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AlPO4-5 is a zeolite (structure type: AFI) with 6-and 12-membered rings, and 12-membered ring channels have a relatively large pore size of 7.3 and can take in a variety of molecules (Fig. 1).Although there have been many studies on the adsorption properties of AlPO4-5 as a molecular sieve, surprisingly, its crystal structure remains unclear.For example, the most accepted space group of AlPO4-5 is P6cc with unit cell parameters of a ~ 13.7 and c ~ 8.5 (e.g., [1]), but several space groups with lower symmetry have also been proposed (e.g., [2,3]).Furthermore, although the existence of satellite reflections suggesting the existence of modulated structures has recently been reported under high pressure [4], a detailed analysis of these satellite reflections has not been performed due to the weakness of the observed satellite reflections.Here we revisit to perform x-ray diffraction using a relatively large single crystal of AlPO4-5.Single crystal x-ray diffraction experiments for calcined AlPO4-5 single crystals were conducted using a laboratory-based x-ray diffractometer (Rigaku/Synergy custom) with a Mo rotating anode (Rigaku/MicroMax-007), a confocal x-ray mirror (Rigaku/VariMax-MoHF), and a hybrid pixel semiconductor detector (Rigaku/Hypix-6000HE).The diffraction images were obtained for single crystals of about 100 m in diameter, and we first found the satellite peaks of q = 0.3725(3) c* up to 2 nd order even at ambient conditions.The observed q value is similar to the previously reported value under high pressure [4], and its noninteger value indicates that the AlPO4-5 has an incommensurate structure.We also tested the thermal stability of the incommensurate structure by single crystal x-ray diffraction and Raman spectroscopy using a purpose-built high-temperature chamber under vacuum.The detailed analysis of the incommensurate structure and its thermal stability is going to be discussed.Figure 1.Crystal structure of AlPO4-5 along c-axis (left) and a 12-membered channel (right).
3The crystal structure and characterization of 2-D and 3-D indium phosphates synthesized from a water/ethylene glycol mixed-solvent system
The crystal structure and characterization of 2-D and 3-D indium phosphates synthesized from a water/ethylene glycol mixed-solvent system
Read more10Synthesis and Characterization of a Two-Dimensional Zinc Phosphite, Zn3(tren)(HPO3)3·xH2O (x ≈ 0.5; tren = tris(2-aminoethyl)amine)
A new zinc phosphite with the formula Zn3(tren)(HPO3)3·xH2O (x≈0.5) has been synthesized under hydrothermal conditions and characterized by FTIR, elemental analysis, powder X-ray diffraction, single-crystal X-ray diffraction, thermogravimetric analysis and its fluorescent spectrum. The compound crystallizes in the triclinic system, space group (No.2), a = 10.1188(9) Å, b = 10.4194(9) Å, c = 10.5176(9) Å, α = 60.763(2)°, β = 70.6150(10)°, γ = 80.725(2)°, V = 912.77(14) Å3, Z = 2. The structure consists of double crankshaft chains, which are linked by Zn-O-P bonds to form 8- and 12-membered channels along the [100] direction. The claw-like Zn-centered complexes of Zn(N4C6H18) as the supported templates, hang into the 12-MR channels through Zn-O-P linkages with framework.
Read more3Novel High‐Pressure Potassium Chloride Monohydrate and Its Implications for Water‐Rich Planetary Bodies
Saline water is a common fluid on the Earth‘s surface and in ice planets. Potassium chloride (KCl) is a common salt and is expected to be a ubiquitous solute in salt water in the Universe; however, few studies investigated the behavior of KCl‐H2O system at high pressures and temperatures. In this study, powder and single‐crystal X‐ray diffraction (SC‐XRD), Raman and Brillouin scattering combined with diamond anvil cells were used to investigate the phase relation in the KCl‐H2O system for different KCl concentrations at 0–4 GPa and 298–405 K. The results of powder X‐ray diffraction and Raman scattering demonstrate that a novel KCl hydrate is formed when KCl aqueous solutions transform to solid ice‐VI and ice‐VII at high pressure. Simultaneously, the single‐crystal of KCl hydrate is synthesized from a supersaturated KCl solution at 298 K and 1.8 GPa. The structure is solved by SC‐XRD, indicating a KCl monohydrate with the P21/n space group is formed. We have verified the phase stability of KCl monohydrate by using Raman spectroscopy and density functional theory. Our results indicate that KCl monohydrate is a stable phase under pressure and temperature conditions between 1.6 and 2.4 GPa and 298–359 K. By considering the thermal profile and composition of icy moons, we hypothesize that the formation and decomposition of KCl monohydrate might induce mantle convection in these moons.
Read more5The synthesis and crystal structure of Rb4TmI6: Lattice energy calculations on networks of condensed cubes
The synthesis and crystal structure of Rb4TmI6: Lattice energy calculations on networks of condensed cubes
9Synthesis, structure and photoluminescence properties of amine-templated open-framework bismuth sulfates
Synthesis, structure and photoluminescence properties of amine-templated open-framework bismuth sulfates
Synthesis, Crystal Structure and Thermal Decomposition of Triaminoguanidinium 2, 4, 6-Trioxo-1, 3, 5-triazinan-1-ide Based on Cyanuric Acid
A nitrogen-rich energetic compound-triaminoguanidinium 2, 4, 6-trioxo-1, 3, 5-triazinan-1-ide (1) was prepared with a yield of 91% via one-step metathesis reaction using triaminoguanidinium hydrochloride (TAG-HCl) and sodium cyanurate (CANa) as raw materials. The structure of the product was characterized by X-ray single-crystal diffraction, UV-Vis, FT-IR, 1H NMR, mass spectrometry and elemental analysis. The enthalpy of formation and detonation parameters of the product were calculated. Its thermal stability, non-isothermal reaction kinetics and decomposition process were studied by differential scanning calorimetry(DSC) at a heating rate of 10 K·min-1 and thermogravimetric (TG) analysis coupled with Fourier transform infrared spectroscopy (FTIR). The impact sensitivity of the product was determined by the drop hammer test. Results show that the crystal of compound 1 is monoclinic, space group P21/n with a calculated density of 1.676 g·cm-3. Its enthalpy of formation is 327.9 kJ mol-1, the detonation velocity 7900 m·s-1, and the detonation pressure 26.5 GPa. Probable thermal decomposition mechanism of 1 under N2 atmosphere as shown in the text is proposed. Compound 1 is very insensitive to impact, and the impact sensitivity is greater than 60 J, which is better than that of TATB (50 J).
Read more8Synthesis and Crystal Structure of a 6H Hexagonal Fluoro-Perovskite: RbMgF3
RbMgF3, a perovskite halide, serendipitously crystallized from a reaction between MgCl2 and TiO2 in molten RbCl/RbF eutectic flux (melting point = 546 °C) and was characterized by single crystal X-ray diffraction. RbMgF3 crystals can also be grown directly in higher yield using a molten RbCl–RbF flux layered over MgCl2 or MgF2 contained in a silver tube at 575 °C. RbMgF3 crystallizes in the hexagonal space group P63/mmc in the 6H hexagonal perovskite structure type with lattice parameters a = 5.8368(2) A and c = 14.2087(5) A. The crystal structure exhibits face-sharing Mg2F9 octahedra connected via corner-sharing MgF6 octahedra. Elemental composition for RbMgF3 was semi-quantitatively confirmed by energy dispersive spectroscopy (EDS). X-ray diffraction quality single crystals of RbMgF3 were grown from a molten RbCl/RbF eutectic flux at 850 °C and used for structure determination using single crystal X-ray diffraction. The compound crystallizes in the hexagonal space group P63/mmc in the 6H hexagonal structure type.
Read moreCrystallographic Study of a coordination polymer based on Zn2+ion
Several studies have aimed to better understand coordination polymers, which are structures based on a connection between a metal ion and an organic ligand that extends infinitely, forming a macro-structure1. The interest in this type of structure is mainly due to its properties, such as its pore-forming ability, presenting many potential applications2 like selective separations, catalysis and gas storage. It is interesting to study the structure of coordination polymers to focus in some particular future application. In these way, a coordination polymer was synthetized by simple mixture with isonicotinylhydrazine (INH) and 1,2,4,5-benzenetetracarboxylic acid (BTC) ligands and zinc metallic ion. Yellow single crystals were formed in solution and one was separated, measured and solved by single crystal X-ray diffraction. The crystal-data for the structure were collected using an Oxford GEMINI A-Ultra diffractometer with MoKα radiation (λ = 0.71073 Å) at room temperature and solved using SHELXL-97 program3. The compound crystallized in monoclinic crystalline system in space group P21/c, cell parameters: a=9.2502(6) Å, b= 15.0004(6) Å, c=9.2947(4) Å, β= 108.4590(6), V=1223,35 Å3and Z=4. The final statistical parameters of the structure refinement were R=0.0326, wR=0.0835 and S=1,053. In this compound the BTC and INH ligands are coordinated like a bridge to two zinc ions. The BTC forms chelates by two carboxylate groups and INH coordinates by pyridine ring and by chelate at hydrazide group. This polymer extends in only one direction along a axis forming a 1D network. There is only one metallic zinc ion crystallographically independent on structure, it is in a distorted octahedral geometry with oxygen and nitrogen atoms of ligands and one coordinated water molecule in its coordination sphere. The 1D network formed by coordination polymers stabilizes the crystalline arrangement by hydrogen bonds between carboxylate and hydrazide groups and coordinated water molecules.
Read more21Bulk crystal growth and their effective third order nonlinear optical properties of 2-(4-fluorobenzylidene) malononitrile (FBM) single crystal
Bulk crystal growth and their effective third order nonlinear optical properties of 2-(4-fluorobenzylidene) malononitrile (FBM) single crystal
Read more7Growth and characterization of glycine sodium nitrate (GSN) single crystal
Good optical quality single crystals of glycine sodium nitrate (GSN) were grown by slow evaporation technique from its aqueous solution at room temperature. Single crystal X-ray diffraction (XRD) studies revealed the presence of monoclinic structure with space group Cc, and Fourier transform infrared transmission (FTIR) has confirmed the presence of the functional groups present in the single crystal system. The thermal stability of the crystal was studied by Thermogravimetric/Differential Thermal Analyzer (TG/DTA). Ultraviolet (UV) spectrum showed no significant absorption in the region 200-2000 nm suggesting the optical transparency of the grown crystals. Key words: Single crystal, solution growth, X-ray diffraction (XRD), thermogravimetric/differential thermal analyzer (TG/DTA).
Read more19Synthesis and characterization of new fluoride-containing manganese vanadates A2Mn2V2O7F2 (A=Rb, Cs) and Mn2VO4F
Synthesis and characterization of new fluoride-containing manganese vanadates A2Mn2V2O7F2 (A=Rb, Cs) and Mn2VO4F
5Growth and characterization of Fe:Ti:Al2O3 single crystal by floating zone method
Growth and characterization of Fe:Ti:Al2O3 single crystal by floating zone method
10(C 5H 16N 2)·[Zn 3(HPO 3) 4]·H 2O: A new three-dimensional zincophosphite with 12-membered ring channels and infinite edge shared 4-membered ring ladders
(C 5H 16N 2)·[Zn 3(HPO 3) 4]·H 2O: A new three-dimensional zincophosphite with 12-membered ring channels and infinite edge shared 4-membered ring ladders
Read more25Syntheses and Characterization of Two New Open-Framework Zinc Phosphites with 12-Ring Channels, [H3N(CH2)4NH3]·[Zn3(HPO3)4]·H2O and [C3N2H5]2·[Zn3(HPO3)4
Two new organically templated zinc phosphites, [H3N(CH2)4NH3]·[Zn3(HPO3)4]·H2O (1) and [C3N2H5]2·[Zn3(HPO3)4] (2) have been synthesized under mild hydrothermal conditions. Their structures were determined by single-crystal X-ray diffraction and further characterized by FTIR, elemental analysis, inductively coupled plasma (ICP) analysis, powder X-ray diffraction, and thermogravimetric analysis. In addition to the same anionic framework compositions of [Zn3(HPO3)4]2-, both phases consist of strictly alternating ZnO4 tetrahedra and HPO3 pseudo-pyramids linked through their vertexes to generate the three-dimensional frameworks with intersecting 8- and 12-membered ring channels, where the template molecules reside. Compound 1 crystallizes in the triclinic system, space group P1 with the following cell parameters: a = 7.7703(4) A; b = 9.1499(4) A; c = 14.4685(3) A; α = 89.965(2)°; β = 87.050(2)°; γ = 65.332(2)°; V = 933.31(7) A3; Z = 2. Compound 2 crystallizes in the triclinic system, space group P1 with the...
Read more60Application of a Mild Hydrothermal Approach Containing an in Situ Reduction Step to the Growth of Single Crystals of the Quaternary U(IV)-Containing Fluorides Na4MU6F30 (M = Mn2+, Co2+, Ni2+, Cu2+, and Zn2+) Crystal Growth, Structures, and Magnetic Properties
A family of rare U(IV)-containing quaternary fluorides, Na4MU6F30 (M = Mn(2+), Co(2+), Ni(2+), Cu(2+), and Zn(2+)), was synthesized in single crystal form via a mild hydrothermal technique utilizing an in situ U(VI) to U(IV) reduction step. The modified hydrothermal route is described, and the conditions to obtain single crystals in high yield are detailed. The crystal structures were determined by single crystal X-ray diffraction. The isostructural fluorides crystallize in a new structure type in the trigonal space group P3̅c1. They exhibit a complex three-dimensional crystal structure consisting of corner- and edge-shared UF9 and MF6 polyhedra. The main building block, a U6F30(6-) group, is arranged to create two distinct hexagonal channels, inside which MF6 octahedra and Na(+) cations are located. The copper-containing member of the series, Na4CuU6F30, is unusual in that the Cu(2+) cation exhibits a rare symmetrical coordination environment consisting of six identical Cu-F bond distances, indicating the lack of the expected Jahn-Teller distortion. Magnetic susceptibility measurements of Na4ZnU6F30 yielded an effective magnetic moment of 3.42 μB for the U(4+) (f(2)) cation in the structure. Measurements of the other members containing magnetic transition-metal cations in addition to U(4+), Na4MU6F30 (M = Mn(2+), Co(2+), Ni(2+), and Cu(2+)) yielded total effective magnetic moments of 10.2, 9.84, 8.87, and 8.52 μB for the Mn-, Co-, Ni-, and Cu-containing materials, respectively. No evidence for long-range magnetic ordering was found down to 2 K. Measurements of the magnetization as a function of applied magnetic field at 2 K for Na4MnU6F30 confirmed that the U(4+) magnetic cation exhibits a nonmagnetic singlet ground state at low temperature. Thermal stability measurements and UV-vis diffuse reflectance spectroscopy are also reported.
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