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Inorganic Chemistry

Yu Zhang, Basharat Ali, Jianfeng Wu, Mei Guo, Yang Yu, Zhiliang Liu, Jinkui Tang
The construction of metallosupramolecular complexes toward interesting topological structures is a critical challenge for chemists. The fluctuation in the synthetic strategy, by keeping the same metal-ligand combination, has proved a very significant approach to construct metallosupramolecular architectures. Herein, by varying the reaction conditions four new DyIII -supramolecular complexes based on a flexible dihydrazone ligand H2 L (H2 L = bis(2-hydroxy-3-methoxybenzylidene)adipohydrazide) in cooperation with different anions and solvents having formulas [Dy4 L4 (μ2 -N3 )2 ](NO3 )2 ·6CH3 OH·2H2 O (1), [Dy8 L8 (μ2 -CH3 OH)4 ]Cl8 ·6CH3 OH·14H2 O (2), [Dy12 L12 (μ2 -OH)2 (OH)6 (CH3 O)2 ](NO3 )2 ·2CH3 OH·14H2 O (3), and [Dy12 L12 (μ2 -OH)2 (NO3 )2 (OH)3 (CH3 O)](NO3 )4 ·22H2 O (4), have been successfully synthesized and their crystal structures confirmed by single crystal X-ray diffraction studies...
February 18, 2019: Inorganic Chemistry
Antoine Groué, Jean-Philippe Tranchier, Marie-Noelle Rager, Geoffrey Gontard, Marion Jean, Nicolas Vanthuyne, Harrison R Pearce, Andrew L Cooksy, Hani Amouri
A unique class of enantiopure N-heterocyclic carbene half-sandwich iridium complexes is reported. These compounds display stable configurations at the metal center, as demonstrated by their chiroptical properties. Remarkably, because of the nature of the naphthalimide molecule, two regioisomers containing five-membered [( R)-2a and ( S)-2a] and six-membered [( R)-2b and ( S)-2b] iridacycles were obtained. Density functional theory calculations are advanced to rationalize their relative stability.
February 18, 2019: Inorganic Chemistry
Anokhi Shah, Amandine Roux, Matthieu Starck, Jackie A Mosely, Michael Stevens, David G Norman, Robert I Hunter, Hassane El Mkami, Graham M Smith, David Parker, Janet E Lovett
The design, synthesis, and application of a nine-coordinate gadolinium(III)-containing spin label, [Gd.sTPATCN]-SL, for use in nanometer-distance measurement experiments by EPR spectroscopy is presented. The spin label links to cysteines via a short thioether tether and has a narrow central transition indicative of small zero-field splitting (ZFS). A protein homodimer, TRIM25cc, was selectively labeled with [Gd.sTPATCN]-SL (70%) and a nitroxide (30%) under mild conditions and measured using the double electron electron resonance (DEER) technique with both commercial Q-band and home-built W-band spectrometers...
February 18, 2019: Inorganic Chemistry
Vijay Gupta, Sanjay K Mandal
Using achiral components, a V-shaped dicarboxylic acid (H2 L) and a conformationally flexible bidentate linker (bpp), a thermally stable chiral metal organic framework {[Cd(bpp)(L)(H2 O)]·DMF} n (1), where H2 L = 4,4'-(dimethylsilanediyl)bis-benzoic acid, bpp = 1,3-bis(4-pyridyl)propane and DMF = N,N-dimethylformamide, has been solvothermally synthesized and crystallographically characterized. It consists of 1D helical chains linked at the cadmium centers resulting in an overall 2D framework. Its microporous nature was confirmed by gas-sorption measurements...
February 18, 2019: Inorganic Chemistry
Luca Gregori, Diego Sorbelli, Leonardo Belpassi, Francesco Tarantelli, Paola Belanzoni
A quantitative assessment of the Dewar-Chatt-Duncanson components of the Au(III)-alkyne bond in a series of cationic and dicationic bis- and monocyclometalated gold(III) complexes with 2-butyne via charge-displacement (CD) analysis is reported. Bonding between Au(III) and 2-butyne invariably shows a dominant σ donation component, a smaller, but significant, π back-donation, and a remarkable polarization of the alkyne CC triple bond toward the metal fragment. A very large net electron charge transfer from CC triple bond to the metal fragment results, which turns out to be unexpectedly insensitive to the charge of the complex and more strictly related to the nature of the ancillary ligand...
February 18, 2019: Inorganic Chemistry
Lizandra L L S Melo, Gerson P Castro, Simone M C Gonçalves
A luminescence quantum yield of 7.8% was obtained for a quaternary mixed-ligand samarium complex; this value is higher than those previously reported in the literature for such complexes in solution. The complex was prepared by microwave-assisted synthesis in 15 min with a yield of 69%; that is, ∼400 times faster than the usual synthesis that required 4 days and led to a yield of only 30%. Therefore, we propose microwave-assisted synthesis as the method of choice for preparing mixed-ligand lanthanoid complexes...
February 18, 2019: Inorganic Chemistry
Xiaonan Gao, Ai-Yun Fu, Bo Liu, Jun-Cheng Jin, Long-Tao Dou, Li-Xia Chen
The reactions of 2-(4-pyridyl) thiazole-4-carboxylic acid (Hptca) and CuCl2 ·6H2 O have led to a novel 3D mixed-valence, four-copper-center, metal-organic framework (MOF) [Cu8 Cl2 (ptca)10 ·17H2 O] n (1). The topology analysis using ToposPro software package for 1 resulted in three chain-based topology types of sra (42 , 63 , 8), pcu (412 , 63 ), and dia (66 ) via choosing corresponding connection atoms as central atoms. The study indicates that connection atoms associated directly with multiple coordination centers are applicable to act as central atoms...
February 15, 2019: Inorganic Chemistry
Cong Wang, Yang-Hui Luo, Xiao-Tong He, Dan-Li Hong, Jia-Ying Wang, Fang-Hui Chen, Chen Chen, Bai-Wang Sun
The design and preparation of a porous high-valence metal-organic framework (MOF) featuring open coordination sites are of utmost importance for the development of adsorbent materials. Here in this work, the three-dimensional (3D) high-valence MOF [Er(dcbp)3/2 (DMF)(H2 O)2 ]·2H2 O (HV-MOF-1; H2 dcbp = 4,4'-dicarboxy-2,2'-bipyridine, DMF = N,N-dimethylformamide), which possesses permanent porosity and two open coordination sites, has been prepared and characterized. In the 3D framework, the dcbp molecules display two different bridging styles, resulting in ordered diamondlike pores with bared carboxyl oxygen and pyridine nitrogen atoms on dcbp exposed directly to the pores, generating hydrophilic characteristics and high water affinity...
February 15, 2019: Inorganic Chemistry
Alexei A Belik, Lei Zhang, Ran Liu, Dmitry D Khalyavin, Yoshio Katsuya, Masahiko Tanaka, Kazunari Yamaura
Sm2 MnMn(Mn4- x Ti x )O12 with 1 ≤ x ≤ 3 were prepared by a high-pressure, high-temperature method at 6 GPa and about 1570-1670 K. They belong to a family of A-site columnar-ordered quadruple perovskites A2 A'A″B4 O12 , where A' is a site with a square-planar coordination and A″ is a site with a tetrahedral coordination. Their crystal structures were investigated using synchrotron X-ray and neutron powder diffraction. They crystallize in space group P42 / nmc (No. 137) with a = 7.41172 Å and c = 7...
February 15, 2019: Inorganic Chemistry
Yanying Zhao, Fan Yu, Caixia Wang, Zhaoman Zhou
Understanding the mechanisms of methane activation is an important and active research area of the contemporary catalyzed conversion of hydrocarbons to shippable, valuable feedstock and has invoked close collaborations between experimentalists and theorists. This article describes the trapping of reaction intermediates in a copper-catalyzed direct methane-to-methanol conversion. Specifically, two hydroxy(methoxy)copper(I) [CH3 OCu(OH)] isomeric intermediates were distinguished and characterized by matrix isolation infrared spectroscopy and 18 O2 , CD4 , and 13 CH4 isotopic substitution experiments combined with quantum chemical calculations...
February 15, 2019: Inorganic Chemistry
Jia Wen, Kui Yang, Xingcheng Ding, Hongjuan Li, Yongqian Xu, Fengyu Liu, Shiguo Sun
A folic acid (FA) functional drug delivery system (MT@L-PTX@FA) based on in situ formation of tellurium nanodots (Te NDs) in paclitaxel (PTX)-loaded MgAl layered double hydroxide (LDHs) gated mesoporous silica nanoparticles (MSNs) has been designed and fabricated for targeted chemo/PDT/PTT trimode combinatorial therapy. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), N2 adsorption-desorption, Fourier transform infrared (FT-IR) spectra, and UV-vis spectra were used to demonstrate the successful fabrication of MT@L-PTX@FA...
February 15, 2019: Inorganic Chemistry
Senkuttuvan Rajendiran, Vinothkumar Ganesan, Sungho Yoon
The synthesis of a unique heterogeneous catalyst that combines the functionality of a homogeneous catalyst and the advantages of a heterogeneous catalytic process is a continuing goal in various industrially applicable reactions. Here, we report heterogenization of homogeneous catalyst for lactone production from epoxide carbonylation through a facile polymerization using Friedel-Crafts reaction. A correlation between reactivity and degree of heterogeneity has been deduced by synthesizing different sized polymeric catalysts...
February 15, 2019: Inorganic Chemistry
Michael D Turlington, Ludovic Troian-Gautier, Renato N Sampaio, Evan E Beauvilliers, Gerald J Meyer
Ground- and excited-state control of halide supramolecular assembly was achieved through the preparation of a series of ester- and amide-functionalized ruthenium polypyridyl complexes in CH2 Cl2 . Hydrogen-bonding amide and alcohol groups on the receptor ligand were found to direct interactions with halide, while halide association with the ethyl ester groups was not observed. The various functional groups on the receptor ligands tuned the ground-state equilibrium constants over 2 orders of magnitude (1 × 105 to 1 × 107 M-1 ), and the fractional contribution of each hydrogen-bond donor to the total equilibrium constant was determined...
February 15, 2019: Inorganic Chemistry
Philip I Richards, Gavin T Lawson, Jamie F Bickley, Craig M Robertson, Jonathan A Iggo, Alexander Steiner
Trimethylaluminum finds widespread applications in chemical and materials synthesis, most prominently in its partially hydrolyzed form of methylalumoxane (MAO), which is used as a cocatalyst in the polymerization of olefins. This work investigates the sequential reactions of trimethylaluminum with hexaprotic phosphazenes (RNH)6 P3 N3 (=XH6 ) equipped with substituents R of varied steric bulk including tert-butyl (1H6 ), cyclohexyl (2H6 ), isopropyl (3H6 ), isobutyl (4H6 ), ethyl (5H6 ), propyl (6H6 ), methyl (7H6 ), and benzyl (8H6 )...
February 15, 2019: Inorganic Chemistry
Vanessa Proust, Renaud Jeannin, Frankie D White, Thomas E Albrecht-Schmitt
Perovskite ceramics have been extensively studied as host matrixes for radionuclide entrapment for nuclear waste disposal. As an expansion of these investigations, cerium, neodymium, and plutonium were incorporated into a perovskite phase, ACu3 FeTi3 O12 (A = Nd, Ce, Pu), using sol-gel methods under oxidizing and reducing atmospheres. The targeted materials contained varying levels of Ce3+ and Nd3+ on the A site, yielding potential compositions of Nd1- x Ce x Cu3 FeTi3 O12 ( x = 0, 0.1, 0.2, 0.3, 0.4, 0.8)...
February 15, 2019: Inorganic Chemistry
Sanghamitra Das, Vasudevan Subramaniyan, Ganesan Mani
Unsymmetrical pincers have been shown to be better than the corresponding symmetrical pincers in several catalysis reactions. A new unsymmetrical PNN propincer, 2-(3,5-dimethylpyrazolylmethyl)-5-(diphenylphosphinomethyl)pyrrole (1), was synthesized from pyrrole through Mannich bases in a good yield. In addition, the new byproduct 2-(3,5-dimethylpyrazolylmethyl)-5-(dimethylaminomethyl)- N-(hydroxymethyl)pyrrole was also isolated. The reaction of 1 with [PdCl2 (PhCN)2 ] and Et3 N in toluene yielded [PdCl{C4 H2 N-2-(CH2 Me2 pz)-5-(CH2 PPh2 )-κ3 P,N,N}] (2)...
February 15, 2019: Inorganic Chemistry
Manila Sharma, Aymen Yangui, Vincent R Whiteside, Ian R Sellers, Dan Han, Shiyou Chen, Mao-Hua Du, Bayrammurad Saparov
Replacement of the toxic heavy element lead in metal halide perovskites has been attracting a great interest because the high toxicity and poor air stability are two of the major barriers for their widespread utilization. Recently, mixed-cation double perovskite halides, also known as elpasolites, were proposed as an alternative lead-free candidate for the design of nontoxic perovskite solar cells. Herein, we report a new nontoxic and air stable lead-free all-inorganic semiconductor Rb4 Ag2 BiBr9 prepared using the mixed-cation approach; however, Rb4 Ag2 BiBr9 adopts a new structure type (Pearson's code oP32) featuring BiBr6 octahedra and AgBr5 square pyramids that share common edges and corners to form a unique 2D layered non-perovskite structure...
February 15, 2019: Inorganic Chemistry
Jongwook W Heo, Munseok S Chae, Jooeun Hyoung, Seung-Tae Hong
Rhombohedral potassium-zinc hexacyanoferrate K1.88 Zn2.88 [Fe(CN)6 ]2 (H2 O)5 (KZnHCF) synthesized using a precipitation method is demonstrated as a high-voltage cathode material for potassium-ion batteries (PIBs), exhibiting an initial discharge capacity of 55.6 mAh g-1 with a discharge voltage of 3.9 V versus K/K+ and a capacity retention of ∼95% after 100 cycles in a nonaqueous electrolyte. All K ions are extracted from the structure upon the initial charge process. However, only 1.61 out of 1.88 K ions per formula unit are inserted back into the structure upon discharge, and it becomes the reversible ion of the second cycle onward...
February 15, 2019: Inorganic Chemistry
Christian Reichardt, Susan Monro, Fabian H Sobotta, Katsuya L Colón, Tariq Sainuddin, Mat Stephenson, Eric Sampson, John Roque, Huimin Yin, Johannes C Brendel, Colin G Cameron, Sherri McFarland, Benjamin Dietzek
This study investigates the correlation between photocytotoxicity and the prolonged excited-state lifetimes exhibited by certain Ru(II) polypyridyl photosensitizers comprised of π-expansive ligands. The eight metal complexes selected for this study differ markedly in their triplet state configurations and lifetimes. Human melanoma SKMEL28 and human leukemia HL60 cells were used as in vitro models to test photocytotoxicity induced by the compounds when activated by either broadband visible or monochromatic red light...
February 14, 2019: Inorganic Chemistry
Tim P Seifert, Johannes Klein, Michael T Gamer, Nicolai D Knöfel, Thomas J Feuerstein, Biprajit Sarkar, Peter W Roesky
Ethynylferrocene (FcC≡CH) was utilized as a redox-active metalloligand for the synthesis of polynuclear coinage metal complexes. The reaction of [FcC≡CLi] with tri- tert-butylphosphine metal chlorides [t Bu3 P-MCl] (M = Au, Ag, Cu) yielded different heteronuclear ferrocene-funtionalized alkyne complexes featuring metallophilic interactions. Furthermore, the redox properties of the ferrocenyl-functionalized tetracopper complex were investigated by cyclic voltammetry and UV-vis-near-IR spectroelectrochemistry...
February 14, 2019: Inorganic Chemistry
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