The search for new zeolites is of continuous interest in the field of zeolite science because of their widespread application in catalysis and adsorption–separation. To this end, considerable efforts have been devoted to the preparation of new zeolites with novel porous architectures and compositions. Taking account of the key factors governing the formation of zeolites (e.g., guest species, framework elements, construction processes, etc.), several synthetic strategies have been developed recently. These allow the discovery of many new zeolites with unprecedented structural features, such as hierarchical pores, odd-ring numbers (11-, 15-rings), extra-large pores (16-, 18-, 20-, 28-, and 30-rings), chiral pores, and extremely complex framework topologies, etc. In this review, we will present the advances in the synthesis of new zeolite structures in the last decade, which are achieved by utilization of the synthetic strategies based on pre-designed structure-directing agents, heteroatom substitution, and topotactic transformations.

/pdf/synthesis-of-new-zeolite-structures-2ko332k5bn.pdf

Synthesis of new zeolite structures

New stories of zeolite structures: their descriptions, determinations, predictions, and evaluations.

Zeolites are porous materials with potential uses in electronics, catalysis and gas storage. A new zeolite named ITQ-33 has now been synthesized with the advantage over previous compounds of a very large micropore volume. The conditions for synthesis were identified using high-throughput techniques. The new material has two pore systems, one with a very large diameter ring structure (relative to pores found in other zeolites), intersected by a second of medium diameter. This open architecture will be particularly suited to catalysis. Crystalline molecular sieves with large pores and high adsorption capacities have many potential applications1,2,3,4. Of these materials, zeolites are of particular interest owing to their stability in a wide range of experimental conditions. An aluminophosphate with very large circular channels5 containing 18 oxygen atoms (18-ring channels) has been synthesized, but in the search for large-pore zeolites, most of the materials which have been synthesized up to now contain only 14-ring channels; the synthesis of zeolites with larger ring structures has been believed to be hindered by the low Si-O-Si bond angles available. A silicogaloaluminate (ECR-34) with unidirectional 18-ring channels12 was recently reported, but exhibited low micropore volume, thus rendering the material less attractive for catalytic applications. Here we report the structure and catalytic activity of the silicogermanate zeolite ITQ-33; this material exhibits straight large pore channels with circular openings of 18-rings along the c axis interconnected by a bidirectional system of 10-ring channels, yielding a structure with very large micropore volume. The conditions for synthesis are easily accessible, but are not typical, and were identified using high-throughput techniques.

High-throughput synthesis and catalytic properties of a molecular sieve with 18- and 10-member rings

Probing liquid/solid interfaces at the molecular level.

Cite we must, cite we do. We cite because we are links in a chain, using properties and methods validated by others. We also cite to negotiate the anxiety of influence. And to be fair. After outlining the reasons for citation, we use two case studies of citation amnesia in the field of hypothetical carbon allotropes to present a computer-age search tool (SACADA) in that subsubfield. Finally, we advise on good search practice, including what to do if you miss a citation.

https://onlinelibrary.wiley.com/doi/pdf/10.1002/anie.201600655

Homo Citans and Carbon Allotropes: For an Ethics of Citation.

A framework topology, that has not been observed previously, has been discovered in oxonitridophosphates. The structural characterization by single-crystal structure determination shows that the network is composed of comer-sharing P(O,N) 4 -tetrahedra forming 12-ring channels.

LixH12-x-y+z[P12OyN24-y]Clz--an oxonitridophosphate with a zeolitelike framework structure composed of 3-rings.

LixH12xyz[P12OyN24y]Clz – ein Oxonitridophosphat mit zeolithartiger Gerüststruktur aus Dreierringen

Die Oxonitridophosphate LixH12-x-y+z[P12OyN24-y]Clz (1a) und LixH12-x-y+z[P12OyN24-y]Brz (1b) wurden durch Reaktion von Li2S, SP(NH2)3, OP(NH2)3 und NH4Cl bzw. NH4Br in geschlossenen Ampullen bei 700 °C im Rohrenofen erhalten. Die Kristallstruktur von LixH12-x-y+z[P12OyN24-y]Xz (X = Cl, Br) (1) wurde an Einkristallen von 1a und Mischkristallen 1ab mittels Rontgenbeugung (Pna21; a = 475.3(1) pm, b = 1420.8(3) pm, c = 820.3(2) pm (1a) bzw. a = 476.6(1) pm, b = 1426.3(3) pm, c = 823.5(2) pm (1ab); Z = 1) und an Pulverproben von 1a mittels Rontgenbeugung, Neutronenbeugung, Elektronenbeugung und Festkorper-NMR-Spektroskopie aufgeklart. Das anionische Netzwerk ist aus allseitig eckenverknupften P(O, N)4Tetraedern unter Ausbildung von Zwolferring-Kanalen aufgebaut. Die Lithium- und Halogenid-Ionen befinden sich in diesen Kanalen. Die chemische Zusammensetzung der Proben wurde uber EDX- und Elementaranalysen bestimmt. IR- und Raman-spektroskopische Eigenschaften sowie das thermische Verhalten wurden untersucht. Impedanzspektroskopische Messungen zeigten eine Lithium-Ionen-Leitfahigkeit.



LixH12-x-y+z[P12OyN24-y]Xz (X = Cl, Br) - Oxonitridophosphates with NPO Zeolite Structure



The oxonitridophosphates LixH12-x-y+z[P12OyN24-y]Clz (1a) and LixH12-x-y+z[P12OyN24-y]Brz (1b) were obtained by the reaction of Li2S, SP(NH2)3, OP(NH2)3 and NH4Cl or NH4Br, respectively, in closed ampoules at 700 °C in a tube furnace. The crystal structure of LixH12-x-y+z[P12OyN24-y]Xz (X = Cl, Br) (1) was elucidated by means of X-ray diffraction of single crystals of 1a and of mixed single crystals 1ab (Pna21; a = 475.3(1) pm, b = 1420.8(3) pm, c = 820.3(2) pm (1a) and a = 476.6(1) pm, b = 1426.3(3) pm, c = 823.5(2) pm (1ab), respectively; Z = 1) and via X-ray diffraction, neutron diffraction, electron diffraction and solid state NMR spectroscopy of powder samples of 1a. The anionic network is composed of corner-sharing P(O, N)4-tetrahedra forming 12-ring channels. The lithium and the halide ions are located in these channels. The chemical composition of the samples was determined by EDX analysis and chemical elemental analysis. IR and Raman spectroscopic properties as well as the thermal behaviour were investigated. Impedance spectroscopic measurements showed a lithium ion conductivity.

LixH12‐x‐y+z[P12OyN24‐y]Xz (X = Cl, Br) ‐ Oxonitridophosphate mit NPO‐Zeolithstruktur

Synthesis, crystal structures and properties of the bis-(trimetaphosphimato)-metallates Na4{Co[(PO2NH)3]2}·12H2O and Na4{Ni[(PO2NH)3]2}·12H2O

Tetranatrium-bis(trimetaphosphimato)cuprat(II)-Decahydrat, Na4{Cu[(PO2NH)3]2} · 10 H2O, wurde durch Umsetzung einer wassrigen Losung von Na3(PO2NH)3 · 4 H2O mit Cu(NO3)2 · 3 H2O im molaren Verhaltnis 2 : 1 dargestellt. Die Struktur von Na4{Cu[(PO2NH)3]2} · 10 H2O (1) wurde durch Einkristall-Rontgenstrukturanalyse ermittelt (P 1, a = 912,51(6), b = 932,14(6), c = 966,10(6) pm, α = 94,840(5), β = 108,652(6), γ = 118,588(6)°, Z = 1). Die P3N3-Ringe in den Trimetaphosphimat-Ionen liegen in einer leicht verzerrten Sofakonformation vor. Die Konformation der Ringe last sich mit Hilfe der Torsionswinkel, der Displacement-Asymmetrie- und der Puckering-Parameter beschreiben. Die Trimetaphosphimat-Ionen koordinieren Cu2+ als zweizahnige Liganden und bilden zusammen mit Wassermolekulen komplexe Anionen der Zusammensetzung {Cu[(PO2NH)3]2 · 2 H2O}4–, welche im Kristall uber Wasserstoffbrucken (N–H…O und O–H…O) und durch Koordination uber Na+ zu einem dreidimensionalen Netzwerk verknupft werden.



Synthesis, Crystal Structure, and Properties of Tetrasodium Bis(trimetaphosphimato)cuprate(II) Decahydrate, Na4{Cu[(PO2NH)3]2} · 10 H2O



Tetrasodium bis(trimetaphosphimato)cuprate(II) decahydrate, Na4{Cu[(PO2NH)3]2} · 10 H2O, was obtained by the reaction of an aqueous solution of Na3(PO2NH)3 · 4 H2O with Cu(NO3)2 · 3 H2O (molar ratio 2 : 1). The structure of Na4{Cu[(PO2NH)3]2} · 10 H2O (1) was solved by single-crystal X-ray methods (P 1, a = 912.51(6), b = 932.14(6), c = 966.10(6) pm, α = 94.840(5), β = 108.652(6), γ = 118.588(6)°, Z = 1). The P3N3 rings of the trimetaphosphimate ions exhibit a slightly distorted sofa conformation. The conformation of the anions have been analysed using torsion angles, displacement asymmetry parameters, and puckering parameters. The trimetaphosphimate ions act as bidentate ligands of Cu2+. With additionally coordinated water molecules, anionic complexes {Cu[(PO2NH)3]2 · 2 H2O}4– are formed. In the crystal these complexes are interconnected by N–H…O und O–H…O hydrogen bonds and they coordinate the Na+. Thus, a three-dimensional network is formed.

Synthese, Kristallstruktur und Eigenschaften von Tetranatrium‐bis(trimetaphosphimato)cuprat(II)‐Decahydrat, Na4{Cu[(PO2NH)3]2} · 10 H2O

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