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12 pages, 5726 KiB

Open AccessArticle

Gallium Trichloride Fluid: Dimer Dissociation Mechanism, Local Structure, and Atomic Dynamics

by Maxim Khomenko, Anton Sokolov, Andrey Tverjanovich, Maria Bokova, Mohammad Kassem, Takeshi Usuki and Eugene Bychkov

Molecules 2024, 29(6), 1358; https://doi.org/10.3390/molecules29061358 - 19 Mar 2024

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Abstract

Molten gallium trichloride emerges as a promising solvent for oxidative metal recycling. The use of supercritical fluid enhances the performance and kinetics of metal dissolution due to significantly lower viscosity in the reaction media. Additionally, the dual molecular nature of gallium trichloride, existing [...] Read more.

Molten gallium trichloride emerges as a promising solvent for oxidative metal recycling. The use of supercritical fluid enhances the performance and kinetics of metal dissolution due to significantly lower viscosity in the reaction media. Additionally, the dual molecular nature of gallium trichloride, existing as edge-sharing ES-Ga₂Cl₆ dimers at low temperatures and high pressure, or flat trigonal GaCl₃ monomers in the vicinity of the critical point and low pressures, creates the possibility to tailor the chemical geometry to a particular metallic species. Nevertheless, the mechanism of dimer dissociation, local structure, and atomic dynamics in supercritical gallium trichloride fluids are not known. Using first-principles molecular dynamics, validated by comparison with our high-energy X-ray diffraction results, we illustrate the elementary steps in dimer dissociation. These include the formation of intermediate corner-sharing CS-Ga₂Cl₆ dimers, the partial disproportionation of GaCl₃ monomers at high temperatures and low pressures, changes in the local environment of molecular entities, and unusual atomic dynamics in supercritical fluids. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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10 pages, 2445 KiB

Open AccessArticle

Synthesis of Alkenylgold(I) Complexes Relevant to Catalytic Carboxylative Cyclization of Unsaturated Amines and Alcohols

by Shun Hase, Kyohei Yamashita and Yoshihito Kayaki

Molecules 2024, 29(6), 1331; https://doi.org/10.3390/molecules29061331 - 16 Mar 2024

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Abstract

The carboxylation of unsaturated amine and alcohol compounds, including 4-benzylamino-1-phenyl-1-butyne (homopropargylamine), 2-butyne-1-ol (propargylic alcohol), and 2,3-butadiene-1-ol (allenylmethyl alcohol), using the hydroxidogold(I) complex, AuOH(IPr) [IPr = 1,3-bis(2,6-diisopropylphenyl)-imidazol-2-ylidene], produces corresponding alkenylgold(I) complexes with a cyclic urethane or carbonate framework in high yields. The reaction takes [...] Read more.

The carboxylation of unsaturated amine and alcohol compounds, including 4-benzylamino-1-phenyl-1-butyne (homopropargylamine), 2-butyne-1-ol (propargylic alcohol), and 2,3-butadiene-1-ol (allenylmethyl alcohol), using the hydroxidogold(I) complex, AuOH(IPr) [IPr = 1,3-bis(2,6-diisopropylphenyl)-imidazol-2-ylidene], produces corresponding alkenylgold(I) complexes with a cyclic urethane or carbonate framework in high yields. The reaction takes place in aprotic THF at room temperature under the atmospheric pressure of CO₂ in the absence of base additives. The products were characterized by NMR spectroscopy, elemental analysis, and X-ray crystallography. The functionalized alkenyl complexes prepared from the alkynes can be protonated by treatment with an equimolar amount of acetic acid to afford five- or six-membered carboxylation products, whereas the related alkenyl complex derived from allenylmethyl alcohol decomposed to recover the starting allene via ring-opening decarboxylation. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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18 pages, 3579 KiB

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Metal Complexes Containing Homoleptic Diorganoselenium(II) Ligands: Synthesis, Characterization and Investigation of Optical Properties

by Darius Dumitraș, Emese Gal, Cristian Silvestru and Alexandra Pop

Molecules 2024, 29(4), 792; https://doi.org/10.3390/molecules29040792 - 08 Feb 2024

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Abstract

[(Z)-2′-{2-C₆H₅-(4H)-oxazol-5-one}CHC₆H₄]₂Se (5, L¹) and [(Z)-4′-{2-C₆H₅-(4H)-oxazol-5-one}CHC₆H₄]₂Se (6, L [...] Read more.

[(Z)-2′-{2-C₆H₅-(4H)-oxazol-5-one}CHC₆H₄]₂Se (5, L¹) and [(Z)-4′-{2-C₆H₅-(4H)-oxazol-5-one}CHC₆H₄]₂Se (6, L²) were prepared, structurally characterized and used as ligands to obtain new metal complexes of types [MX(Lⁿ)] [L¹: M = Ag, X = OTf (7); M = Au, X = Cl (13); L²: M = Ag, X = OTf (8); M = Au, X = Cl (14)], [(MX)₂(Lⁿ)] [M = Ag, X = OTf, L¹ (9); L² (10)], [ZnCl₂(Lⁿ)] [L¹ (15); L² (16)] and [Ag(Lⁿ)][PF₆] [L¹ (11); L² (12)]. The silver complexes 7 and 8 were ionic species (1:1 electrolytes) in a MeCN solution, while in the solid state, the triflate fragments were bonded to the silver cations. Similarly, the 2:1 complexes 9 and 10 were found to behave as 1:2 electrolytes in a MeCN solution, but single-crystal X-ray diffraction demonstrated that compound 9 showed the formation of a dimer in the solid state: a tetranuclear [Ag(OTf)]₄ built through bridging triflate ligands was coordinated by two bridging organoselenium ligands through the nitrogen from the oxazolone ring and the selenium atoms in a 1κN:2κSe fashion. Supramolecular architectures supported by intermolecular C−H∙∙∙π, C−H∙∙∙O, Cl∙∙∙H and F∙∙∙H interactions were observed in compounds 4, 5 and 9. The compounds exhibited similar photophysical properties, with a bathochromic shift in the UV-Vis spectra caused by the position of the oxazolone ring on the phenyl ring attached to the selenium atoms. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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15 pages, 2985 KiB

Open AccessArticle

New Stable Gallium(III) and Indium(III) Complexes with Thiosemicarbazone Ligands: A Biological Evaluation

by Lorenzo Verderi, Mirco Scaccaglia, Martina Rega, Cristina Bacci, Silvana Pinelli, Giorgio Pelosi and Franco Bisceglie

Molecules 2024, 29(2), 497; https://doi.org/10.3390/molecules29020497 - 19 Jan 2024

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Abstract

The aim of this work is to explore a new library of coordination compounds for medicinal applications. Gallium is known for its various applications in this field. Presently, indium is not particularly important in medicine, but it shares a lot of chemical traits [...] Read more.

The aim of this work is to explore a new library of coordination compounds for medicinal applications. Gallium is known for its various applications in this field. Presently, indium is not particularly important in medicine, but it shares a lot of chemical traits with its above-mentioned lighter companion, gallium, and is also used in radio imaging. These metals are combined with thiosemicarbazones, ligating compounds increasingly known for their biological and pharmaceutical applications. In particular, the few ligands chosen to interact with these hard metal ions share the ideal affinity for a high charge density. Therefore, in this work we describe the synthesis and the characterization of the resulting coordination compounds. The yields of the reactions vary from a minimum of 21% to a maximum of 82%, using a fast and easy procedure. Nuclear Magnetic Resonance (NMR) and Infra Red (IR) spectroscopy, mass spectrometry, elemental analysis, and X-ray Diffraction (XRD) confirm the formation of stable compounds in all cases and a ligand-to-metal 2:1 stoichiometry with both cations. In addition, we further investigated their chemical and biological characteristics, via UV-visible titrations, stability tests, and cytotoxicity and antibiotic assays. The results confirm a strong stability in all explored conditions, which suggests that these compounds are more suitable for radio imaging applications rather than for antitumoral or antimicrobic ones. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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16 pages, 3688 KiB

Open AccessArticle

Aluminium 8-Hydroxyquinolinate N-Oxide as a Precursor to Heterometallic Aluminium–Lanthanide Complexes

by Elisa Gallo, Luca Bellucci, Silvia Carlotto, Gregorio Bottaro, Luca Babetto, Luca Giordano, Fabio Marchetti, Simona Samaritani, Lidia Armelao and Luca Labella

Molecules 2024, 29(2), 451; https://doi.org/10.3390/molecules29020451 - 17 Jan 2024

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Abstract

A reaction in anhydrous toluene between the formally unsaturated fragment [Ln(hfac)₃] (Ln³⁺ = Eu³⁺, Gd³⁺ and Er³⁺; Hhfac = hexafluoroacetylacetone) and [Al(qNO)₃] (HqNO = 8-hydroxyquinoline N-oxide), here prepared for the first time [...] Read more.

A reaction in anhydrous toluene between the formally unsaturated fragment [Ln(hfac)₃] (Ln³⁺ = Eu³⁺, Gd³⁺ and Er³⁺; Hhfac = hexafluoroacetylacetone) and [Al(qNO)₃] (HqNO = 8-hydroxyquinoline N-oxide), here prepared for the first time from [Al(O^tBu)₃] and HqNO, affords the dinuclear heterometallic compounds [Ln(hfac)₃Al(qNO)₃] (Ln³⁺ = Eu³⁺, Gd³⁺ and Er³⁺) in high yields. The molecular structures of these new compounds revealed a dinuclear species with three phenolic oxygen atoms bridging the two metal atoms. While the europium and gadolinium complexes show the coordination number (CN) 9 for the lanthanide centre, in the complex featuring the smaller erbium ion, only two oxygens bridge the two metal atoms for a resulting CN of 8. The reaction of [Eu(hfac)₃] with [Alq₃] (Hq = 8-hydroxyquinoline) in the same conditions yields a heterometallic product of composition [Eu(hfac)₃Alq₃]. A recrystallization attempt from hot heptane in air produced single crystals of two different morphologies and compositions: [Eu₂(hfac)₆Al₂q₄(OH)₂] and [Eu₂(hfac)₆(µ-Hq)₂]. The latter compound can be directly prepared from [Eu(hfac)₃] and Hq at room temperature. Quantum mechanical calculations confirm (i) the higher stability of [Eu(hfac)₃Al(qNO)₃] vs. the corresponding [Eu(hfac)₃Alq₃] and (ii) the preference of the Er complexes for the CN 8, justifying the different behaviour in terms of the Lewis acidity of the metal centre. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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19 pages, 3055 KiB

Open AccessArticle

Photocatalytic Reduction of CO₂ into CO with Cyclometalated Pt(II) Complexes of N^C^N Pincer Dipyridylbenzene Ligands: A DFT Study

by Antonia Sarantou and Athanassios Tsipis

Molecules 2024, 29(2), 403; https://doi.org/10.3390/molecules29020403 - 14 Jan 2024

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Abstract

In this work, density functional theory (DFT) calculations were employed to study the photocatalytic reduction of CO₂ into CO using a series of Pt(II) square planar complexes with the general formula [Pt(5-R-dpb)Cl] (dpb = 1,3-di(2-pyridyl)benzene anion, R = H, N,N [...] Read more.

In this work, density functional theory (DFT) calculations were employed to study the photocatalytic reduction of CO₂ into CO using a series of Pt(II) square planar complexes with the general formula [Pt(5-R-dpb)Cl] (dpb = 1,3-di(2-pyridyl)benzene anion, R = H, N,N-dimethylaniline,T thiophene, diazaborinine). The CO₂-into-CO conversion process is thought to proceed via two main steps, namely the photocatalytic/reduction step and the main catalytic step. The simulated absorption spectra exhibit strong bands in the range 280–460 nm of the UV-Vis region. Reductive quenching of the T₁ state of the complexes under study is expected to be favorable since the calculated excited state redox potentials for the reaction with sacrificial electron donors are highly positive. The redox potentials reveal that the reductive quenching of the T₁ state, important to the overall process, could be modulated by suitable changes in the N^C^N pincer ligands. The CO₂ fixation and activation by the three coordinated Pt(II) catalytically active species are predicted to be favorable, with the Pt–CO₂ bond dissociation energies D₀ in the range of −36.9–−10.3 kcal/mol. The nature of the Pt–CO₂ bond of the Pt(II) square planar intermediates is complex, with covalent, hyperconjugative and H-bonding interactions prevailing over the repulsive electrostatic interactions. The main catalytic cycle is estimated to be a favorable exergonic process. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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13 pages, 3248 KiB

Open AccessArticle

{Gd^III₇} and {Gd^III₁₄} Cluster Formation Based on a Rhodamine 6G Ligand with a Magnetocaloric Effect

by Lin Miao, Cai-Ming Liu and Hui-Zhong Kou

Molecules 2024, 29(2), 389; https://doi.org/10.3390/molecules29020389 - 12 Jan 2024

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Abstract

Heptanuclear {Gd^III₇} (complex 1) and tetradecanuclear {Gd^III₁₄} (complex 2) were synthesized using the rhodamine 6G ligand HL (rhodamine 6G salicylaldehyde hydrazone) and characterized. Complex 1 has a rare disc-shaped structure, where the central Gd ion [...] Read more.

Heptanuclear {Gd^III₇} (complex 1) and tetradecanuclear {Gd^III₁₄} (complex 2) were synthesized using the rhodamine 6G ligand HL (rhodamine 6G salicylaldehyde hydrazone) and characterized. Complex 1 has a rare disc-shaped structure, where the central Gd ion is connected to the six peripheral Gd^III ions via CH₃O⁻/μ₃-OH⁻ bridges. Complex 2 has an unexpected three-layer double sandwich structure with a rare μ₆-O²⁻ ion in the center of the cluster. Magnetic studies revealed that complex 1 exhibits a magnetic entropy change of 17.4 J kg⁻¹ K⁻¹ at 3 K and 5 T. On the other hand, complex 2 shows a higher magnetic entropy change of 22.3 J kg⁻¹ K⁻¹ at 2 K and 5 T. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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13 pages, 1490 KiB

Open AccessArticle

Cd²⁺-Selective Fluorescence Enhancement of Bisquinoline Derivatives with 2-Aminoethanol Skeleton

by Yuji Mikata, Aya Tsuruta, Hinata Koike, Sunao Shoji and Hideo Konno

Molecules 2024, 29(2), 369; https://doi.org/10.3390/molecules29020369 - 11 Jan 2024

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Abstract

The development of fluorescent Cd²⁺ sensors requires strict selectivity over Zn²⁺ because of the high availability of Zn²⁺ in the natural environment. In this paper, bisquinoline-based fluorescent sensors with a 2-aminoethanol backbone were investigated. The weak coordination ability of quinoline [...] Read more.

The development of fluorescent Cd²⁺ sensors requires strict selectivity over Zn²⁺ because of the high availability of Zn²⁺ in the natural environment. In this paper, bisquinoline-based fluorescent sensors with a 2-aminoethanol backbone were investigated. The weak coordination ability of quinoline compared to well-studied pyridine is suitable for Cd²⁺ selectivity rather than Zn²⁺. In the presence of 3 equiv. of metal ions, TriMeO-N,O-BQMAE (N,O-bis(5,6,7-trimethoxy-2-quinolylmethyl)-2-methylaminoethanol (3)), as well as its N,N-isomer TriMeO-N,N-BQMAE (N,N-bis(5,6,7-trimethoxy-2-quinolylmethyl)-2-methoxyethylamine (6)), exhibits Cd²⁺-selective fluorescence enhancement over Zn²⁺ in DMF-HEPES buffer (1:1, 50 mM HEPES, 0.1 M KCl, pH = 7.5) (I_Zn/I_Cd = 26–34%), which has similar selectivity in comparison to the corresponding ethylenediamine derivative TriMeOBQDMEN (N,N’-bis(5,6,7-trimethoxy-2-quinolylmethyl)-N,N’-dimethylethylenediamine) under the same experimental condition (I_Zn/I_Cd = 24%). The fluorescence mechanisms of N,O- and N,N-isomers of BQMAE are quite different, judging from the fluorescence lifetimes of their metal complexes. The Cd²⁺ complex with TriMeO-N,O-BQMAE (3) exhibits a long fluorescence lifetime similar to that of TriMeOBQDMEN via intramolecular excimer emission, whereas the Cd²⁺ complex with TriMeO-N,N-BQMAE (6) exhibits a short lifetime from monomer emission. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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13 pages, 2415 KiB

Open AccessArticle

A Pair of Multifunctional Cu(II)–Dy(III) Enantiomers with Zero–Field Single–Molecule Magnet Behaviors, Proton Conduction Properties and Magneto–Optical Faraday Effects

by Shui-Dong Zhu, Yu-Lin Zhou, Fang Liu, Yu Lei, Sui-Jun Liu, He-Rui Wen, Bin Shi, Shi-Yong Zhang, Cai-Ming Liu and Ying-Bing Lu

Molecules 2023, 28(22), 7506; https://doi.org/10.3390/molecules28227506 - 09 Nov 2023

Cited by 1 | Viewed by 837

Abstract

Multifunctional materials with a coexistence of proton conduction properties, single–molecule magnet (SMM) behaviors and magneto–optical Faraday effects have rarely been reported. Herein, a new pair of Cu(II)–Dy(III) enantiomers, [DyCu₂(RR/SS–H₂L)₂(H₂O)₄(NO₃) [...] Read more.

Multifunctional materials with a coexistence of proton conduction properties, single–molecule magnet (SMM) behaviors and magneto–optical Faraday effects have rarely been reported. Herein, a new pair of Cu(II)–Dy(III) enantiomers, [DyCu₂(RR/SS–H₂L)₂(H₂O)₄(NO₃)₂]·(NO₃)·(H₂O) (R–1 and S–1) (H₄L = [RR/SS] –N,N′–bis [3–hydroxysalicylidene] –1,2–cyclohexanediamine), has been designed and prepared using homochiral Schiff–base ligands. R–1 and S–1 contain linear Cu(II)–Dy(III)–Cu(II) trinuclear units and possess 1D stacking channels within their supramolecular networks. R–1 and S–1 display chiral optical activity and strong magneto–optical Faraday effects. Moreover, R–1 shows a zero–field SMM behavior. In addition, R–1 demonstrates humidity– and temperature–dependent proton conductivity with optimal values of 1.34 × 10⁻⁴ S·cm⁻¹ under 50 °C and 98% relative humidity (RH), which is related to a 1D extended H–bonded chain constructed by water molecules, nitrate and phenol groups of the RR–H₂L ligand. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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14 pages, 1573 KiB

Open AccessArticle

Antimicrobial Activity of Manganese(I) Tricarbonyl Complexes Bearing 1,2,3-Triazole Ligands

by Sofia Friães, Cândida Trigueiros, Clara S. B. Gomes, Alexandra R. Fernandes, Oscar A. Lenis-Rojas, Marta Martins and Beatriz Royo

Molecules 2023, 28(21), 7453; https://doi.org/10.3390/molecules28217453 - 06 Nov 2023

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Abstract

Background. Antimicrobial resistance is one of the most pressing health issues of our time. The increase in the number of antibiotic-resistant bacteria allied to the lack of new antibiotics has contributed to the current crisis. It has been predicted that if this situation [...] Read more.

Background. Antimicrobial resistance is one of the most pressing health issues of our time. The increase in the number of antibiotic-resistant bacteria allied to the lack of new antibiotics has contributed to the current crisis. It has been predicted that if this situation is not dealt with, we will be facing 10 million deaths due to multidrug resistant infections per year by 2050, surpassing cancer-related deaths. This alarming scenario has refocused attention into researching alternative drugs to treat multidrug-resistant infections. Aims. In this study, the antimicrobial activities of four manganese complexes containing 1,2,3,-triazole and clotrimazole ligands have been evaluated. It is known that azole antibiotics coordinated to manganese tricarbonyl complexes display interesting antimicrobial activities against several microbes. In this work, the effect of the introduction of 1,2,3,-triazole-derived ligands in the [Mn(CO)₃(clotrimazole)] fragment has been investigated against one Gram-positive bacterium and five Gram-negative bacteria. Methods. The initial antimicrobial activity of the above-mentioned complexes was assessed by determining the minimum inhibitory and bactericidal concentrations using the broth microdilution method. Growth curves in the presence and absence of the complexes were performed to determine the effects of these complexes on the growth of the selected bacteria. A possible impact on cellular viability was determined by conducting the MTS assay on human monocytes. Results. Three of the Mn complexes investigated (4–6) had good antimicrobial activities against all the bacteria tested, with values ranging from 1.79 to 61.95 µM with minimal toxicity. Conclusions. Due to the increased problem of antibiotic resistance and a lack of new antibacterial drugs with no toxicity, these results are exciting and show that these types of complexes can be an avenue to pursue in the future. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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15 pages, 2590 KiB

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A Norbornadiene-Based Molecular System for the Storage of Solar–Thermal Energy in an Aqueous Solution: Study of the Heat-Release Process Triggered by a Co(II)-Complex

by Franco Castro, Jorge S. Gancheff, Juan C. Ramos, Gustavo Seoane, Carla Bazzicalupi, Antonio Bianchi, Francesca Ridi and Matteo Savastano

Molecules 2023, 28(21), 7270; https://doi.org/10.3390/molecules28217270 - 25 Oct 2023

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Abstract

It is urgent yet challenging to develop new environmentally friendly and cost-effective sources of energy. Molecular solar thermal (MOST) systems for energy capture and storage are a promising option. With this in mind, we have prepared a new water-soluble (pH > 6) norbornadiene [...] Read more.

It is urgent yet challenging to develop new environmentally friendly and cost-effective sources of energy. Molecular solar thermal (MOST) systems for energy capture and storage are a promising option. With this in mind, we have prepared a new water-soluble (pH > 6) norbornadiene derivative (HNBD1) whose MOST properties are reported here. HNBD1 shows a better matching to the solar spectrum compared to unmodified norbornadiene, with an onset absorbance of λ_onset = 364 nm. The corresponding quadricyclane photoisomer (HQC1) is quantitatively generated through the light irradiation of HNBD1. In an alkaline aqueous solution, the MOST system consists of the NBD1⁻/QC1⁻ pair of deprotonated species. QC1⁻ is very stable toward thermal back-conversion to NBD1⁻; it is absolutely stable at 298 K for three months and shows a marked resistance to temperature increase (half-life t_½ = 587 h at 371 K). Yet, it rapidly (t_½ = 11 min) releases the stored energy in the presence of the Co(II) porphyrin catalyst Co-TPPC (ΔH_storage = 65(2) kJ∙mol⁻¹). Under the explored conditions, Co-TPPC maintains its catalytic activity for at least 200 turnovers. These results are very promising for the creation of MOST systems that work in water, a very interesting solvent for environmental sustainability, and offer a strong incentive to continue research towards this goal. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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26 pages, 9014 KiB

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Effects of Ferrocene and Ferrocenium on MCF-7 Breast Cancer Cells and Interconnection with Regulated Cell Death Pathways

by Cristina Favaron, Elisabetta Gabano, Ilaria Zanellato, Ludovica Gaiaschi, Claudio Casali, Maria Grazia Bottone and Mauro Ravera

Molecules 2023, 28(18), 6469; https://doi.org/10.3390/molecules28186469 - 06 Sep 2023

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Abstract

The effects of ferrocene (Fc) and ferrocenium (Fc⁺) induced in triple negative human breast cancer MCF-7 cells were explored by immunofluorescence, flow cytometry, and transmission electron microscopy analysis. The different abilities of Fc and Fc⁺ to produce [...] Read more.

The effects of ferrocene (Fc) and ferrocenium (Fc⁺) induced in triple negative human breast cancer MCF-7 cells were explored by immunofluorescence, flow cytometry, and transmission electron microscopy analysis. The different abilities of Fc and Fc⁺ to produce reactive oxygen species and induce oxidative stress were clearly observed by activating apoptosis and morphological changes after treatment, but also after tests performed on the model organism D. discoideum, particularly in the case of Fc⁺. The induction of ferroptosis, an iron-dependent form of regulated cell death driven by an overload of lipid peroxides in cellular membranes, occurred after 2 h of treatment with Fc⁺ but not Fc. However, the more stable Fc showed its effects by activating necroptosis after a longer-lasting treatment. The differences observed in terms of cell death mechanisms and timing may be due to rapid interconversion between the two oxidative forms of internalized iron species (from Fe²⁺ to Fe³⁺ and vice versa). Potential limitations include the fact that iron metabolism and mitophagy have not been investigated. However, the ability of both Fc and Fc⁺ to trigger different and interregulated types of cell death makes them suitable to potentially overcome the shortcomings of traditional apoptosis-mediated anticancer therapies. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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13 pages, 7623 KiB

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The Preparation of a Challenging Superconductor Nb₃Al by Exploiting Nano Effect

by Chengkai Luan, Xiyue Cheng, Xiuping Gao, Jürgen Köhler and Shuiquan Deng

Molecules 2023, 28(18), 6455; https://doi.org/10.3390/molecules28186455 - 06 Sep 2023

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Abstract

The Nb₃Al superconductor with excellent physical and working properties is one of the most promising materials in high-magnetic-field applications. However, it is difficult to prepare high-quality Nb₃Al with a desired superconducting transition temperature (T_c) because of [...] Read more.

The Nb₃Al superconductor with excellent physical and working properties is one of the most promising materials in high-magnetic-field applications. However, it is difficult to prepare high-quality Nb₃Al with a desired superconducting transition temperature (T_c) because of its narrow phase formation area at high temperatures (>1940 °C). This work reports a method to prepare stoichiometric Nb₃Al powder samples at a relatively low temperature (1400 °C) by exploiting the nano effect of Nb particles with pretreatment of Nb powder under H₂/Ar atmosphere. The obtained Nb₃Al samples exhibit high T_c’s of ~16.8K. Based on density functional theory (DFT) calculations and statistical mechanics analysis, the crucial role of quantum effect in leading to the success of the preparation method was studied. A new measure of surface energy (MSE) of a model particle is introduced to study its size and face dependence. A rapid convergence of the MSE with respect to the size indicates a quick approach to the solid limit, while the face dependence of MSE reveals a liquid-like behavior. The surface effect and quantum fluctuation of the Nb_n clusters explain the success of the preparation method. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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12 pages, 3362 KiB

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Terbium and Europium Chlorocyananilate-Based 2D Coordination Polymers

by Mariangela Oggianu, Alexandre Abhervé, Daniela Marongiu, Francesco Quochi, José Ramón Galán-Mascarós, Federica Bertolotti, Norberto Masciocchi, Narcis Avarvari and Maria Laura Mercuri

Molecules 2023, 28(18), 6453; https://doi.org/10.3390/molecules28186453 - 06 Sep 2023

Cited by 1 | Viewed by 803

Abstract

Two-dimensional layered coordination polymers based on the hetero-substituted 3-chloro-6-cyano-2,5-dihydroxybenzoquinone ligands, hereafter ClCNAn²⁻ anilate, and Ln^III ions (Tb and Eu) are reported. Compounds 1 and 2, formulated as Ln₂(ClCNAn)₃(DMSO)₆ (Ln^III = Tb, 1; Eu, [...] Read more.

Two-dimensional layered coordination polymers based on the hetero-substituted 3-chloro-6-cyano-2,5-dihydroxybenzoquinone ligands, hereafter ClCNAn²⁻ anilate, and Ln^III ions (Tb and Eu) are reported. Compounds 1 and 2, formulated as Ln₂(ClCNAn)₃(DMSO)₆ (Ln^III = Tb, 1; Eu, 2), and their related intermediates 1′ and 2′, formulated as Ln₂(ClCNAn)₃(H₂O)_x·yH₂O (x + y likely = 12, Ln = Tb, 1′; and Eu, 2′), were prepared by a conventional one-pot reaction (the latter) and recrystallized from DMSO solvent (the former). Polyhydrated intermediates 1′ and 2′ show very similar XRPD patterns, while, despite their common stoichiometry, 1 and 2 are not isostructural. Compound 1 consists of a 2D coordination framework of 3,6 topology, where [Tb(DMSO)₃]^III moieties are bridged by three bis-chelating ClCNAn²⁻ ligands, forming distorted hexagons. Ultrathin nanosheets of 1 were obtained by exfoliation via the liquid-assisted sonication method and characterized by atomic force microscopy, confirming the 2D nature of 1. The crystal structure of 2, still showing the presence of 2D sheets with a “hexagonal” mesh and a common (3,6) connectivity, is based onto flat, non-corrugated slabs. Indeed, at a larger scale, the different “rectangular tiles” show clear roofing in 1, which is totally absent in 2. The magnetic behavior of 1 very likely indicates depopulation of the highest crystal-field levels, as expected for Tb^III compounds. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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13 pages, 2159 KiB

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The Anti-Breast Cancer Stem Cell Potency of Copper(I)-Non-Steroidal Anti-Inflammatory Drug Complexes

by Alice Johnson, Xiao Feng, Kuldip Singh, Fabrizio Ortu and Kogularamanan Suntharalingam

Molecules 2023, 28(17), 6401; https://doi.org/10.3390/molecules28176401 - 01 Sep 2023

Cited by 1 | Viewed by 959

Abstract

Cancer stem cells (CSCs) are thought to be partly responsible for metastasis and cancer relapse. Currently, there are no effective therapeutic options that can remove CSCs at clinically safe doses. Here, we report the synthesis, characterisation, and anti-breast CSC properties of a series [...] Read more.

Cancer stem cells (CSCs) are thought to be partly responsible for metastasis and cancer relapse. Currently, there are no effective therapeutic options that can remove CSCs at clinically safe doses. Here, we report the synthesis, characterisation, and anti-breast CSC properties of a series of copper(I) complexes, comprising of non-steroidal anti-inflammatory drugs (NSAIDs) and triphenylphosphine ligands (1–3). The copper(I) complexes are able to reduce the viability of breast CSCs grown in two- and three-dimensional cultures at micromolar concentrations. The potency of the copper(I) complexes towards breast CSCs was similar to salinomycin (an established anti-breast CSC agent) and cisplatin (a clinically used metallopharmaceutical). Cell-based studies showed that the copper(I) complexes are readily, and similarly, internalised by breast CSCs. The copper(I) complexes significantly increase the intracellular reactive oxygen species (ROS) levels in breast CSCs, and their ROS generation profile with respect to time is dependent on the NSAID component present. The generation of intracellular ROS by the copper(I) complexes could be part of the underlying mechanism by which they evoke breast CSC death. As far as we are aware, this is the first study to explore the anti-breast CSC properties of copper(I) complexes. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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16 pages, 16575 KiB

Open AccessArticle

Aldiminium Cations as Countercations to Discrete Main Group Fluoroanions

by Evelin Gruden and Gašper Tavčar

Molecules 2023, 28(17), 6270; https://doi.org/10.3390/molecules28176270 - 27 Aug 2023

Viewed by 748

Abstract

The reactions of group 14 tetrafluorides (SiF₄, GeF₄, and SnF₄) and group 15 pentafluorides (PF₅, AsF₅, and SbF₅) with the CAAC-based trifluoride reagent [^MeCAACH][F(HF)₂] led to the [...] Read more.

The reactions of group 14 tetrafluorides (SiF₄, GeF₄, and SnF₄) and group 15 pentafluorides (PF₅, AsF₅, and SbF₅) with the CAAC-based trifluoride reagent [^MeCAACH][F(HF)₂] led to the isolation of salts containing discrete 5- or 6-coordinated fluoroanions. The syntheses of [^MeCAACH][SiF₅], [^MeCAACH][GeF₅], [^MeCAACH][(THF)SnF₅], and the structurally related [^MeCAACH][(dioxane)SnF₅], [^MeCAACH][PF₆], [^MeCAACH][AsF₆], and [^MeCAACH][SbF₆] are effective, selective and in high yield. All compounds were characterized by X-ray single-crystal structure analysis, NMR and Raman spectroscopy. It is worth noting that the synthesized [^MeCAACH][GeF₅] is a rare example of a structurally characterized compound with discrete [GeF₅]⁻ anion, while [^MeCAACH][(THF)SnF₅] and [^MeCAACH][(dioxane)SnF₅] represent the first compounds with discrete octahedrally coordinated tin fluoride anions with incorporated solvent molecules. Finally, the aldiminium-based cation [^MeCAACH]⁺ proved to be suitable for the stabilization of rare discrete main group fluoride anions. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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12 pages, 3578 KiB

Open AccessArticle

Observation of Two-Step Spin Transition in Graphene Oxide-Based Hybrids with Iron(II) 4-amino-1,2,4-triazole Spin Crossover Nanoparticles

by Nikolia Lalioti, Alexander Charitos, John Parthenios, Ondrej Malina, Michaela Polaskova, Martin Petr and Vassilis Tangoulis

Molecules 2023, 28(15), 5816; https://doi.org/10.3390/molecules28155816 - 02 Aug 2023

Viewed by 857

Abstract

A novel experimental protocol based on a reverse micellar method is presented for the synthesis of graphene oxide (GO)-based hybrids with spin crossover nanoparticles (SCO NPs) of the 1D iron(II) coordination polymer with the formula [Fe(NH₂trz)₃](Br₂). By [...] Read more.

A novel experimental protocol based on a reverse micellar method is presented for the synthesis of graphene oxide (GO)-based hybrids with spin crossover nanoparticles (SCO NPs) of the 1D iron(II) coordination polymer with the formula [Fe(NH₂trz)₃](Br₂). By introducing different quantities of 0.5% and 1.0% of GO (according to iron(II)) into the aqueous phase, two hybrids, NP4 and NP5, were synthesized, respectively. The morphological homogeneity of the NPs on the surface of the GO flakes is greatly improved in comparison to the pristine [Fe(NH₂trz)₃](Br₂) NPs. From the magnetic point of view and at a low magnetic sweep rate of 1 K/min, a two-step hysteretic behavior is observed for NP4 and NP5, where the onset of the low-temperature second step appeared at 40% and 30% of the HS fraction, respectively. For faster sweep rates of 5–10 K/min, the two steps from the cooling branch are progressively smeared out, and the critical temperatures observed are T_1/2

↑

= 343 K and T_1/2

↓

= 288 K, with a thermal width of 55 K for both NP4 and NP5. A Raman laser power-assisted protocol was used to monitor the thermal tolerance of the hybrids, while XPS analysis revealed electronic interactions between the SCO NPs and the GO flakes. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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31 pages, 94288 KiB

Open AccessArticle

Syntheses, Structures, and Corrosion Inhibition of Various Alkali Metal Carboxylate Complexes

by Vidushi P. Vithana, Zhifang Guo, Glen B. Deacon and Peter C. Junk

Molecules 2023, 28(14), 5515; https://doi.org/10.3390/molecules28145515 - 19 Jul 2023

Viewed by 1350

Abstract

Complexes of the alkali metals Li-Cs with 3-thiophenecarboxylate (3tpc), 2-methyl-3-furoate (2m3fur), 3-furoate (3fur), 4-hydroxycinnamate (4hocin), and 4-hydroxybenzoate (4hob) ions were prepared via neutralisation reactions, and the structures of [Li₂(3tpc)₂]_n (1Li); [K₂(3tpc)₂]_n [...] Read more.

Complexes of the alkali metals Li-Cs with 3-thiophenecarboxylate (3tpc), 2-methyl-3-furoate (2m3fur), 3-furoate (3fur), 4-hydroxycinnamate (4hocin), and 4-hydroxybenzoate (4hob) ions were prepared via neutralisation reactions, and the structures of [Li₂(3tpc)₂]_n (1Li); [K₂(3tpc)₂]_n (1K); [Rb(3tpc)(H₂O)]_n (1Rb); [Cs{H(3tpc)₂}]_n (1Cs); [Li₂(2m3fur)₂(H₂O)₃] (2Li); [K₂(2m3fur)₂(H₂O)]_n (2K); [Li(3fur)]_n(3Li); [K(4hocin](H₂O)₃]_n (4K); [Rb{H(4hocin)₂}]_n.nH₂O (4Rb); [Cs(4hocin)(H₂O)]_n (4Cs); [Li(4hob)]_n (5Li); [K(4hob)(H₂O)₃]_n (5K); [Rb(4hob)(H₂O)]_n (5Rb); and [Cs(4hob)(H₂O)]_n (5Cs) were determined via X-ray crystallography. Bulk products were also characterised via XPD, IR, and TGA measurements. No sodium derivatives could be obtained as crystallographically suitable single crystals. All were obtained as coordination polymers with a wide variety of carboxylate-binding modes, except for dinuclear 2Li. Under conditions that normally gave coordinated carboxylate ions, the ligation of hydrogen dicarboxylate ions was observed in 1Cs and 4Rb, with short H-bonds and short O…O distances associated with the acidic hydrogen. The alkali-metal carboxylates showed corrosion inhibitor properties inferior to those of the corresponding rare-earth carboxylates. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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17 pages, 15144 KiB

Open AccessArticle

Ge–Cu-Complexes Ph(pyO)Ge(μ²-pyO)₂CuCl and PhGe(μ²-pyO)₄CuCl—Representatives of Cu(I)→Ge(IV) and Cu(II)→Ge(IV) Dative Bond Systems

by Jörg Wagler and Robert Gericke

Molecules 2023, 28(14), 5442; https://doi.org/10.3390/molecules28145442 - 16 Jul 2023

Viewed by 966

Abstract

Phenylgermaniumpyridine-2-olate PhGe(pyO)₃ (compound 1Ge) and CuCl react with the formation of the heteronuclear complex Ph(pyO)Ge(μ²-pyO)₂CuCl (2Ge’) rather than forming the expected compound PhGe(μ²-pyO)₃CuCl (2Ge). Single-point calculations (at the B2T-PLYP [...] Read more.

Phenylgermaniumpyridine-2-olate PhGe(pyO)₃ (compound 1Ge) and CuCl react with the formation of the heteronuclear complex Ph(pyO)Ge(μ²-pyO)₂CuCl (2Ge’) rather than forming the expected compound PhGe(μ²-pyO)₃CuCl (2Ge). Single-point calculations (at the B2T-PLYP level) of the optimized molecular structures confirmed the relative stability of isomer 2Ge’ over 2Ge and, for the related silicon congeners, the relative stability of 2Si over 2Si’. Decomposition of a solution of 2Ge’ upon access to air provided access to some crystals of the copper(II) compound PhGe(μ²-pyO)₄CuCl (3Ge). Compounds 2Ge’ and 3Ge were characterized by single-crystal X-ray diffraction analyses, and the Ge–Cu bonds in these compounds were analyzed with the aid of quantum chemical calculations, e.g., Natural Bond Orbital analyses (NBO), Non-Covalent Interactions descriptor (NCI), and topology of the electron density at bond critical point using Quantum Theory of Atoms-In-Molecules (QTAIM) in conjunction with the related silicon compounds PhSi(μ²-pyO)₃CuCl (2Si), PhSi(μ²-pyO)₄CuCl (3Si), as well as the potential isomers Ph(pyO)Si(μ²-pyO)₂CuCl (2Si’) and PhGe(μ²-pyO)₃CuCl (2Ge). Pronounced Cu→Ge (over Cu→Si) lone pair donation was found for the Cu(I) compounds, whereas in Cu(II) compounds 3Si and 3Ge, this σ-donation is less pronounced and only marginally enhanced in 3Ge over 3Si. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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Review

Jump to: Research

38 pages, 19100 KiB

Open AccessReview

Polyanion Condensation in Inorganic and Hybrid Fluoridometallates (IV) of Octahedrally Coordinated Ti, Zr, Hf, V, Cr, W, Mn, Ge, Sn, and Pb

by Zoran Mazej

Molecules 2024, 29(6), 1361; https://doi.org/10.3390/molecules29061361 - 19 Mar 2024

Viewed by 556

Abstract

In fluorides, the M⁴⁺ cations of M = Ti, V, Cr, Mn, Ge, Sn, and Pb favour the octahedral coordination of six F ligands. Some examples of M⁴⁺ with larger cations (M = Zr, Hf, W) in octahedral coordination are also [...] Read more.

In fluorides, the M⁴⁺ cations of M = Ti, V, Cr, Mn, Ge, Sn, and Pb favour the octahedral coordination of six F ligands. Some examples of M⁴⁺ with larger cations (M = Zr, Hf, W) in octahedral coordination are also known. If not enough F ligands are available to have isolated M^IVF₆ octahedra, they must share their F ligands. The crystal structures of such fluoride metalates (IV) show the variety of possible structural motifs of the zero-dimensional oligomeric anions [M₂F₁₁]³⁻ (M = Ti, Cr), [M₃F₁₅]³⁻ (M = Zr, Hf), [M₃F₁₆]⁴⁻ (M = Ge), [M₄F₁₈]²⁻ (M = Ti, W), [M₄F₁₉]³⁻ (M = Ti), [M₄F₂₀]⁴⁻ (M = Ti), [M₅F₂₃]³⁻ (M = Ti), [M₆F₂₇]³⁻ (M = Ti), [M₆F₂₈]⁴⁻ (M = Ti), [M₈F₃₆]⁴⁻ (M = Ti, Mn), [M₁₀F₄₅]⁵⁻ (M = Ti) to one-dimensional chains ([MF₅]⁻)_∞ (M = V, Ti, Cr, Ge, Sn, Pb), double chains ([M₂F₉]⁻)_∞ (M = Ti, Mn), columns ([M₃F₁₃]⁻)_∞ (M = Ti), ([M₄F₁₉]³⁻)_∞ (M = Ti), ([M₇F₃₀]²⁻)_∞ (M = Ti), ([M₉F₃₈]²⁻)_∞) (M = Ti), two-dimensional layers ([M₂F₉]⁻)_∞ (M = Cr), ([M₈F₃₃]⁻)_∞ (M = Ti), and three-dimensional ([M₆F₂₇]³⁻)_∞ (M = Ti) architectures. A discrete monomeric [M₂F₉]⁻ anion with two M^IVF₆ octahedra sharing a common face has not yet been experimentally demonstrated, while two examples containing discrete dimeric [M₂F₁₀]²⁻ anions (M = Ti) with two M^IVF₆ octahedra sharing an edge are still in question. Full article

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18 pages, 7634 KiB

Open AccessReview

Biomedical Applications of Sulfonylcalix[4]arene-Based Metal–Organic Supercontainers

by Ya-Wen Fan, Meng-Xue Shi, Zhenqiang Wang, Feng-Rong Dai and Zhong-Ning Chen

Molecules 2024, 29(6), 1220; https://doi.org/10.3390/molecules29061220 - 08 Mar 2024

Viewed by 714

Abstract

Coordination cages sustained by metal–ligand interactions feature polyhedral architectures and well-defined hollow structures, which have attracted significant attention in recent years due to a variety of structure-guided promising applications. Sulfonylcalix[4]arenes-based coordination cages, termed metal–organic supercontainers (MOSCs), that possess unique multi-pore architectures containing an [...] Read more.

Coordination cages sustained by metal–ligand interactions feature polyhedral architectures and well-defined hollow structures, which have attracted significant attention in recent years due to a variety of structure-guided promising applications. Sulfonylcalix[4]arenes-based coordination cages, termed metal–organic supercontainers (MOSCs), that possess unique multi-pore architectures containing an endo cavity and multiple exo cavities, are emerging as a new family of coordination cages. The well-defined built-in multiple binding domains of MOSCs allow the efficient encapsulation of guest molecules, especially for drug delivery. Here, we critically discuss the design strategy, and, most importantly, the recent advances in research surrounding cavity-specified host–guest chemistry and biomedical applications of MOSCs. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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18 pages, 8970 KiB

Open AccessReview

Recent Progress on Perovskite-Based Electrocatalysts for Efficient CO₂ Reduction

by Tong Wu, Lihua Zhang, Yinbo Zhan, Yilin Dong, Zheng Tan, Bowei Zhou, Fei Wei, Dongliang Zhang and Xia Long

Molecules 2023, 28(24), 8154; https://doi.org/10.3390/molecules28248154 - 18 Dec 2023

Viewed by 1210

Abstract

An efficient carbon dioxide reduction reaction (CO₂RR), which reduces CO₂ to low-carbon fuels and high-value chemicals, is a promising approach for realizing the goal of carbon neutrality, for which effective but low-cost catalysts are critically important. Recently, many inorganic perovskite-based [...] Read more.

An efficient carbon dioxide reduction reaction (CO₂RR), which reduces CO₂ to low-carbon fuels and high-value chemicals, is a promising approach for realizing the goal of carbon neutrality, for which effective but low-cost catalysts are critically important. Recently, many inorganic perovskite-based materials with tunable chemical compositions have been applied in the electrochemical CO₂RR, which exhibited advanced catalytic performance. Therefore, a timely review of this progress, which has not been reported to date, is imperative. Herein, the physicochemical characteristics, fabrication methods and applications of inorganic perovskites and their derivatives in electrochemical CO₂RR are systematically reviewed, with emphasis on the structural evolution and product selectivity of these electrocatalysts. What is more, the current challenges and future directions of perovskite-based materials regarding efficient CO₂RR are proposed, to shed light on the further development of this prospective research area. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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16 pages, 4824 KiB

Open AccessReview

Chiral Metal Halide Perovskites: Focus on Lead-Free Materials and Structure-Property Correlations

by Clarissa Coccia, Marco Moroni and Lorenzo Malavasi

Molecules 2023, 28(16), 6166; https://doi.org/10.3390/molecules28166166 - 21 Aug 2023

Cited by 2 | Viewed by 1784

Abstract

Hybrid organic–inorganic perovskites (HOIPs) are promising materials in several fields related to electronics, offering long carrier-diffusion lengths, high absorption coefficients, tunable band gaps, and long spin lifetimes. Recently, chiral perovskites have attracted huge interest thanks to the possibility of further widening the applications [...] Read more.

Hybrid organic–inorganic perovskites (HOIPs) are promising materials in several fields related to electronics, offering long carrier-diffusion lengths, high absorption coefficients, tunable band gaps, and long spin lifetimes. Recently, chiral perovskites have attracted huge interest thanks to the possibility of further widening the applications of HOIPs. Chiral materials, being intrinsically non-centrosymmetric, display several attractive physicochemical properties, including circular dichroism, circularly polarized photoluminescence, nonlinear optics, ferroelectricity, and spin-related effects. Recent studies have shown that chirality can be transferred from the chiral organic ligands into the inorganic perovskite framework, resulting in materials combining the advantages of both chirality and perovskite superior optoelectronic characteristics. As for HOIPs for photovoltaics, strong interest is currently devoted towards the development of lead-free chiral perovskites to overcome any toxicity issue. While considering the basic and general features of chiral HOIPs, this review mainly focuses on lead-free materials. It highlights the first attempts to understand the correlation between the crystal structure characteristics and the chirality-induced functional properties in lead and lead-free chiral perovskites. Full article

(This article belongs to the Special Issue Exclusive Feature Papers in Inorganic Chemistry 2.0)

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