CCDC 1535081: Experimental Crystal Structure Determination
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An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.Sodalite
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Monoclinic crystal system
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Crystal Structure of BaNb6.3(1)Ti3.6(1)O16 containing Nb6O12, fused Ti3O13 Clusters and Ti3O10 Units
A new phase, BaNb6.3(1)Ti3.6(1)O16, has been synthesised. Electron diffraction studies indicate an hexagonal substructure with unit cell parameters a ≈ 8.9 Å and c ≈ 9.5 Å. In some of the ED patterns superstructure reflections are present, indicating a supercell with a = √3 · asub and c = csub. However, X-ray single-crystal diffraction studies of a crystallite yielding reflections corresponding to the supercell revealed it to be monoclinic, with the unit cell parameters a = 26.811(2) Å, b = 15.4798(2) Å, c = 9.414(2) Å, β = γ = 90° and α = 90.0(3)°. The average crystal structure was refined, using the subcell with a = 8.937(2) Å, b = 15.479(2) Å, c = 9.414(2) Å, β = γ = 90° and α = 90.0(3)°, space group Cm11, and Z = 4, to RI = 3.24% and RwI = 3.44%. The structure can be described as an hexagonal close packing layers of Nb6 octahedra, Ba, and O atoms (A1, A2) and layers of O atoms (B1, B2), appearing in the packing sequence: A1B1A2B2. The Nb6 octahedra are found in isolated Nb6O12O6 clusters, and the Ti atoms in Ti3O13 and Ti3O10 units in octahedral and tetrahedral voids formed by O atoms, respectively. The Ti positions were found to be only partly occupied. Microanalysis indicates that some Nb atoms are located in the Ti3 triangles. A model is presented that interprets these not fully occupied Ti3 triangles as a result of a superimposing of three different structures. Two of these consist of two fused Ti3O13 units, forming an Ti6O19 unit, and a Ti3O10 unit, while the third consists of alternating Ti3O13 units. Die Kristallstruktur von BaNb6.3(1)Ti3.6(1)O16 mit Nb6O12, und verknüpften Ti3O13-Clustern sowie Ti3O10-Einheiten Eine neue Phase, BaNb6.3(1)Ti3.6(1)O16, wurde synthetisiert. Elektronenbeugungsuntersuchungen zeigen eine hexagonale Überstruktur mit den Zellparametern a £ 8.9 Å und c ≈ 9.5 Å. In einigen Beugungsbildern sind Überstrukturreflexe vorhanden, die auf eine Superzelle mit a = √3 · asub und c = csub hinweisen. Röntgen-Einkristallbeugungsaufnahmen an einem Kristall ergeben eine monokline Superzelle mit a = 26.811(2) Å, b = 15.4798(2) Å, c = 9.414(2) Å, β = γ = 90° und α = 90.0(3)°. Die (mittlere) Kristallstruktur wurde verfeinert unter Einbeziehung der Subzelle mit a = 8.937(2) Å, b = 15.479(2) Å, c = 9.414(2) Å, β = γ = 90° und α = 90.0(3)°, Raumgruppe Cm11, Z = 4, RI = 3.24% und RwI = 3.44%. Die Struktur kann als hexagonal dichteste Packung von zwei Schichten bestehend aus Nb6-Oktaedern, Ba- und O-Atomen (A1, A2) sowie aus O-Atomen (B1, B2) mit der Packungsfolge A1B1A2B2 beschrieben werden. Die Nb6-Oktaeder sind in isolierte Nb6O12O6-Clustern inkorpuriert, und die Ti-Atome in Ti3O13- und Ti3O10-Einheiten in oktaedrischen bzw. tetraedrischen Lücken, die von O-Atomen gebildet werden. Die Ti-Positionen sind nur teilweise besetzt. Mikroanalysen zeigen, dass einige Nb-Atome in den Ti3-Dreiecken lokalisiert sind. Ein Modell wird vorgestellt, nach dem die nicht vollbesetzten Ti3-Dreiecke als Ergebnis einer Überlagerung von drei unterschiedlichen Strukturen interpretiert werden: Zwei von diesen bestehen aus verknüpften Ti3O13-Einheiten, die eine Ti6O19- und eine Ti3O10-Einheit bilden, während eine dritte aus alternierenden Ti3O13-Einheiten besteht.
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The new compounds Li(2-x)Na(x)Ni[PO(4)]F (x = 0.7, 1, and 2) have been synthesized by a solid state reaction route. Their crystal structures were determined from single-crystal X-ray diffraction data. Li(1.3)Na(0.7)Ni[PO(4)]F crystallizes with the orthorhombic Li(2)Ni[PO(4)]F structure, space group Pnma, a = 10.7874(3), b = 6.2196(5), c = 11.1780(4) Å and Z = 8, LiNaNi[PO(4)]F crystallizes with a monoclinic pseudomerohedrally twinned structure, space group P2(1)/c, a = 6.772(4), b = 11.154(6), c = 5.021(3) Å, β = 90° and Z = 4, and Na(2)Ni[PO(4)]F crystallizes with a monoclinic twinned structure, space group P2(1)/c, a = 13.4581(8), b = 5.1991(3), c = 13.6978(16) Å, β = 120.58(1)° and Z = 8. For x = 0.7 and 1, the structures contain NiFO(3) chains made up of edge-sharing NiO(4)F(2) octahedra, whereas for x = 2 the chains are formed of dimer units (face-sharing octahedra) sharing corners. These chains are interlinked by PO(4) tetrahedra forming a 3D framework for x = 0.7 and different Ni[PO(4)]F layers for x = 1 and 2. A sodium/lithium disorder over three atomic positions is observed in Li(1.3)Na(0.7)Ni[PO(4)]F structure, whereas the alkali metal atoms are well ordered in between the layers in the LiNaNi[PO(4)]F and Na(2)Ni[PO(4)]F structures, which makes both compounds of great interest as potential positive electrodes for sodium cells.
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Scandium
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Five isomorphous d 0 transition metal oxofluoride compounds A 3 [ M 2 O x F 11 − x ]·( A F) 0.333 ( A = K, Rb, NH 4 ; M = Nb, Mo, W; x = 2, 4) have been synthesized from acid fluoride solutions, and their crystal structures have been determined by single-crystal X-ray diffraction. The basic structural building units are dinuclear M 2 X 11 (dimers) formed from NbOF 5 or Mo(W)O 2 F 4 octahedra connected by the fluorine bridging atom. In the Nb 2 O 2 F 9 dimer, the O atoms occupy apical corners. In the M 2 O 4 F 7 ( M = Mo, W) dimers two O atoms are also apically placed, whereas the other two O atoms are statistically disordered in equatorial planes. The arrangement of dimers is so that the hexagonal tunnels containing `free' fluoride ions are formed. During the irradiation process the orthorhombic structure of K 3 Nb 2 O 2 F 9 ·(KF) 0.333 transforms into a pseudo-trigonal one with a = 23.15 Å, which is the [101] diagonal of the orthorhombic unit cell. The other four trigonal crystals are merohedral twins.
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Monoclinic crystal system
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Monoclinic crystal system
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Organometallic Chemistry
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A new vanadium(III) phosphate, Ba[VIII2(HPO4)4](H2O), has been synthesized by hydrothermal methods, and its structure solved by single-crystal X-ray diffraction. This vanadium phosphate crystallizes in the monoclinic system, space group P21. The cell parameters are a = 9.441(2), b = 7.913(2), c = 9.521(2) Å; β = 117.91(2)°; V= 628.5(3)Å3; Z = 2; Dcalc = 3.387 mg mm−3; R = 0.055 and Rw = 0.065 for 1885 reflections with F > 6.0σ(F). The threedimensional [V2(HPO4)4(H2O)]2− lattice can be described as being built up of chains of eight-membered rings along the c axis, formed by corner-shared VO6 octahedra and HPO4 tetrahedra (-V-O-P-O-), which are crosslinked via interchain V-O-P bonding to produce a three-dimensional lattice. The crosslinking interaction produces 16-membered rings. Contrary to other low-valent vanadium phosphates, cavities are found in the solid,rather than tunnels. The Ba2+ and H2O are located in these cavities.
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