application toward Catalytic and Metal-Sensing Activity
by Achyut Adhikari, Laxman Lamichhane, Anup Adhikari, Gobinda Gyawali, Debendra Acharya, Ek Raj Baral and Kisan Chhetri
Inorganics 2022, 10(8), 113; https://doi.org/10.3390/inorganics10080113 - 4 Aug 2022
Cited by 20 | Viewed by 3674
Abstract
Nonessential heavy metals are toxic to human health. In this study, mercury, a hazardous metal, was detected by colorimetric analysis using Artemisia vulgaris-mediated silver nanoparticles (AgNP) without any modification in an aqueous solution. The UV–vis spectroscopy showed a characteristic SPR band of [...] Read more.
Nonessential heavy metals are toxic to human health. In this study, mercury, a hazardous metal, was detected by colorimetric analysis using Artemisia vulgaris-mediated silver nanoparticles (AgNP) without any modification in an aqueous solution. The UV–vis spectroscopy showed a characteristic SPR band of Ag0 at 418 nm, indicating the formation of AgNPs. The AgNPs were crystalline, with an average size of 7 nm, as calculated from the XRD data. The SEM images revealed the spherical and polycrystalline AgNPs within the agglomerated form. The FTIR spectra elucidated the functional group of the extract attached with the Ag0. The broad, strong peak at 3632 cm−1 indicated the involvement of the -OH group of compounds of extract in reducing silver ions. The peak of EDX spectra around 3 keV confirmed the silver in the nanostructure. A colorimetric method was employed for the heavy metal sensing in the aqueous medium without modification of AgNPs suspension. The obtained AgNPs were found to be selective and highly sensitive toward Hg2+ ions. The AgNPs suspension turned colorless after adding 380 µL of 1 mM Hg2+. The synthesized AgNPs showed the catalytic activity on reduction of 4-nitrophenol in the presence of NaBH4 within 8 min with a rate constant of 1.21 × 10−2 s−1. The outcome of these findings suggests that the application of Artemisia vulgaris influenced AgNPs for metal sensing and green catalysis. Full article
(This article belongs to the Special Issue Metal Nanomaterials as Efficient Electrocatalysts)
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13 pages, 4331 KiB  
Article
Stabilizing the (003) Facet of Micron-Sized LiNi0.6Co0.2Mn0.2O2 Cathode Material Using Tungsten Oxide as an Exemplar
by Yang Li, Liubin Ben, Hailong Yu, Wenwu Zhao, Xinjiang Liu and Xuejie Huang
Inorganics 2022, 10(8), 111; https://doi.org/10.3390/inorganics10080111 - 3 Aug 2022
Cited by 7 | Viewed by 2616
Abstract
The structural stability of layered LiNi1-x-yCoxMnyO2 cathode materials is critical for guaranteeing their excellent electrochemical cycling performance, particularly at elevated temperatures. However, the notorious H2–H3 phase transition along with associated large changes in [...] Read more.
The structural stability of layered LiNi1-x-yCoxMnyO2 cathode materials is critical for guaranteeing their excellent electrochemical cycling performance, particularly at elevated temperatures. However, the notorious H2–H3 phase transition along with associated large changes in the c-axis or (003) facet is the fundamental origin of the anisotropic and abrupt change in the unit cell and the degradation of the cycling performance. In this study, we coat micron-sized LiNi0.6Co0.2Mn0.2O2 (NCM) with tungsten oxide via atomic layer deposition and investigate the atomic-to-microscopic structures in detail via advanced characterization techniques, such as Cs-corrected scanning transmission electron microscopy. The results reveal that coated tungsten oxide is predominately accumulated on the (003) facet of NCM, with the migration of a small amount of W6+ into this facet, resulting in a reduction of Ni3+ to Ni2+ and the formation of a rock-salt-like structure on the surface. The electrochemical cycling performance of tungsten-oxide-coated NCM is significantly improved, showing a capacity retention of 86.8% after 300 cycles at 55 °C, compared to only 69.4% for the bare NCM. Through further structural analysis, it is found that the initial tungsten-oxide-coating-induced (003) facet distortion effectively mitigates the expansion of the c-lattice during charge, as well as oxygen release from the lattice, resulting in a lowered strain in the cathode lattices and a crack in the cathode particles after prolonged cycling. Full article
(This article belongs to the Special Issue A Themed Issue in Honor of Professor Michel Armand on the Occasion of His 75th Birthday)
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15 pages, 3119 KiB  
Article
Synthesis, Characterization, Computational and Biological Activity of Some Schiff Bases and Their Fe, Cu and Zn Complexes
by Tareq M. A. Al-Shboul, Mohammad El-khateeb, Zaid H. Obeidat, Taher S. Ababneh, Suha S. Al-Tarawneh, Mazhar S. Al Zoubi, Walhan Alshaer, Anas Abu Seni, Taqwa Qasem, Hayato Moriyama, Yukihiro Yoshida, Hiroshi Kitagawa and Taghreed M. A. Jazzazi
Inorganics 2022, 10(8), 112; https://doi.org/10.3390/inorganics10080112 - 2 Aug 2022
Cited by 15 | Viewed by 4086
Abstract
Four new symmetrical Schiff bases derived from 2,2′-diamino-6,6′-dibromo-4,4′-dimethyl-1,1′-biphenyl or 2,2′-diamino-4,4′-dimethyl-1,1′-biphenyl, and 3,5-dichloro- or 5-nitro-salicylaldehyde, were synthesized and reacted with copper-, iron- and zinc-acetate, producing the corresponding complexes. The Schiff bases and their metal complexes were characterized by 1H-, 13C-NMR, IR and [...] Read more.
Four new symmetrical Schiff bases derived from 2,2′-diamino-6,6′-dibromo-4,4′-dimethyl-1,1′-biphenyl or 2,2′-diamino-4,4′-dimethyl-1,1′-biphenyl, and 3,5-dichloro- or 5-nitro-salicylaldehyde, were synthesized and reacted with copper-, iron- and zinc-acetate, producing the corresponding complexes. The Schiff bases and their metal complexes were characterized by 1H-, 13C-NMR, IR and UV-Vis spectroscopy and elemental analysis. The structures of one Schiff base and the two zinc complexes were resolved by X-ray structure determination. Density functional theory (DFT) calculations at the B3LYP/6-31G(d) level of the latter compounds were carried out to optimize and examine their molecular geometries. The biomedical applications of the Schiff bases and their complexes were investigated as anticancer or antimicrobial agents. Full article
(This article belongs to the Special Issue Synthesis, Structure and Properties of Schiff Base Metal Complexes)
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14 pages, 3764 KiB  
Review
Solid Polymer Electrolytes for Lithium Batteries: A Tribute to Michel Armand
by Alain Mauger and Christian M. Julien
Inorganics 2022, 10(8), 110; https://doi.org/10.3390/inorganics10080110 - 29 Jul 2022
Cited by 10 | Viewed by 4047
Abstract
In a previous publication, a tribute to Michel Armand was provided, which highlighted his outstanding contribution to all aspects of research and development of lithium-metal and lithium-ion batteries. This area is in constant progress and rather than an overview of the work of [...] Read more.
In a previous publication, a tribute to Michel Armand was provided, which highlighted his outstanding contribution to all aspects of research and development of lithium-metal and lithium-ion batteries. This area is in constant progress and rather than an overview of the work of Armand et al. since the seventies, we mainly restrict this review to his contribution to advances in solid polymer electrolytes (SPEs) and their performance in all-solid-state lithium-metal batteries in recent years. Full article
(This article belongs to the Special Issue A Themed Issue in Honor of Professor Michel Armand on the Occasion of His 75th Birthday)
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16 pages, 2605 KiB  
Article
New Phosphonite Ligands with High Steric Demand and Low Basicity: Synthesis, Structural Properties and Cyclometalated Complexes of Pt(II)
by María M. Alcaide, Matteo Pugliesi, Eleuterio Álvarez, Joaquín López-Serrano and Riccardo Peloso
Inorganics 2022, 10(8), 109; https://doi.org/10.3390/inorganics10080109 - 29 Jul 2022
Viewed by 2118
Abstract
Two phosphonite ligands bearing the highly sterically demanding 2,6-bis (2,6-dimethylphenyl)phenyl group (ArXyl2), PArXyl2(OPhNO2)2 and PArXyl2(OPhNO2,Me)2, were prepared from the parent dihalophosphines PArXyl2 [...] Read more.
Two phosphonite ligands bearing the highly sterically demanding 2,6-bis (2,6-dimethylphenyl)phenyl group (ArXyl2), PArXyl2(OPhNO2)2 and PArXyl2(OPhNO2,Me)2, were prepared from the parent dihalophosphines PArXyl2X2 (X = Cl, Br) and the corresponding phenols, 4-nitrophenol and 4-nitro-2,6-dimethylphenol, respectively. DFT methods were used to examine their structural features and to determine three steric descriptors, namely the Tolman cone angle, the percentage of buried volume, and the percentage of the coordination sphere protected by the ligand. A comparison with the related terphenyl phosphines is also provided. Reactions of PArXyl2(OPhNO2)2 and PArXyl2(OPhNO2,Me)2 with several Pt(II) precursors were investigated, revealing a high tendency of both phosphonites to undergo C-H activation processes and generate five- or six-membered cyclometalated structures. The coordination chemistry of the new ligands was explored with isolation, among others, of three carbonyl complexes, 1-3∙CO, and the triphenylphosphine adduct 3∙PPh3. X-ray diffraction methods permitted the determination of the solid-state structures of the mononuclear methyl carbonyl complex 1∙CO, the dinuclear chloride-bridged complex 2 and the doubly cyclometalated complex 3∙SMe2, including the conformations adopted by the ligands upon coordination. All of the new compounds were characterized by multinuclear NMR spectroscopy in solution. Full article
(This article belongs to the Special Issue Phosphorus Ligands for the Stabilization of Unusual and Elusive Structures in Transition Metal Complexes)
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5 pages, 205 KiB  
Editorial
Cornerstones in Contemporary Inorganic Chemistry
by Duncan H. Gregory
Inorganics 2022, 10(8), 108; https://doi.org/10.3390/inorganics10080108 - 28 Jul 2022
Viewed by 1556
Abstract
I am very happy to be able to present this Special Issue of Inorganics [...] Full article
(This article belongs to the Special Issue Cornerstones in Contemporary Inorganic Chemistry)
16 pages, 3687 KiB  
Article
Fluoro-Germanium (IV) Cations with Neutral Co-Ligands—Synthesis, Properties and Comparison with Neutral GeF4 Adducts
by Madeleine S. Woodward, Rhys P. King, Robert D. Bannister, Julian Grigg, Graeme McRobbie, William Levason and Gillian Reid
Inorganics 2022, 10(8), 107; https://doi.org/10.3390/inorganics10080107 - 27 Jul 2022
Cited by 4 | Viewed by 2382
Abstract
The reaction of [GeF4L2], L = dmso (Me2SO), dmf (Me2NCHO), py (pyridine), pyNO (pyridine-N-oxide), OPPh3, OPMe3, with Me3SiO3SCF3 (TMSOTf) and monodentate ligands, L, in a 1:1:1 [...] Read more.
The reaction of [GeF4L2], L = dmso (Me2SO), dmf (Me2NCHO), py (pyridine), pyNO (pyridine-N-oxide), OPPh3, OPMe3, with Me3SiO3SCF3 (TMSOTf) and monodentate ligands, L, in a 1:1:1 molar ratio in anhydrous CH2Cl2 formed the monocations [GeF3L3][OTf]. These rare trifluoro-germanium (IV) cations were characterised by microanalysis, IR, 1H, 19F{1H} and, where appropriate, 31P{1H} NMR spectroscopy. The 19F{1H} NMR data show that in CH3NO2 solution the complexes exist as a mixture of mer and fac isomers, with the mer isomer invariably having the higher abundance. The X-ray structure of mer-[GeF3(OPPh3)3][OTf] is also reported. The attempts to remove a second fluoride using a further equivalent of TMSOTf and L were mostly unsuccessful, although a mixture of [GeF2(OAsPh3)4][OTf]2 and [GeF3(OAsPh3)3][OTf] was obtained using excess TMSOTf and OAsPh3. The reaction of [GeF4(MeCN)2] with TMSOTf in CH2Cl2 solution, followed by the addition of 2,2′:6′,2”-terpyridine (terpy) formed mer-[GeF3(terpy)][OTf], whilst a similar reaction with 1,4,7-trimethyl-1,4,7-triazacyclononane (Me3-tacn) in MeCN solution produced fac-[GeF3(Me3-tacn)][OTf]. Dicationic complexes bearing the GeF22+ fragment were isolated using the tetra-aza macrocycles, 1,4,7,10-tetramethyl-1,4,7,10-tetra-azacyclododecane (Me4-cyclen) and 1,4,8,11-tetramethyl-1,4,8,11-tetra-azacyclotetradecane (Me4-cyclam), which reacted with [GeF4(MeCN)2] and two equivalents of TMSOTf to cleanly form the dicationic difluoride salts, cis-[GeF2(Me4-cyclen)][OTf]2 and trans-[GeF2(Me4-cyclam)][OTf]2. The 19F{1H} NMR spectroscopy shows that in CH3NO2 solution there are four stereoisomers present for trans-[GeF2(Me4-cyclam)][OTf]2, whereas the smaller ring-size of Me4-cyclen accounts for the formation of only cis-[GeF2(Me4-cyclen)][OTf], and is confirmed crystallographically. New spectroscopic data are also reported for [GeF4(L)2] (L = dmso, dmf and pyNO). Density functional theory calculations were used to probe the effect on the bonding as fluoride ligands were sequentially removed from the germanium centre in the OPMe3 complexes. Full article
(This article belongs to the Special Issue Synergy between Main Group and Transition Metal Chemistry)
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21 pages, 8279 KiB  
Review
Research Progress on Preparation Methods of Skutterudites
by Chengyu Zhao, Minhua Wang and Zhiyuan Liu
Inorganics 2022, 10(8), 106; https://doi.org/10.3390/inorganics10080106 - 26 Jul 2022
Cited by 8 | Viewed by 2645
Abstract
Thermoelectric material is a new energy material that can realize the direct conversion of thermal energy and electric energy. It has important and wide applications in the fields of the recycling of industrial waste heat and automobile exhaust, efficient refrigeration of the next [...] Read more.
Thermoelectric material is a new energy material that can realize the direct conversion of thermal energy and electric energy. It has important and wide applications in the fields of the recycling of industrial waste heat and automobile exhaust, efficient refrigeration of the next generation of integrated circuits and full spectrum solar power generation. Skutterudites have attracted much attention because of their excellent electrical transport performance in the medium temperature region. In order to obtain skutterudites with excellent properties, it is indispensable to choose an appropriate preparation method. This review summarizes some traditional and advanced preparation methods of skutterudites in recent years. The basic principles of these preparation methods are briefly introduced. Single-phase skutterudites can be successfully obtained by these preparation methods. The study of these preparation methods also provides technical support for the rapid, low-cost and large-scale preparation of high-performance thermoelectric materials. Full article
(This article belongs to the Special Issue Advances of Thermoelectric Materials)
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12 pages, 2526 KiB  
Article
Field-Induced Single Molecule Magnetic Behavior of Mononuclear Cobalt(II) Schiff Base Complex Derived from 5-Bromo Vanillin
by Fikre Elemo, Sören Schlittenhardt, Taju Sani, Cyril Rajnák, Wolfgang Linert, Roman Boča, Madhu Thomas and Mario Ruben
Inorganics 2022, 10(8), 105; https://doi.org/10.3390/inorganics10080105 - 25 Jul 2022
Cited by 1 | Viewed by 2334
Abstract
A mononuclear Co(II) complex of a Schiff base ligand derived from 5-Bromo-vanillin and 4-aminoantipyrine, that has a compressed tetragonal bipyramidal geometry and exhibiting field-induced slow magnetic relaxation, has been synthesized and characterized by single crystal X-ray diffraction, elemental analysis and molecular spectroscopy. In [...] Read more.
A mononuclear Co(II) complex of a Schiff base ligand derived from 5-Bromo-vanillin and 4-aminoantipyrine, that has a compressed tetragonal bipyramidal geometry and exhibiting field-induced slow magnetic relaxation, has been synthesized and characterized by single crystal X-ray diffraction, elemental analysis and molecular spectroscopy. In the crystal packing, a hydrogen-bonded dimer structural topology has been observed with two distinct metal centers having slightly different bond parameters. The complex has been further investigated for its magnetic nature on a SQUID magnetometer. The DC magnetic data confirm that the complex behaves as a typical S = 3/2 spin system with a sizable axial zero-field splitting parameter D/hc = 38 cm−1. The AC susceptibility data reveal that the relaxation time for the single-mode relaxation process is τ = 0.16(1) ms at T = 2.0 K and BDC = 0.12 T. Full article
(This article belongs to the Special Issue Synthesis, Structure and Properties of Schiff Base Metal Complexes)
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17 pages, 8959 KiB  
Article
New Carboxylate Anionic Sm-MOF: Synthesis, Structure and Effect of the Isomorphic Substitution of Sm3+ with Gd3+ and Tb3+ Ions on the Luminescent Properties
by Anna A. Ivanova, Victoria E. Gontcharenko, Alexey M. Lunev, Anastasia V. Sidoruk, Ilya A. Arkhipov, Ilya V. Taydakov and Yuriy A. Belousov
Inorganics 2022, 10(8), 104; https://doi.org/10.3390/inorganics10080104 - 25 Jul 2022
Cited by 14 | Viewed by 3334
Abstract
Two new compounds, namely {(NMe2H2)}[Ln(TDA)(HCOO)] 0.5H2O, Ln = Sm3+ (Sm-TDA) and Gd3+ (Gd-TDA), where TDA3− is the anion of 1H-1,2,3-triazole-4,5-dicarboxylic acid (H3TDA), were synthesized by the [...] Read more.
Two new compounds, namely {(NMe2H2)}[Ln(TDA)(HCOO)] 0.5H2O, Ln = Sm3+ (Sm-TDA) and Gd3+ (Gd-TDA), where TDA3− is the anion of 1H-1,2,3-triazole-4,5-dicarboxylic acid (H3TDA), were synthesized by the solvothermal method in a DMF:H2O mixture. According to single-crystal X-ray diffraction data, the compounds are 3d-MOFs with an anionic lattice and dimethylammonium cations occupying part of the cavities. Based on these compounds, two series of mixed-metal complexes, [NMe2H2][SmxLn1-x(TDA)(HCOO)], (x = 0.9 (Sm0.9Ln0.1-TDA), x = 0.8 (Sm0.8-Ln0.2-TDA)…Sm0.02Ln0.98-TDA, Ln = Tb, Gd), were also obtained and characterized by powder XRD. The luminescent properties of the compounds were studied and it was shown that the resulting compounds are two- or three-component emitters with the possibility of fine color tuning by changing the intensities of fluorescence and phosphorescence of the ligand, as well as the luminescence of Sm3+ and Tb3+ f-ions. Full article
(This article belongs to the Special Issue Recent Advances in the Synthesis and Luminescence Properties of Metal Complexes)
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