Hydrated Cs+-Exchanged MFI Zeolites:  Location and Population of Cs+Cations and Water Molecules in Hydrated Cs6.6MFI from In and Ex Situ Powder X-ray Diffraction Data as a Function of Temperature and Other Experimental Conditions

2006 ◽  
Vol 110 (28) ◽  
pp. 13741-13752 ◽  
Author(s):  
Bernard F. Mentzen ◽  
Gérard Bergeret ◽  
Hermann Emerich ◽  
Hans-Peter Weber
2021 ◽  
Vol 12 (1) ◽  
Author(s):  
Giulio I. Lampronti ◽  
Adam A. L. Michalchuk ◽  
Paolo P. Mazzeo ◽  
Ana M. Belenguer ◽  
Jeremy K. M. Sanders ◽  
...  

AbstractTime resolved in situ (TRIS) monitoring has revolutionised the study of mechanochemical transformations but has been limited by available data quality. Here we report how a combination of miniaturised grinding jars together with innovations in X-ray powder diffraction data collection and state-of-the-art analysis strategies transform the power of TRIS synchrotron mechanochemical experiments. Accurate phase compositions, comparable to those obtained by ex situ measurements, can be obtained with small sample loadings. Moreover, microstructural parameters (crystal size and microstrain) can be also determined with high confidence. This strategy applies to all chemistries, is readily implemented, and yields high-quality diffraction data even using a low energy synchrotron source. This offers a direct avenue towards the mechanochemical investigation of reactions comprising scarce, expensive, or toxic compounds. Our strategy is applied to model systems, including inorganic, metal-organic, and organic mechanosyntheses, resolves previously misinterpreted mechanisms in mechanochemical syntheses, and promises broad, new directions for mechanochemical research.


1991 ◽  
Vol 56 (7) ◽  
pp. 1454-1460 ◽  
Author(s):  
Jaroslav Podlaha ◽  
Jana Podlahová

The crystal structure of the title compound containing a phosphorus analogue of EDTA as the ligand was determined from single-crystal X-ray diffraction data and refined to R = 0.028 for 1 920 observed reflections. The crystals are monocyclic, space group P21/c,a = 8.6169(8), b = 16.0539(9), c = 8.2504(6)Å, β = 103.458(7)° and Z = 2. The structure is completely different from that of the nitrogen prototype, [CdEDTA]2-. It consists of double-stranded polymeric layers which are composed of metal coordination polyhedra linked by μ6-hexadentate ligands; the layers lie parallel to the bc plane and are joined along the a axis through hydrogen bonding donated by water molecules. Because of steric requirements of phosphorus, the coordination polyhedron around Cd is greatly distorted and can best be described as a 5 + 3 type. One P atom, two oxygen atoms from two monodentate carboxylate groups and two water molecules form an approximate trigonal bipyramid and further three more remote carboxylate oxygens complete the arrangement, resulting in an O7P distorted bicapped trigonal prism.


1998 ◽  
Vol 54 (4) ◽  
pp. 464-470 ◽  
Author(s):  
T. Steiner

For 71 water molecules donating two Ow—H...O hydrogen bonds, the correlation of the covalent H—O—H angle and the O...Ow...O angle is inspected from 49 well refined organic and organometallic neutron diffraction crystal structures. Compared to sample average, the water angle is opened for large and narrowed for small O...Ow...O angles. Notably, the H—O—H angle is widened compared with the gas phase value even for small O...Ow...O. Related behavior is observed for chloride anion acceptors. The correlation exhibits a considerable scatter which should not be interpreted as experimental inaccuracies, but as secondary effects. Possible secondary effects are multi-center hydrogen bonding and effects of coordination to the water O atom. In a comparative test, low-temperature X-ray diffraction data were shown to be completely unsuitable for this type of analysis. The dependence of the C—O—H angle on the C—O...O angle in hydrogen bonds donated by hydroxyl groups in carbohydrates is also shown.


2021 ◽  
Author(s):  
Giulio I. Lampronti ◽  
Adam Michalchuk ◽  
Paolo P. Mazzeo ◽  
Ana Belenguer ◽  
Jeremy K. M. Sanders ◽  
...  

<p>Time resolved in situ (TRIS) monitoring has revolutionised the study of mechanochemical transformations but has been limited by available data quality. We report how a combination of new miniaturised grinding jars together with innovations in X-ray powder diffraction data collection and state-of-the-art analysis strategies transform the power of TRIS synchrotron mechanochemical experiments. Accurate phase compositions, comparable to those obtained by <i>ex situ</i> measurements, can be obtained with small sample loadings. Moreover, microstructural parameters (crystal size and microstrain) can be also determined with high confidence. This strategy applies to all chemistries, is readily implemented, and yields high-quality diffraction data even using a low energy synchrotron source. This offers a direct avenue towards the mechanochemical investigation of reactions comprising scarce, expensive, or toxic compounds. Our strategy is applied to model systems, including inorganic, metal-organic, and organic mechanosyntheses, resolves previously misinterpreted mechanisms in mechanochemical syntheses, and promises broad, new directions for mechanochemical research.<b></b></p>


2016 ◽  
Vol 69 (11) ◽  
pp. 1261 ◽  
Author(s):  
Masoumeh Tabatabaee ◽  
Boris-Marko Kukovec ◽  
Saeed Amjad ◽  
Masoud R. Shishebor

Two novel barium(ii) 2D coordination polymers, {[Ba(µ-H2O)(H2O)2(µ-pyzdc)]}n (1) and {[Ba(H2O)2(µ-Hpyzdc)(Hpyzdc)]⋅2H2O}n (2) (pyzdcH2 = pyrazine-2,3-dicarboxylic acid), were prepared by reaction of barium(ii) chloride dihydrate and pyrazine-2,3-dicarboxylic acid under similar experimental conditions (slightly different pH values) and characterised by elemental analysis, IR spectroscopy, and thermogravimetric analysis/differential thermal analysis methods. Their crystal structures were determined by single-crystal X-ray structure analysis and it was revealed that the barium(ii) ion has a distorted bicapped square antiprismatic coordination geometry in 1 and a distorted tricapped trigonal prismatic geometry in 2, composed of water molecules, carboxylate O, and pyrazine N atoms in both cases. The polymers 1 and 2 have different connectivity, as the pyrazine-2,3-dicarboxylate ion acts as multidentate bridging ligand in both 1 and 2, but also as an N,O′-bidentate terminal ligand in 2. There are terminal coordinated water molecules in both 1 and 2, but bridging water molecules are present only in 1 and water molecules of crystallisation only in 2. BaCO3 nanoparticles were formed by thermal decomposition of 1 in the presence of polyethylene glycol, and their structure and morphology were studied by powder X-ray diffraction and scanning electron microscopy. According to the powder X-ray diffraction pattern, BaCO3 was formed with an orthorhombic witherite structure.


2021 ◽  
Author(s):  
Giulio I. Lampronti ◽  
Adam Michalchuk ◽  
Paolo P. Mazzeo ◽  
Ana Belenguer ◽  
Jeremy K. M. Sanders ◽  
...  

<p>Time resolved in situ (TRIS) monitoring has revolutionised the study of mechanochemical transformations but has been limited by available data quality. We report how a combination of new miniaturised grinding jars together with innovations in X-ray powder diffraction data collection and state-of-the-art analysis strategies transform the power of TRIS synchrotron mechanochemical experiments. Accurate phase compositions, comparable to those obtained by <i>ex situ</i> measurements, can be obtained with small sample loadings. Moreover, microstructural parameters (crystal size and microstrain) can be also determined with high confidence. This strategy applies to all chemistries, is readily implemented, and yields high-quality diffraction data even using a low energy synchrotron source. This offers a direct avenue towards the mechanochemical investigation of reactions comprising scarce, expensive, or toxic compounds. Our strategy is applied to model systems, including inorganic, metal-organic, and organic mechanosyntheses, resolves previously misinterpreted mechanisms in mechanochemical syntheses, and promises broad, new directions for mechanochemical research.<b></b></p>


Author(s):  
M. E. Twigg ◽  
B. R. Bennett ◽  
J. R. Waterman ◽  
J. L. Davis ◽  
B. V. Shanabrook ◽  
...  

Recently, the GaSb/InAs superlattice system has received renewed attention. The interest stems from a model demonstrating that short period Ga1-xInxSb/InAs superlattices will have both a band gap less than 100 meV and high optical absorption coefficients, principal requirements for infrared detector applications. Because this superlattice system contains two species of cations and anions, it is possible to prepare either InSb-like or GaAs-like interfaces. As such, the system presents a unique opportunity to examine interfacial properties.We used molecular beam epitaxy (MBE) to prepare an extensive set of GaSb/InAs superlattices grown on an GaSb buffer, which, in turn had been grown on a (100) GaAs substrate. Through appropriate shutter sequences, the interfaces were directed to assume either an InSb-like or GaAs-like character. These superlattices were then studied with a variety of ex-situ probes such as x-ray diffraction and Raman spectroscopy. These probes confirmed that, indeed, predominantly InSb-like and GaAs-like interfaces had been achieved.


2010 ◽  
Vol 6 (1) ◽  
pp. 891-896
Author(s):  
Manel Halouani ◽  
M. Dammak ◽  
N. Audebrand ◽  
L. Ktari

One nickel 1,4-cyclohexanedicarboxylate coordination polymers, Ni2 [(O10C6H4)(COO)2].2H2O  (I), was hydrothermally synthesized from an aqueous solution of Ni (NO3)2.6H2O, (1,4-CDC) (1,4-CDC = 1,4-cyclohexanedicarboxylic acid) and tetramethylammonium nitrate. Compound (I) crystallizes in the monoclinic system with the C2/m space group. The unit cell parameters are a = 20.1160 (16) Å, b = 9.9387 (10) Å, c = 6.3672 (6) Å, β = 97.007 (3) (°), V= 1263.5 (2) (Å3) and Dx= 1.751g/cm3. The refinement converged into R= 0.036 and RW = 0.092. The structure, determined by single crystal X-ray diffraction, consists of two nickel atoms Ni (1) and Ni (2). Lots of ways of which is surrounded by six oxygen atoms, a carboxyl group and two water molecules.


2019 ◽  
Vol 74 (4) ◽  
pp. 357-363
Author(s):  
Daniela Vitzthum ◽  
Hubert Huppertz

AbstractThe mixed cation triel borate Ga4In4B15O33(OH)3 was synthesized in a Walker-type multianvil apparatus at high-pressure/high-temperature conditions of 12.5 GPa and 1300°C. Although the product could not be reproduced in further experiments, its crystal structure could be reliably determined via single-crystal X-ray diffraction data. Ga4In4B15O33(OH)3 crystallizes in the tetragonal space group I41/a (origin choice 2) with the lattice parameters a = 11.382(2), c = 15.244(2) Å, and V = 1974.9(4) Å3. The structure of the quaternary triel borate consists of a complex network of BO4 tetrahedra, edge-sharing InO6 octahedra in dinuclear units, and very dense edge-sharing GaO6 octahedra in tetranuclear units.


1984 ◽  
Vol 140 (2-3) ◽  
pp. 202-205 ◽  
Author(s):  
Walter Morisset ◽  
Werner Wehrmeyer ◽  
Tilman Schirmer ◽  
Wolfram Bode

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