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Inorganics
Volume 7
Issue 12
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Inorganics, Volume 7, Issue 12 (December 2019) – 7 articles

Cover Story (view full-size image): Borosulfates are a rapidly expanding class of silicate analog materials. They are composed of vertex shared (BO4)- and (SO4)-tetrahedra, whereas borosulfates with cross-linking of the anionic network into two or even three dimensions are still very rare. We found that reactions between oleum enriched with 65% SO3 and boric acid in evacuated torch-sealed glass ampoules can be a powerful strategy to synthesize borosulfates with layer-like anionic substructures of divalent metals. The two new representatives Mn[B2(SO4)4] and Zn[B2(SO4)4] reveal alternating vierer- and zwölfer-rings of exclusively corner-linked (SO4)- and (BO4)-tetrahedra within the anionic layers. Both borosulfates are the first representatives with cations residing in the planes of the anionic networks. View this paper.
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9 pages, 1917 KiB  
Article
M[B2(SO4)4] (M = Mn, Zn)—Syntheses and Crystal Structures of Two New Phyllosilicate Analogue Borosulfates
by Leonard C. Pasqualini, Hubert Huppertz and Jörn Bruns
Inorganics 2019, 7(12), 145; https://doi.org/10.3390/inorganics7120145 - 17 Dec 2019
Cited by 11 | Viewed by 3579
Abstract
Borosulfates are a rapidly expanding class of silicate analogue materials, where the structural diversity is expected to be at least as large as known for silicates. However, borosulfates with cross-linking of the anionic network into two or even three dimensions are still very [...] Read more.
Borosulfates are a rapidly expanding class of silicate analogue materials, where the structural diversity is expected to be at least as large as known for silicates. However, borosulfates with cross-linking of the anionic network into two or even three dimensions are still very rare. Herein, we present two new representatives with phyllosilicate analogue topology. Through solvothermal reactions of ZnO and MnCl2∙4H2O with boric acid in oleum (65% SO3), we obtained single-crystals of Mn[B2(SO4)4] (monoclinic, P21/n, Z = 2, a = 8.0435(4), b = 7.9174(4), c = 9.3082(4) Å, β = 110.94(1)°, V = 553.63(5) Å3) and Zn[B2(SO4)4] (monoclinic, P21/n, Z = 2, a = 7.8338(4), b = 8.0967(4), c = 9.0399(4) Å, β = 111.26(1)°, V = 534.36(5) Å3). The crystal structures reveal layer-like anionic networks with alternating vierer- and zwölfer-rings formed exclusively by corner-linked (SO4)- and (BO4)-tetrahedra. Full article
(This article belongs to the Special Issue Oxido Compounds)
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16 pages, 4351 KiB  
Review
Thiazole- and Thiadiazole-Based Metal–Organic Frameworks and Coordination Polymers for Luminescent Applications
by Giorgio Mercuri, Giuliano Giambastiani and Andrea Rossin
Inorganics 2019, 7(12), 144; https://doi.org/10.3390/inorganics7120144 - 14 Dec 2019
Cited by 27 | Viewed by 5817
Abstract
This mini-review focuses on the 2015–2019 literature survey of thiazole- and thiadiazole-containing Metal–Organic Frameworks (MOFs) and Coordination Polymers (CPs) exploited in the applicative field of luminescent sensing. Full article
(This article belongs to the Special Issue Functional Coordination Polymers and Metal–Organic Frameworks)
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12 pages, 7787 KiB  
Article
High-Pressure Modification of BiI3
by Ulrich Schwarz, Aron Wosylus, Marcus Schmidt, Lev Akselrud, Alim Ormeci, Michael Hanfland, Volker Hermann and Christine Kuntscher
Inorganics 2019, 7(12), 143; https://doi.org/10.3390/inorganics7120143 - 13 Dec 2019
Cited by 5 | Viewed by 3484
Abstract
Structural and optical properties as well as chemical bonding of BiI3 at elevated pressures are investigated by means of refinements of X-ray powder diffraction data, measurements of the optical absorption, and calculations of the band structure involving bonding analysis in real space. [...] Read more.
Structural and optical properties as well as chemical bonding of BiI3 at elevated pressures are investigated by means of refinements of X-ray powder diffraction data, measurements of the optical absorption, and calculations of the band structure involving bonding analysis in real space. The data evidence the onset of a phase transition from trigonal (hR24) BiI3 into PuBr3-type (oS16) BiI3 around 4.6 GPa. This high-pressure modification remains stable up to 40 GPa, the highest pressure of this study. The phase exhibits semiconducting properties with constantly decreasing band gap between 5 and 18 GPa. Above this pressure, the absorbance edge broadens significantly. Extrapolation of the determined band gap values implies a semiconductor to metal transition at approximately 35 GPa. The value is in accordance with subtle structural anomalies and the results of band structure calculations. Topological analysis of the computed electron density and the electron-localizability indicator reveal fingerprints for weak covalent Bi-I contributions in addition to dominating ionic interactions for both modifications. Full article
(This article belongs to the Special Issue Structure, Properties, and Bonding in Solid State Compounds)
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10 pages, 695 KiB  
Article
Technetium Nitrido-Peroxo Complexes: An Unexplored Class of Coordination Compounds
by Micol Pasquali, Emilija Janevik-Ivanovska and Adriano Duatti
Inorganics 2019, 7(12), 142; https://doi.org/10.3390/inorganics7120142 - 11 Dec 2019
Cited by 1 | Viewed by 3153
Abstract
The purpose of this work was to further expand the chemistry of mixed technetium nitrido-peroxo complexes, a still poorly explored class of compounds containing the Tc(VII) moiety, [99gTc][Tc(N)(O2)2]. A number of novel complexes of the formula [ [...] Read more.
The purpose of this work was to further expand the chemistry of mixed technetium nitrido-peroxo complexes, a still poorly explored class of compounds containing the Tc(VII) moiety, [99gTc][Tc(N)(O2)2]. A number of novel complexes of the formula [99gTc][Tc(N)(O2)2(L)] with bidentate ligands (L) (where L = deprotonated alanine, glycine, proline) were prepared by reacting a solution of nitrido-technetic(VI) acid with L in the presence of a source of H2O2. Alternatively, the complex [99gTc][Tc(N)(O2)2X]− (X = Cl, Br) was used as a precursor for substitution reactions where the halogenide ion was replaced by the bidentate ligand. The new complexes were characterized by elemental analysis and mass spectroscopy. The preparation of the analogous [99mTc][Tc(N)(O2)2] moiety, radiolabeled with the metastable isomer Tc-99m, was also studied at a no-carrier-added level, using S-methyl-N-methyl-dithiocarbazate as the donor of the nitrido nitrogen atoms. Full article
(This article belongs to the Special Issue Advanced Applications of Technetium Chemistry)
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14 pages, 3028 KiB  
Article
Alkali-Activated Metakaolin as a Zeolite-Like Binder for the Production of Adsorbents
by Kristine Vegere, Laura Vitola, Pauls P. Argalis, Diana Bajare and Andrey E. Krauklis
Inorganics 2019, 7(12), 141; https://doi.org/10.3390/inorganics7120141 - 6 Dec 2019
Cited by 14 | Viewed by 3536
Abstract
This work reports and describes a novel alkali-activated metakaolin as a potential binder material for the granulation of zeolites, which are widely used as CO2 adsorbents. The alkali-activated binders are zeolite-like materials, resulting in good material compatibility with zeolite-based adsorbents. A major [...] Read more.
This work reports and describes a novel alkali-activated metakaolin as a potential binder material for the granulation of zeolites, which are widely used as CO2 adsorbents. The alkali-activated binders are zeolite-like materials, resulting in good material compatibility with zeolite-based adsorbents. A major problem during the granulation of zeolites is that their adsorption capacities decrease by about 15–20%, because typical binder materials (for example bentonite or kaolin clay) are inactive towards CO2 adsorption. A possible pathway to solve this problem is to introduce a novel binder that is also able to sorb CO2. In such a case, a binder plays a dual role, acting both as a binding material and as a sorbent. However, it is important that, alongside the adsorptive properties, a novel binder material must fulfil mechanical and morphological requirements. Thus, in this work, physical and mechanical properties of this novel binder for zeolite granulation for CO2 adsorption are studied. Alkali-activated metakaolin was found to be efficient and competitive as a binder material, when mechanical and physical properties were concerned. The compressive strengths of most of the obtained binders reported in this work are above the compressive strength threshold of 10 MPa. The future work on this novel binder will be conducted, which includes granulation-related details and the CO2 adsorptive properties of the novel binder material. Metakaolin was used as a precursor for alkali-activated binders. Binders were synthesized using varying molarity of a NaOH solution and at varying curing conditions. The final products were characterized using density measurements, compressive strength tests, X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), Brunauer–Emmett–Teller (BET) analysis, and scanning electron microscopy (SEM). Full article
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10 pages, 2952 KiB  
Communication
A PAlP Pincer Ligand Bearing a 2-Diphenylphosphinophenoxy Backbone
by Kazuhiko Semba, Ikuya Fujii and Yoshiaki Nakao
Inorganics 2019, 7(12), 140; https://doi.org/10.3390/inorganics7120140 - 28 Nov 2019
Cited by 18 | Viewed by 4230
Abstract
A PAlP pincer ligand derived from 2-diphenylphosphino-6-isopropylphenol was synthesized. The Lewis acidity of the Al center of the ligand was evaluated with coordination of (O)PEt3. A zwitterionic rhodium-aluminum heterobimetallic complex bearing the PAlP ligand was synthesized through its complexation with [RhCl(nbd)] [...] Read more.
A PAlP pincer ligand derived from 2-diphenylphosphino-6-isopropylphenol was synthesized. The Lewis acidity of the Al center of the ligand was evaluated with coordination of (O)PEt3. A zwitterionic rhodium-aluminum heterobimetallic complex bearing the PAlP ligand was synthesized through its complexation with [RhCl(nbd)]2. Moreover, reduction of the zwitterionic rhodium-aluminum complex with KC8 afforded heterobimetallic complexes bearing an X-type PAlP pincer ligand. Full article
(This article belongs to the Special Issue Organoaluminum Compounds)
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15 pages, 3476 KiB  
Review
Metal Hydride Compressors with Gas-Gap Heat Switches: Concept, Development, Testing, and Space Flight Operation for the Planck Sorption Cryocoolers
by Robert C. Bowman, Jr.
Inorganics 2019, 7(12), 139; https://doi.org/10.3390/inorganics7120139 - 21 Nov 2019
Cited by 19 | Viewed by 4328
Abstract
Two closed-cycle cryogenic refrigerators were used to generate temperatures of ~18 K via evaporation of liquid hydrogen at the interfaces with radiofrequency and infrared sensors on an Earth-orbiting spacecraft that measured the anisotropy of the cosmic microwave background (CMB) during the European Space [...] Read more.
Two closed-cycle cryogenic refrigerators were used to generate temperatures of ~18 K via evaporation of liquid hydrogen at the interfaces with radiofrequency and infrared sensors on an Earth-orbiting spacecraft that measured the anisotropy of the cosmic microwave background (CMB) during the European Space Agency (ESA) Planck Mission from June 2009 until October 2013. The liquid hydrogen phase was continuously generated in each Planck Sorption Cryocooler (PSC) by coupling a Joule–Thomson (J–T) expander to hydrogen gas initially pressurized to nominally 3000 kPa (i.e., ~30 bar) and subsequently discharged at pressure of 30 kPa (i.e., ~0.3 bar) by desorption and absorption using LaNi4.78Sn0.22Hx contained in six individual sorbent beds. The pressures were varied by alternately heating and cooling this hydride that included temperature modulation with an integrated Gas-Gap Heat Switch (GGHS). The novel GGHS used the low-pressure hydride ZrNiHx to vary thermal conductance between the bed containing the LaNi4.78Sn0.22Hx sorbent and the rest of the compressor system. The design features and development of these hydride components are described along with details of fabrication and assembly. The results obtained during extended laboratory testing are also summarized. The predictions from this preflight testing are compared to the performance observed while operating in orbit during the Planck Mission. This review ends with a summary of lessons learned and recommendations for improved systems. Full article
(This article belongs to the Special Issue Beyond Hydrogen Storage—Metal Hydrides as Multifunctional Materials for Energy Storage and Conversion)
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