scholarly journals A novel layered aluminophosphate with corner-sharing AlO6chains

2014 ◽  
Vol 70 (a1) ◽  
pp. C993-C993
Author(s):  
Fernando Cámara ◽  
Linda Pastero ◽  
Rossella Arletti ◽  
Monica Cagnoni

The synthesis, Raman spectroscopy and crystal structure of a novel layered aluminophosphate is described. The new phase was derived by the sol-gel method starting from a modified low hydrothermal ALPO4-34 zeolite synthesis procedure[1].The structure was solved by direct methods using single-crystal X-ray diffraction. The synthesized layered material, with composition [AlPO3(OH)F(H2O)]-(H9C4ON), crystallizes in the monoclinic space group P21/a with a = 9.2282(5) Å, b = 6.9152(4) Å, c = 14.4615(9) Å, β = 101.57(1)0. Layered aluminophosphates with AlO6polyhedra have been previously described [2], although in these compounds Al octahedral share edges. The novel compound has corner sharing AlO4F(H2O) chains along [010], where fluorine is at the shared apex, four oxygen atoms are shared with PO4tetrahedra and the fifth oxygen is a H2O group. This kind of aluminophosphate chains is found in nature in tancoite [3]. Chains are linked along [100] through corner sharing with a PO4group of the adjacent chain plus hydrogen bonding of the H2O group. Layers are stacked along c* through hydrogen bonding with a double layer of morpholine (H9C4ON) molecules. The chemical stability field of the novel materialis strongly dependent from the fluorine/aluminum ratio of the starting gel. At lower fluorine concentrations only ALPO4-34 and/or AlPO4(berlinite) are stable depending on the morpholine content. Crystals growth morphology depends on the supersaturation conditions of the starting gel: at low concentrations crystals are well developed hexagonal like plate shaped and are very thin. At higher concentrations they show a more elongated morphology. A treatment with H2CO3leads to a complete morpholine removal, as shown by in situ Raman spectroscopy. Powder X-ray diffraction reveals that after morpholine extraction, the material diffract still coherently in two dimensions while a strong broadening is shown for basal planes.

1993 ◽  
Vol 58 (12) ◽  
pp. 2924-2935 ◽  
Author(s):  
Jane H. Jones ◽  
Bohumil Štíbr ◽  
John D. Kennedy ◽  
Mark Thornton-Pett

Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11] in boiling toluene solution results in an elimination of the platinum centre and cluster closure to give the ten-vertex closo species [6-(PMe2Ph)-closo-1-CB9H9] in 85% yield as a colourles air stable solid. The product is characterized by NMR spectroscopy and single-crystal X-ray diffraction analysis. Crystals (from hexane-dichloromethane) are monoclinic, space group P21/c, with a = 903.20(9), b = 1 481.86(11), c = 2 320.0(2) pm, β = 97.860(7)° and Z = 8, and the structure has been refined to R(Rw) = 0.045(0.051) for 3 281 observed reflections with Fo > 2.0σ(Fo). The clean high-yield elimination of a metal centre from a polyhedral metallaborane or metallaheteroborane species is very rare.


2007 ◽  
Vol 63 (11) ◽  
pp. i186-i186 ◽  
Author(s):  
Stanislav Ferdov ◽  
Uwe Kolitsch ◽  
Christian Lengauer ◽  
Ekkehart Tillmanns ◽  
Zhi Lin ◽  
...  

The structure of the layered noncentrosymmetric titanosilicate AM-1 (also known as JDF-L1, disodium titanium tetrasilicate dihydrate), Na4Ti2Si8O22·4H2O, grown as small single crystals without the use of organics, has been refined from single-crystal X-ray diffraction data. The H atom has been located for the first time, and the hydrogen-bonding scheme is also characterized by IR and Raman spectroscopy. All atoms are in general positions except for the Na, the Ti, one Ti-bound O, one Si-bound O and the water O atoms (site symmetries 2, 4, 4, 2 and 2, respectively).


1980 ◽  
Vol 35 (7) ◽  
pp. 824-831 ◽  
Author(s):  
Hans Georg von Schnering ◽  
Manfred Wittmann

The novel polyphosphide EuP7 was prepared under controlled conditions by the reaction of the elements in salt melts at 750-800 K. EuP7 forms black prismatic crystals not attacked by diluted mineral acids and bases. The thermal decomposition yields EuP3 at 700 K and in further steps EuP2, Eu3P4 and EuP, respectively. According to the crystal structure as well as the electrical, optical and magnetic properties EuP7 is a semiconductor (EG = 0.9 eV; EG (vert) = 1.1 eV) with divalent europium (μ = 7.55 B.M.). The compound crystallizes in the monoclinic space group P21/n with a = 1148.8(7) pm, b = 570.0(3) pm, c = 1061.0(6) pm, and β= 106.08°(5); (X-ray diffraction data; 1479 hkl, R = 0.031). The P-atoms are connected (P-P) = 218.0-223.5 pm) to a 2-dimensional infinite polyanionic structure with homonuclear 3-bonded and 2-bonded P-atoms in the ratio 5:2. The polyanionic network contains P6-rings (chair conformation) as well as P8-rings and P10-rings. The Eu-atoms are bonded to 9 P-atoms (1,4,4-polyhedra) with bond distances ranging from 306.6 to 326.6 pm. The Eu-atoms complete the tetrahedral environment of the P-atoms


1997 ◽  
Vol 12 (6) ◽  
pp. 1441-1444 ◽  
Author(s):  
L. Armelao ◽  
A. Armigliato ◽  
R. Bozio ◽  
P. Colombo

The microstructure of Fe2O3 sol-gel thin films, obtained from Fe(OCH2CH3)3, was investigated by x-ray diffraction (XRD), transmission electron microscopy (TEM), and Raman spectroscopy. Samples were nanocrystalline from 400 °C to 1000 °C, and the crystallized phase was haematite. In the coatings, the α–Fe2O3 clusters were dispersed as single particles in a network of amorphous ferric oxide.


2018 ◽  
Vol 2018 ◽  
pp. 1-7 ◽  
Author(s):  
Tanat Chokpanyarat ◽  
Vittaya Punsuvon ◽  
Supakit Achiwawanich

The novel three-dimensionally ordered macroporous (3DOM) CaO/SiO2, 3DOM CaO/Al2O3, and 3DOM Ca12Al14O32Cl2 catalysts for biodiesel transesterification were prepared by sol-gel method. The 3DOM catalysts were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR). The hierarchical porous structure was achieved; however, only 3DOM CaO/Al2O3 and 3DOM Ca12Al14O32Cl2 catalysts were used for transesterification due to high amount of active CaO. Various parameters such as methanol to oil molar ratio, catalyst concentration, reaction time, and their influence on the biodiesel production were studied. The result showed that 99.0% RPO conversion was achieved using the 3DOM Ca12Al14O33Cl2 as a catalyst under the optimal condition of 12 : 1 methanol to oil molar ratio and 6 wt.% catalyst with reaction time of 3 hours at 65°C.


2017 ◽  
Vol 1 (4) ◽  
pp. 737-747 ◽  
Author(s):  
W. Zhu ◽  
A. Paolella ◽  
C.-S. Kim ◽  
D. Liu ◽  
Z. Feng ◽  
...  

In liithium–sulfur battery the lithium metal surface was analyzed by in situ Raman spectroscopy.


2005 ◽  
Vol 19 (01n03) ◽  
pp. 671-673
Author(s):  
PENG XIAO ◽  
WANLU WANG

The Fe 3+- TiO 2 thin films obtained through sol-gel method were characterized by x-ray diffraction, AFM and Raman spectroscopy. It was found that TiO 2 films consisted of nanometer particles. The experimental results shows that the nanometer TiO 2 thin films doped with Fe 3+ were greatly improved in the activity aspect. This may be ascribed to change their structure and electrical properties after doping with Fe 3+. The results were discussed theoretically in detail.


1997 ◽  
Vol 52 (8) ◽  
pp. 901-905 ◽  
Author(s):  
Vera V Ponomareva ◽  
Victor V Skopenko ◽  
Konstantin V Domasevitch ◽  
Joachim Sieler ◽  
Thomas Gelbrich

Abstract The caesium hydrogen benzoylcyanoximate (L-) complex with 18-crown-6 of composition Cs(18-crown-6){H(L)2} has been prepared and studied by means of X-ray diffraction [monoclinic, space group P21/n, with a = 9.906(1), b = 18.387(3), c = 18.855(3)Å, β = 90.13(1)°, V = 3434.3(9) Å, Z = 4; final R1 = 0.043 for the 6431 independent reflections used. The lattice consists of Cs(18-crown-6)+ cations and complex hydrogen oximate anions {H(L)2}-, formed via strong hydrogen bonding between the oxygen atoms of nitroso-groups [O - - - O ca. 2.456(5)Å]. The caesium atom deviates by 1.492(3) Å from the mean plane of the oxygen atoms of the macrocyclic ether (dominant orientation of disordered ligand, 60%) and adopts a typical “sunrise coordination” [Cs-O (ether) 3.040(9)-3.312(7) Å]. The hydrogen oximate groups are bonded to the metal center only on one side of the crown ether plane via the oxygen atoms of nitroso-groups and the nitrogen atoms of cyano groups (Cs-O ca. 3.040(9), 3.312(7) Å; Cs-N ca. 3.469(5), 3.679(6) Å). The coordination polyhedron of Cs+ can be described as a distorted bicapped tetragonal prism.


2013 ◽  
Vol 70 (1) ◽  
pp. 12-15 ◽  
Author(s):  
Patrice Kenfack Tsobnang ◽  
Emmanuel Wenger ◽  
Siméon Ponou ◽  
Slimane Dahaoui ◽  
John Lambi Ngolui ◽  
...  

The title compound, [KCr(C2O2)2(C6H8N2)]n, was obtained from aqueous solution and analyzed with single-crystal X-ray diffraction at 100 K. It crystallizes in the monoclinic space groupC2/cand displays a three-dimensional polymeric architecture built up by bimetallic oxalate-bridged CrIII–K helical chains linked through centrosymmetric K2O2units to yield a sheet-like alternatingP/Marrangement which looks like that of the previously described two-dimensional [NaCr(ox)2(pyim)(H2O)]·2H2O [pyim is 2-(pyridin-2-yl)imidazole; Leiet al.(2006).Inorg. Chem. Commun.9, 486–488]. The CrIIIions in each helix have the same chirality. The infinite neutral sheets are eclipsed with respect to each other and are held together by a hydrogen-bonding network involving 2-(aminomethyl)pyridine H atoms and oxalate O atoms. Each sheet gives rise to channels of Cr4K4octanuclear rings and each resultant hole is occupied by a pair of 2-(aminomethyl)pyridine ligands with partial overlap. The shortest Cr...Cr distance [5.593 (4) Å] is shorter than usually observed in the K–MIII–oxalate family.


ChemInform ◽  
2013 ◽  
Vol 44 (47) ◽  
pp. no-no
Author(s):  
Jing Zhou ◽  
Guanlin Feng ◽  
Liang Li ◽  
Fengxian Huang ◽  
Hongzhi Shen ◽  
...  

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