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Inorganics, Volume 9, Issue 10 (October 2021) – 5 articles

Cover Story (view full-size image): A sterically hindered spirogermabifluorene was successfully synthesized via the reaction of a dilithiated 3,3’,5,5’-tetra-t-butylbiphenyl ligand with an equimolar amount of GeCl2·(dioxane). Theoretical calculations suggested that the spirogermabifluorene would be generated by the biphenyl-migration from the 5H-dibenzogermole-5-ylidene dimer initially generated in situ, along with the elimination of Ge(0). Its solid-state structure and redox behavior were examined by single-crystal X-ray diffraction analysis and electrochemical measurements, respectively. The sterically hindered biphenyl ligands endow the spirogermabifluorene with high redox stability and increased electron affinity. We believe that several families of spirogermabifluorenes can be accessed using the synthetic methodology described in this paper, which may lead to new applications of spirogermabifluorenes on account of [...] Read more.
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Article
Nanostructure and Luminescent Properties of Bimetallic Lanthanide Eu/Gd, Tb/Gd and Eu/Tb Coordination Polymers
Inorganics 2021, 9(10), 77; https://0-doi-org.brum.beds.ac.uk/10.3390/inorganics9100077 - 15 Oct 2021
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Abstract
This study presents the synthesis, structural and luminescence properties for lanthanide metal–organic frameworks (LnMOFs), which belong to the sub-class of coordination polymers. The series of nanosized LnMOFs (Ln = Eu, Gd, Tb, Eu0.5Gd0.5, Tb0.5Gd0.5 and Eu [...] Read more.
This study presents the synthesis, structural and luminescence properties for lanthanide metal–organic frameworks (LnMOFs), which belong to the sub-class of coordination polymers. The series of nanosized LnMOFs (Ln = Eu, Gd, Tb, Eu0.5Gd0.5, Tb0.5Gd0.5 and Eu0.5Tb0.5) was prepared by solvothermal synthesis using a modulator (sodium acetate). We investigated the various surface chemistry compositions of the isostructural LnMOFs with a [Ln(btc)] structure (BTC: Benzene-1,3,5-tricarboxylate) by X-ray photoelectron spectroscopy (XPS). The XPS confirmed the mixed-valent Eu3+ and Eu2+ compounds, and the presence of Tb in both +3 and +4 valence states, and one +3 valency of Gd. A nanostructure of mixed LnMOFs (EuGd, TbGd and EuTb) with a rod-like shape is related to luminescence properties. The MOFs (EuTb and EuGd) presented Comission Internationale de l’Éclairage (CIE) chromaticities of x = 0.666 and y = 0.331, and x = 0.654 and y = 0.348, respectively, in the red region. They were better than the values desired for use in commercial phosphors, which are x = 0.64 and y = 0.35. For [Tb/Gd(btc)], the CIE coordinates were x = 0.334 and y = 0.562, presenting emissions in the green region. Bimetallic LnMOFs are very promising UV light sensors for biological applications. Full article
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Article
Synthesis of N,O-Chelating Hydrazidopalladium Complexes from 1,2-Bis(trifluoroacetyl)hydrazine
Inorganics 2021, 9(10), 76; https://0-doi-org.brum.beds.ac.uk/10.3390/inorganics9100076 - 07 Oct 2021
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Abstract
N,O-chelating dicarbonylhydrazido-palladium complexes were synthesized by treatment of 1,2-bis(trifluoroacetyl)hydrazine with a mixture of a Pd(0) source, [Pd(dba)2] (DBA = dibenzylideneacetone), and four-electron donors including 1,3-bis(diphenylphosphino)propane (DPPP), N,N,N’,N’-tetramethylethylenediamine (TMEDA), and two equivalents [...] Read more.
N,O-chelating dicarbonylhydrazido-palladium complexes were synthesized by treatment of 1,2-bis(trifluoroacetyl)hydrazine with a mixture of a Pd(0) source, [Pd(dba)2] (DBA = dibenzylideneacetone), and four-electron donors including 1,3-bis(diphenylphosphino)propane (DPPP), N,N,N’,N’-tetramethylethylenediamine (TMEDA), and two equivalents of triphenylphosphine. The same products from DPPP and TMEDA could be obtained alternatively by using Pd(OAc)2 through deprotonation of the diacylhydrazine. The five-membered chelate structure was confirmed by NMR spectra and X-ray crystal structure determination. The X-ray structures indicate that the products are formally considered as Pd(II) complexes with a hydrazido(2–) ligand. In the case of the triphenylphosphine-coordinated complex, a fluxional behavior in dichloromethane-d2 was observed by variable temperature NMR experiments, possibly due to structural changes between the square planar and pseudo-tetrahedral geometries. Full article
(This article belongs to the Section Organometallic Chemistry)
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Article
Facile Synthesis and Redox Behavior of an Overcrowded Spirogermabifluorene
Inorganics 2021, 9(10), 75; https://0-doi-org.brum.beds.ac.uk/10.3390/inorganics9100075 - 06 Oct 2021
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Abstract
A spirogermabifluorene that bears sterically demanding 3,3′,5,5′-tetra(t-butyl)-2,2′-biphenylene groups (1) was obtained from the reaction of in-situ-generated 2,2′-dilithiobiphenylene with GeCl2·(dioxane). The solid-state structure and the redox behavior of 1 were examined by single-crystal X-ray diffraction analysis and electrochemical [...] Read more.
A spirogermabifluorene that bears sterically demanding 3,3′,5,5′-tetra(t-butyl)-2,2′-biphenylene groups (1) was obtained from the reaction of in-situ-generated 2,2′-dilithiobiphenylene with GeCl2·(dioxane). The solid-state structure and the redox behavior of 1 were examined by single-crystal X-ray diffraction analysis and electrochemical measurements, respectively. The sterically hindered biphenyl ligands endow 1 with high redox stability and increased electron affinity. The experimental observations were corroborated by theoretical DFT calculations. Full article
(This article belongs to the Special Issue Redox-Active Ligand Complexes)
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Article
Diverse Coordination Numbers and Geometries in Pyridyl Adducts of Lanthanide(III) Complexes Based on β-Diketonate
Inorganics 2021, 9(10), 74; https://0-doi-org.brum.beds.ac.uk/10.3390/inorganics9100074 - 30 Sep 2021
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Abstract
Ten mononuclear rare earth complexes of formula [La(btfa)3(H2O)2] (1), [La(btfa)3(4,4′-Mt2bipy)] (2), [La(btfa)3(4,4′-Me2bipy)2] (3), [La(btfa)3(5,5′-Me2bipy)2] ( [...] Read more.
Ten mononuclear rare earth complexes of formula [La(btfa)3(H2O)2] (1), [La(btfa)3(4,4′-Mt2bipy)] (2), [La(btfa)3(4,4′-Me2bipy)2] (3), [La(btfa)3(5,5′-Me2bipy)2] (4), [La(btfa)3(terpy)] (5), [La(btfa)3(phen)(EtOH)] (6), [La(btfa)3(4,4′-Me2bipy)(EtOH)] (7), [La(btfa)3(2-benzpy)(MeOH)] (8), [Tb(btfa)3(4,4′-Me2bipy)] (9) and (Hpy)[Eu(btfa)4] (10), where btfa = 4,4,4-trifuoro-1-phenylbutane-1,3-dionato anion, 4,4′-Mt2bipy = 4,4′-dimethoxy-2,2′-bipyridine, 4,4′-Me2bipy = 4,4′-dimethyl-2,2′-bipyridine, 5,5′-Me2bipy = 5,5′-dimethyl-2,2′-bipyridine, terpy = 2,2′:6′,2′-terpyridine, phen = 1,10-phenathroline, 2-benzpy = 2-(2-pyridyl)benzimidazole, Hpy = pyridiniumH+ cation) have been synthesized and structurally characterized. The complexes display coordination numbers (CN) eight for 1, 2, 9, 10, nine for 5, 6, 7, 8 and ten for 3 and 4. The solid-state luminescence spectra of Tb-9 and Eu-10 complexes showed the same characteristic bands predicted from the Tb(III) and Eu(III) ions. The Overall Quantum Yield measured (ϕTOT) at the excitation wavelength of 371 nm for both compounds yielded 1.04% for 9 and up to 34.56% for 10. Full article
(This article belongs to the Section Coordination Chemistry)
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Article
Vanadium(V) Complexes with Siderophore Vitamin E-Hydroxylamino-Triazine Ligands
Inorganics 2021, 9(10), 73; https://0-doi-org.brum.beds.ac.uk/10.3390/inorganics9100073 - 29 Sep 2021
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Abstract
Novel vitamin E chelate siderophore derivatives and their VV and FeIII complexes have been synthesised and the chemical and biological properties have been evaluated. In particular, the α- and δ-tocopherol derivatives with bis-methyldroxylamino triazine (α-tocTHMA) and (δ-tocDPA) as well their V [...] Read more.
Novel vitamin E chelate siderophore derivatives and their VV and FeIII complexes have been synthesised and the chemical and biological properties have been evaluated. In particular, the α- and δ-tocopherol derivatives with bis-methyldroxylamino triazine (α-tocTHMA) and (δ-tocDPA) as well their VV complexes, [V2VO3(α-tocTHMA)2] and [V2IVO3(δ-tocTHMA)2], have been synthesised and characterised by infrared (IR), nuclear magnetic resonance (NMR), electron paramagnetic resonance (EPR) and ultra violet-visible (UV-Vis) spectroscopies. The dimeric vanadium complexes in solution are in equilibrium with their respefrctive monomers, H2O + [V2VO2(μ-O)]4+ = 2 [VVO(OH)]2+. The two amphiphilic vanadium complexes exhibit enhanced hydrolytic stability. EPR shows that the complexes in lipophilic matrix are mild radical initiators. Evaluation of their biological activity shows that the compounds do not exhibit any significant cytotoxicity to cells. Full article
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