Solid-state MAS NMR Spectroscopy Research Articles

Manual and automatic assignment of two different Aβ40 amyloid fibril polymorphs using MAS solid-state NMR spectroscopy

Amyloid fibrils from Alzheimer’s amyloid-beta peptides (Aβ) are found to be polymorphic. So far, 14 Aβ40 fibril structures have been determined. The mechanism of why one particular protein sequence adopts so many different three-dimensional structures is yet not understood. In this work, we describe the assignment of the NMR chemical shifts of two Alzheimer’s disease fibril polymorphs, P1 and P2, which are formed by the amyloid-beta peptide Aβ40. The assignment is based on 13C-detected 3D NCACX and NCOCX experiments MAS solid-state NMR experiments. The fibril samples are prepared using an extensive seeding protocol in the absence and presence of the small heat shock protein αB-crystallin. In addition to manual assignments, we obtain chemical shift assignments using the automation software ARTINA. We present an analysis of the secondary chemical shifts and a discussion on the differences between the manual and automated assignment strategies.

CURD: a Single-Shot Strategy to Obtain Assignments and Distance Restraints for Proteins Using Solid-State MAS NMR Spectroscopy.

We present a strategy dubbed CURD (correlations using recycle delays) to acquire chemical-shift assignments and distance restraints for proteins in a single experimental block under slow-moderate magic-angle spinning conditions. This is done by concatenating the 3D-CCC and 3D-NNC experiments, both of which individually require long experimental times for sufficient resolution and sensitivity to be realized. Unlike previous approaches, the CURD strategy does not increase the amount of radio-frequency deposition on the sample and does not require lengthy procedures to optimize any of the pulse sequence elements. Instead, time savings is obtained by using the hitherto unused recycle delay of one of the experiments (2D-CC/3D-CCC) to establish inter-residue correlations for the second experiment (2D-NN/3D-NNC). Experiments are demonstrated on a model protein at the MAS frequency of 12.5 kHz and are shown to result in time savings of the order of days for most of the routine cases.

Belite-calcium sulphoaluminate cement prepared by EMR and BS: Hydration characteristics and microstructure evolution behavior

Belite-calcium sulphoaluminate (B-CSA) cement is regarded as one of the most promising alternatives to ordinary Portland cement (OPC). The production of B-CSA cement from industrial solid waste is a critical technology for maximising mineral resource utilisation. The morphology and microstructure of hydration products produced during the hydration process of B-CSA cement have a significant impact on the mechanical properties of the cement. In this paper, B-CSA cement prepared by electrolytic manganese residue (EMR) and barium slag (BS) was taken as the research object, and the changes of PH, turbidity and electrical conductivity in the early hydration process were monitored. Furthermore, the phase composition and microstructure of hydration products of cement paste were analysed using X-ray diffraction (XRD), Fourier transform infrared (FT-IR), thermogravimetric analysis (TG), solid state MAS-NMR spectroscopy, nitrogen adsorption test, scanning electron microscope (SEM) and electron microprobe analyzer (EPMA). The results show that with the sharp change of pH value, turbidity and electrical conductivity in the early hydration process of B-CSA cement, a large amount of ettringite is formed during the rapid hydration of ye’elimite, the metastable AFt part is transformed into AFm and the hydration reaction of belite was inhibited. The hydration products are mainly ettringite, monosulfate and AH3, which are responsible for the strength development of B-CSA cement. The hydration rate of belite in the early stage is slow, and the C-S-H gel phase can be formed in an aluminum-rich environment. The microstructure evolution of cement paste was revealed by nitrogen adsorption tests and SEM. The crystal state of ettringite changes from columnar to fibrous to construct the hardened framework of disorderly distributed cement paste, and the gel phase fills in the void formed by the ettringite skeleton to form a dense structure and reduce the porosity. The interface between the unreacted belite phase and the AFt skeleton is clear, and the gel phase plays a role in connecting them. Mn2+ was enriched on the C-S-H gel phase to form the Ca-Si-Mn compound and solidified. Ba2+ preferentially forms BaSO4 with SO42− which precipitates at the interface between the ettringite phase and C-S-H gel phase. Based on the analysis of the test results, the hydration characteristics and microstructure evolution of B-CSA cement were determined.

Planar Si5 and Ge5 Pentagons beside Isolated Phosphide Anions in Lithium Phosphide Tetrelides Li10+xSi5P and Li10+xGe5P

AbstractBinary lithium silicides and germanides as well as ternary lithium phosphidotetrelates have been intensively investigated with regard to their suitability as anode materials for all‐solid‐state‐batteries. In this context we studied the ternary phase diagram Li/Tt/P on the phosphorus‐poor side. The phosphide tetrelides Li10.68(8)Si5P and Li10.1(2)Ge5P are ternary compounds in the respective phase systems so far uniquely featuring discrete building blocks, which were previously found exclusively in binary alkali metal tetrelides and phosphides. Li10.68(8)Si5P and Li10.1(2)Ge5P contain aromatic Tt5 pentagons with an environment of mostly ordered Li atoms and isolated P3− anions with a coordination environment of predominantly disordered Li atoms. The five‐membered ring subunits are stacked under formation of [Li6Tt5] chains (Tt=Si, Ge). chains. The compounds crystallize in the space group Pnma (63) (Z=4) with cell parameters of a=10.2434(3) Å, b=4.2788(1) Å, c=23.9767(3) Å for Li10.68(8)Si5P and a=10.3599(11) Å, b=4.3072(2) Å, c=24.267(2) Å for Li10.1(2)Ge5P. The single crystal structure determination is supplemented by X‐ray powder diffraction experiments and 7Li, 29Si and 31P solid state MAS NMR spectroscopy. With respect to their electron count the compounds are placed between compounds comprising aromatic five‐membered rings such as the electron‐precise Zintl phase Li8MgSi6 and the non‐classical Zintl phase Li12Si7 having two extra electrons.

Nucleic acid–protein interfaces studied by MAS solid-state NMR spectroscopy

Solid-state NMR (ssNMR) has become a well-established technique to study large and insoluble protein assemblies. However, its application to nucleic acid–protein complexes has remained scarce, mainly due to the challenges presented by overlapping nucleic acid signals. In the past decade, several efforts have led to the first structure determination of an RNA molecule by ssNMR. With the establishment of these tools, it has become possible to address the problem of structure determination of nucleic acid–protein complexes by ssNMR. Here we review first and more recent ssNMR methodologies that study nucleic acid–protein interfaces by means of chemical shift and peak intensity perturbations, direct distance measurements and paramagnetic effects. At the end, we review the first structure of an RNA–protein complex that has been determined from ssNMR-derived intermolecular restraints.

Hydrodemethoxylation/Dealkylation on Bifunctional Nanosized Zeolite Beta

Mono-, and bimetallic Ni-, Ru-, and Pt-modified nanosized Beta zeolite catalysts were prepared by the post synthesis method and characterized by powder X-ray diffraction (XRD), nitrogen physisorption, HRTEM microscopy, temperature-programmed reduction (TPR-TGA), ATR FT-IR spectroscopy, and by solid-state MAS-NMR spectroscopy. The presence of nanosized nickel-oxide, ruthenium-oxide, and platinum species was detected on the catalysts. The presence of Brønsted and Lewis acid sites, and incorporation of nickel ions into zeolite lattice was proven by FT-IR of adsorbed pyridine. The structural changes in the catalyst matrix were investigated by solid state NMR spectroscopy. The catalysts were used in a gas-phase hydrodemethoxylation and dealkylation of 2-methoxy-4-propylphenol as a lignin derivative molecule for phenol synthesis.

Powder XRD and 31P and 27Al solid state MAS NMR investigations of phase transformations in aluminium phosphate bonded Al2O3–MgAl2O4 refractories

This study elucidates the phase development of an aluminium phosphate bonded Al2O3–MgAl2O4 ceramic body by means of powder X-ray diffraction (PXRD) as well as 31P and 27Al solid state MAS NMR spectroscopy. The binder used for this study was crystalline Al(H2PO4)3 in P2O5 concentrations of 3 wt% and 5 wt% of the total ceramic body. Analyses of the binder itself as well as within the refractory system after thermal treatment of up to T = 1500 °C, reveal how Al(H2PO4)3 acts as a network forming component: Within the refractory body, the binder creates a branched three-dimensional network of Q0, Q1 and Q2 structures by dehydration, chemical reactions, polymerisation and polycondensation. The bonding effect is based on surface reactions of acidic phosphoric components and crystalline phosphate structures on ceramic particles. The degree of cross-linking increases, via P–O–Al and P–O–P bonds, with augmenting temperature (T ≤ 600 °C). This network development is crucial for the formation of a property-determining phosphate bond. At temperatures of T ≥ 600 °C the aluminium phosphate phases react with MgAl2O4 to form Mg3(PO4)2.

Structural details of amyloid β oligomers in complex with human prion protein as revealed by solid-state MAS NMR spectroscopy

Human PrP (huPrP) is a high-affinity receptor for oligomeric amyloid β (Aβ) protein aggregates. Binding of Aβ oligomers to membrane-anchored huPrP has been suggested to trigger neurotoxic cell signaling in Alzheimer’s disease, while an N-terminal soluble fragment of huPrP can sequester Aβ oligomers and reduce their toxicity. Synthetic oligomeric Aβ species are known to be heterogeneous, dynamic, and transient, rendering their structural investigation particularly challenging. Here, using huPrP to preserve Aβ oligomers by coprecipitating them into large heteroassemblies, we investigated the conformations of Aβ(1–42) oligomers and huPrP in the complex by solid-state MAS NMR spectroscopy. The disordered N-terminal region of huPrP becomes immobilized in the complex and therefore visible in dipolar spectra without adopting chemical shifts characteristic of a regular secondary structure. Most of the well-defined C-terminal part of huPrP is part of the rigid complex, and solid-state NMR spectra suggest a loss in regular secondary structure in the two C-terminal α-helices. For Aβ(1–42) oligomers in complex with huPrP, secondary chemical shifts reveal substantial β-strand content. Importantly, not all Aβ(1–42) molecules within the complex have identical conformations. Comparison with the chemical shifts of synthetic Aβ fibrils suggests that the Aβ oligomer preparation represents a heterogeneous mixture of β-strand-rich assemblies, of which some have the potential to evolve and elongate into different fibril polymorphs, reflecting a general propensity of Aβ to adopt variable β-strand-rich conformers. Taken together, our results reveal structural changes in huPrP upon binding to Aβ oligomers that suggest a role of the C terminus of huPrP in cell signaling. Trapping Aβ(1–42) oligomers by binding to huPrP has proved to be a useful tool for studying the structure of these highly heterogeneous β-strand-rich assemblies.

Solid-state NMR and powder X-ray diffraction studies on ammonium ion-exchanged and dealuminated zeolite YNU-5

Aluminosilicate zeolite YNU-5, whose framework type code is YFI , has a unique pore structure consisting of 12–12–8-ring three-dimensional pores and isolated 8-ring straight channels. In this study, we evaluated how the crystal structure of zeolite YNU-5 changed by ammonium ion exchange and acid treatment by structural analysis using powder X-ray diffraction and solid-state MAS NMR spectroscopy. While the elemental ratio of calcined YNU-5 is Si/Al = 9.0, K/Al < 0.52, and Na/Al < 0.12, those of ammonium ion-exchanged sample were Si/Al = 9.3, K/Al < 0.03, and Na/Al < 0.03. That is, most alkali metal cation was exchanged to ammonium ion while suppressing dealumination. In an acid-treated sample with 2 M nitric acid at 353 K for 2 h under stirring conditions (milder dealumination conditions), dealumination took place and Si/Al was increased to 39.4, and almost all alkali metal ions were removed (K/Al < 0.3, and Na/Al < 0.2). When treated with 13.4 M nitric acid for 24 h under reflux conditions (severer dealumination conditions), deep dealumination occurred (Si/Al ~ 300) and the alkali metal ions were hardly detected. The structure refinement by the Rietveld method strongly suggested the presence of Si atom vacancies due to dealumination in the sample after milder acid-treatment conditions. In contrast, Si atom vacancies at specific T sites in the sample after severer acid-treatment conditions were hardly detected even though the presence of a small amount of Q 3 Si atom species ((SiO) 3 Si –OH) with silanol group was identified by 29 Si MAS NMR measurement. This finding suggests that almost all Al atoms were replaced by Si atoms migrated in nanopores and the vacancies are distributed uniformly at every T sites. By reflux acid treatment, the zeolite YNU-5 changed from the aluminosilicate type to the high silica type while maintaining high structural stability and high crystallinity. • Crystal structures of ammonium ion-exchanged and two kinds of dealuminated zeolite YNU-5 were analyzed in detail. • Simultaneously with dealumination, the Si atom migration phenomenon occurs during acid treatment. • The structural thermal stability of zeolite YNU-5 is strongly related to the distribution of T-atom vacancies in the framework.

The big effect of a small change: formation of CuO nanoparticles instead of covalently bound Cu(ii) over functionalized mesoporous silica and its impact on catalytic efficiency.

Two different heterogeneous catalysts, one with Cu(ii) covalently bonded to functionalized mesoporous silica (FMS-Cu(II)) and another with CuO nanoparticles immobilized over the same silica (FMS-CuO-np), have been synthesized by a common route but with a minor alteration in the sequence of addition of reagents. It is interesting to find that by merely changing the order of the addition of reagents Cu(ii) can be incorporated into the framework in two different forms. In one case Cu(ii) binds to the N and O donor centers present in the functionalized material whereas in the other case CuO nanoparticles are generated in situ. The materials have been thoroughly characterized by powder X-ray diffraction, nitrogen adsorption/desorption, transmission electron microscopy, thermal analysis, FT-IR spectroscopy, solid state MAS-NMR spectroscopy and atomic absorption spectrophotometric studies. The synthesized products have been examined for their catalytic efficiencies in the oxidation of olefins, as a model case. Styrene, α-methyl styrene, cyclohexene, trans-stilbene and cyclooctene have been used as substrates in the presence of tert-butyl hydroperoxide as the oxidant in acetonitrile medium under mild conditions. The products of the catalytic reactions have been identified and estimated by gas chromatography and gas chromatography-mass spectrometry. The rate of conversion of the substrates for both the catalysts is high and the selectivity is also good. But from comparative studies, it is found that FMS-CuO-np which contains CuO nanoparticles shows better efficiency than FMS-Cu(II). The catalysts have been recycled for five catalytic cycles without showing much decrease in their catalytic activity.

Effect of n-Butanol Cofeeding on the Methanol to Aromatics Conversion over Ga-Modified Nano H-ZSM-5 and Its Mechanistic Interpretation

Ga-modified nano H-ZSM-5 zeolites with different Ga contents were prepared and applied as methanol-to-aromatics (MTA) catalysts. The Ga introduction can strongly increase the selectivity to aromatics but also decrease the catalyst lifetime simultaneously. Upon the cofeeding of n-butanol with methanol, a significant prolongation of the catalyst lifetime from 18 to ca. 50 h can be achieved. According to several spectroscopic results, e.g., TGA, GC–MS, in situ UV/vis, and solid-state MAS NMR spectroscopy, the addition of n-butanol during the MTA conversion shows no impact on the deactivation mechanism but can influence the dual-cycle mechanism. Namely, n-butanol preferentially adsorbs on Bronsted acid sites over methanol, followed by dehydration into n-butene. The formed n-butene can directly participate in the olefin-based cycle and, therefore, significantly alter the proportions of the dual-cycle mechanism. These results provide mechanistic insights into the roles of n-butanol cofeeding in the MTA conversi...

Cu- and Ni-Grafted Functionalized Mesoporous Silica as Active Catalyst for Olefin Oxidation

Mesoporous silica has been functionalized with 3-aminopropyl triethoxy silane (3-APTES), followed by Schiff-base condensation with 2-hydroxy-1-naphthaldehyde. Incorporation of copper and nickel by covalent grafting onto the Schiff-base loaded materials gives two heterogenized catalysts namely, Cu–Cat and Ni-Cat, respectively. The materials have been characterized by PXRD analyses, nitrogen sorption studies, TEM, TGA, FT-IR, UV-visible and solid state MAS-NMR spectroscopy. The metal-contents in the samples are estimated using ICP-AES studies. Cu–Cat and Ni-Cat have been used as active catalyst in the oxidation of various olefins e. g. styrene, α-methyl styrene, cyclohexene, trans stilbene and cyclooctene in the presence of tert-butyl hydroperoxide as the oxidant in acetonitrile under mild conditions. Different products have been analyzed by gas chromatography and gas chromatography-mass spectrometry. The results show high conversion of the substrates, moderate to good product selectivity and high TOFs of the reactions. The catalysts are recycled without deteriorating their activities and heterogeneous nature.

Novel family of periodic mesoporous organosilicas containing azobenzene within the pore walls

Three new bis-silylated azobenzenes, differently substituted, having terminal triethoxysilyl groups attached directly to the para position of the phenyl rings without linker, namely bis(4-triethoxysilyl)azobenzene, bis(2,6-dimethyl-4-triethoxysilyl)azobenzene and bis(2,6-diisopropyl-4-triethoxysilyl)azobenzene, have been successfully synthesized by Lithium-Iodine exchange from its diiodoazobenzene-derivatives, and used to prepare three novel azobenzene-bridged periodic mesoporous organosilica materials (Azb-PMO-R, R= H, Me and iPr). The synthesis of these materials from 100% of bis-silylated azobenzenes precursors was carried out under basic conditions using octadecyltrimethylammonium chloride (C18TMACl) as structure-directing agent. The successful synthesis was verified by N2 sorption measurements, solid state MAS-NMR spectroscopy, and IR spectroscopy. Materials with pore sizes between 3.7 and 4.6 nm and specific surface areas in the range of 400–700 m2/g were obtained. UV–Visible spectroscopy shows that the prepared PMOs are formed by rigid combination of isomers cis and trans of azobenzene moieties, which do not exhibit a regular photochemical trans-to-cis isomerization of the azo group upon alternating UV–Visible irradiation. However, these materials probably exhibit a dynamic and local bending which could be useful for reversible gas adsorption and release with light.

Improving Sensitivity of Solid-state NMR Spectroscopy by Rational Design of Polarizing Agents for Dynamic Nuclear Polarization.

We review our recent efforts to optimize the efficiency of polarizing agents for Dynamic Nuclear Polarization (DNP) in solid-state MAS NMR spectroscopy. We elucidate the links between DNP performance, molecular structure and electronic relaxation properties of dinitroxide biradicals. We show that deuteration and increased bulkiness lead to slower electronic relaxation and in turn to higher DNP enhancements. We also show that the incorporation of solid dielectric particles into the sample is a general method of amplifying DNP enhancements by about a factor of two.

Combined Solid-State NMR and Computational Approach for Probing the CO2 Binding Sites in a Porous-Organic Polymer

We report on utilization of 1D and 2D 13C cross-polarization magic angle spinning (CPMAS) and MAS solid-state NMR spectroscopy in probing the binding sites and dynamical processes of 13C-enriched CO2 inside the pores of a pyridine-containing porous organic polymer (POP). Our findings from the spectroscopic measurements conducted on the evacuated sample and on the sample dosed with 800 mbar 13CO2 indicated preferential adsorption of the CO2 molecules at the vicinity of the basic binding sites within the POP, the pyridine rings. We further demonstrate the results of a computational study for probing the most favorable binding sites of CO2 inside a geometrically optimized model of the polymer in an attempt to better rationalize the experimental findings from 13C solid-state NMR investigations. Because of the amorphous nature of the studied POP, also being observed for a large number of emerging microporous solids, this combined approach can prove useful and versatile toward drawing a detailed picture of the ...

Characterization of secondary phosphine oxide ligands on the surface of iridium nanoparticles.

The synthesis of iridium nanoparticles (IrNPs) ligated by various secondary phosphine oxides (SPOs) is described. This highly reproducible and simple method via H2 reduction produces well dispersed, small nanoparticles (NPs), which were characterized by the state-of-the-art techniques, such as TEM, HRTEM, WAXS and ATR FT-IR spectroscopy. In particular, multinuclear solid state MAS-NMR spectroscopy with and without cross polarization (CP) enabled us to investigate the different binding modes adopted by the ligand at the nanoparticle surface, suggesting the presence of three possible types of coordination: as a purely anionic ligand Ir-P(O)R2, as a neutral acid R2P-O-H and as a monoanionic bidentate H-bonded dimer R2P-O-HO[double bond, length as m-dash]PR2. Specifically, the higher basicity of the dicyclohexyl system leads to the formation of IrNPs in which the bidentate binding mode is most abundant. Such cyclohexyl groups are bent towards the edges, as is suggested by the study of 13CO coordination on the NP surface. This study also showed that the number of surface sites on faces available for bridging CO molecules is higher than the number of sites for terminal CO species on edges and apices, which is unexpected taking into account the small size of the nanoparticles. In addition, the IrNPs present a high chemoselectivity in the hydrogenation of cinnamaldehyde to the unsaturated alcohol.

29Si,47Ti,49Ti and195Pt solid state MAS NMR spectroscopic investigations of ternary silicides TPtSi, germanides TPtGe (T = Ti, Zr, Hf) and stannide TiPtSn

Eight ternary tetrelides TPtX (T = Ti, Zr, Hf; X = Si, Ge, Sn) were synthesized from the elements by arc-melting and subsequent annealing. TiPtSi, ZrPtSi, ZrPtGe, HfPtSi and HfPtGe crystallize with the orthorhombic TiNiSi type structure, in the space group Pnma. The structures of HfPtSi (a = 654.44(9), b = 387.97(6), c = 750.0(1) pm, wR2 = 0.0592, 411 F(2) values, 20 variables) and HfPtGe (a = 660.36(7), b = 395.18(4), c = 763.05(8) pm, wR2 = 0.0495, 430 F(2) values, 20 variables) were refined from single crystal X-ray diffractometer data. TiPtSn adopts the cubic MgAgAs type. TiPtGe is dimorphic with a TiNiSi type high-temperature modification which transforms to cubic LT-TiPtGe (MgAgAs type). All phases were investigated by high resolution (29)Si, (47)Ti, (49)Ti and (195)Pt solid state MAS NMR spectroscopy. In the cubic compounds, the (47/49)Ti NMR signals are easily detected owing to the absence of quadrupolar broadening effects. The (195)Pt resonances of the orthorhombic compounds are characterized by strongly negative isotropic Knight shifts and large Knight shift anisotropies, whereas positive isotropic Knight shifts and no anisotropies are observed for the cubic compounds. These results indicate that the phase transition in TiPtGe is associated with dramatic changes in the electronic properties. Within each group of isotypic compounds the isotropic (29)Si, (47/49)Ti and (195)Pt Knight shifts show systematic dependences on the transition metal or tetrel atomic number, suggesting that the numerical values are influenced by the electronegativities of the metallic (or metalloid) neighbours.

Identification of Li-Ion Battery SEI Compounds through (7)Li and (13)C Solid-State MAS NMR Spectroscopy and MALDI-TOF Mass Spectrometry.

Solid-state (7)Li and (13)C MAS NMR spectra of cycled graphitic Li-ion anodes demonstrate SEI compound formation upon lithiation that is followed by changes in the SEI upon delithiation. Solid-state (13)C DPMAS NMR shows changes in peaks associated with organic solvent compounds (ethylene carbonate and dimethyl carbonate, EC/DMC) upon electrochemical cycling due to the formation of and subsequent changes in the SEI compounds. Solid-state (13)C NMR spin-lattice (T1) relaxation time measurements of lithiated Li-ion anodes and reference poly(ethylene oxide) (PEO) powders, along with MALDI-TOF mass spectrometry results, indicate that large-molecular-weight polymers are formed in the SEI layers of the discharged anodes. MALDI-TOF MS and NMR spectroscopy results additionally indicate that delithiated anodes exhibit a larger number of SEI products than is found in lithiated anodes.

Structure and Li+ Dynamics of the Single-Ion Conducting Polymer Electrolyte P(STFSI)-Ran-PEGMA

Polymeric, solid-state, single-ion conducting electrolytes with high ionic conductivity are desired for application in high energy battery platforms. Recently, PEO-based copolymers containing the lithiated STFSI monomer have been investigated for use as single-ion conducting electrolytes in lithium batteries. These polymers exhibit wider electrochemical stability windows and sustain capacity of full cell battery cycling at higher discharge rates relative to traditional polymer electrolytes composed of PEO and a mobile, dopant salt. This presentation will report on the characterization of the morphology and dynamics of PSTFSI-ran-PEGMA copolymer electrolytes as a function of the monomer ratio (Li+ loading) and length of the polyethylene glycol comb. Structure of the electrolytes is investigated by SAXS/WAXS, SANS, and TEM. Lithium environment is examined using solid state MAS NMR spectroscopy, and ion dynamics are studied via PFG NMR spectroscopy and dielectric spectroscopy. Polymer dynamics are investigated via QENS. Together, this suite of characterization techniques reveals the structure and corresponding Li+ transport mechanisms in this family of high performing PEO-based single ion conductors.

ChemInform Abstract: Sn6[P12N24] — A Sodalite‐Type Nitridophosphate.

AbstractThe title compound is synthesized from a mixture of Sn powder and HPN2 (evacuated silica ampule, 820 °C, 85 h) and characterized by powder XRD, solid state MAS NMR spectroscopy, 119Sn Moessbauer spectroscopy, and DFT electronic structure calculations.