Structural intergrowth of merlinoite/phillipsite and its temperature-dependent dehydration behaviour: a single-crystal X-ray study

2015 ◽  
Vol 79 (1) ◽  
pp. 191-203 ◽  
Author(s):  
Rosa Micaela Danisi ◽  
Thomas Armbruster ◽  
Mariko Nagashima
Keyword(s):  
Single Crystal ◽  
Unit Cell Volume ◽  
Structure Refinement ◽  
Ambient Conditions ◽  
X Ray Diffraction ◽  
Temperature Dependent ◽  
X Ray ◽  
Khibiny Massif ◽  
Low Symmetry

AbstractSupposed 'merlinoite' crystals from Monte Somma, Vesuvius (Italy) and Fosso Attici, north of Rome (Italy) represent highly twinned coherent intergrowths between merlinoite and phillipsite on a submicroscopic level. The MER (Immm, a ≈ 14.1, b ≈ 14.2, c ≈ 9.9 Å) and PHI (P 21/m, a ≈ 9.9, b ≈ 14.3, c ≈ 8.7 Å, β = 124.8°) frameworks of similar composition are assembled from identical tetrahedral units, though with a different connectivity. Coherent intergrowth and twinning of the two frameworks lead to P42/mnm pseudosymmetry, which is diagnostic of the intergrowth. Under ambient conditions merlinoite has Immm symmetry or I4/mmm if twinned. a low-symmetry model of space group P121/m1 (a ≈ 14.2, b ≈ 14.2, c ≈ 10 Å, β = 90°) allows structure refinement and quantification of the two frameworks.Upon in situ dehydration to 250°C the evolution of the unit-cell volume of the Monte Somma merlinoite/phillipsite intergrowth displays an intermediate trend between previously studied pure merlinoite from the Khibiny massif (Russia) and Ba-rich phillipsite.The Monte Somma crystal studied by temperature-dependent single-crystal X-ray diffraction methods also contained a subordinate chabazite inclusion with no coherent structural relationship to the merlinoite/phillipsite framework. Thus, the modification of the chabazite framework on dehydration could also be studied.

The low-temperature behaviour of cancrinite:an in situ single-crystal X-ray diffraction study

2012 ◽  
Vol 76 (4) ◽  
pp. 933-948 ◽  
Author(s):  
G. Diego Gatta ◽  
P. Lotti ◽  
V. Kahlenberg ◽  
U. Haefeker
Keyword(s):  
Low Temperature ◽  
Single Crystal ◽  
Structure Refinement ◽  
Ambient Conditions ◽  
X Ray Diffraction ◽  
Structural Behaviour ◽  
X Ray ◽  
Positional Disorder ◽  
Deformation Processes

AbstractThe low-temperature structural behaviour of natural cancrinite with a formula Na6.59Ca0.93[Si6.12Al5.88O24](CO3)1.04F0.41·2H2O has been investigated by means of in situ single-crystal X-ray diffraction and Raman spectroscopy. High quality structure refinements were obtained at 293, 250, 220, 180, 140, 100 and at 293 K again (at the end of the low-T experiments). The variation in the unit-cell volume as a function of temperature (T) exhibits a continuous trend, without any evident thermoelastic anomaly. The thermal expansion coefficient αV = (1/V)∂V/∂T is 3.8(7) × 10–5 K–1 (between 100 and 293 K). The structure refinement based on intensity data collected at ambient conditions after the low-T experiment confirmed that the low-T induced deformation processes are completely reversible. The extraframework population does not show significant variations down to 100 K. The strong positional disorder of the carbonate groups along the c axis persists within the T range investigated. The structural behaviour of cancrinite at low-T is mainly governed by the continuous framework rearrangement through the ditrigonalization of the six-membered rings which lie in a plane perpendicular to [0001], the contraction of the four-membered ring joint units, the decrease of the ring corrugation in the (0001) plane, and the flattening of the cancrinite cages. A list of the principal Raman active modes in ambient conditions is provided and discussed.

Molecular motions of a tetraphenylethylene-derived AIEgen directly monitored through in situ variable temperature single crystal X-ray diffraction

CrystEngComm ◽  
2021 ◽  
Author(s):  
Wei Meng ◽  
Lin Du ◽  
Lin Sun ◽  
Lian Zhou ◽  
Xiaopeng Xuan ◽  
...  
Keyword(s):  
Single Crystal ◽  
Phenyl Ring ◽  
Functional Group ◽  
Variable Temperature ◽  
Molecular Motions ◽  
X Ray Diffraction ◽  
Temperature Dependent ◽  
X Ray ◽  
Conformation Changes

One organic functional group was introduced to distinguish the four phenyl ring of tetraphenylethylene, and the In situ temperature-dependent crystal structures were determined to exhibit the conformation changes of tert-butyl...

scholarly journals Crystal structure refinement of MgSiO3high temperature C2/c clinoenstatite

2014 ◽  
Vol 70 (a1) ◽  
pp. C79-C79
Author(s):  
Akira Yoshiasa ◽  
Akihiko Nakatsuka ◽  
Maki Okube ◽  
Tomoo Katsura
Keyword(s):  
High Temperature ◽  
Single Crystal ◽  
Structure Refinement ◽  
Ambient Conditions ◽  
X Ray Diffraction ◽  
Temperature Quenching ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
Metastable Structure ◽  
Rapid Pressure

The high-temperature clinoenstatite (HT-CEn) is one of the important MgSiO3 pyroxene polymorph. The single-crystal of C2/c HT-CEn endmember is firstly synthesized by rapid pressure-temperature quenching from 15-16 GPa and 900-19000C [1]. No report that it is produced as single crystal or large domain has been made on the MgSiO3 endmember. The HT-CEn-type modifications are observed in Ca-poor Mg-Fe clinoenstatite and pigeonite and are always found to be unquenchable in rapid cooling. The high pressure and high temperature experiments of MgSiO3 composition were carried out with a Kawai-type multi-anvil apparatus. The samples were quenched by rapidly releasing the oil pressure load and/or by blow out of anvil cell gasket. The space group of C2/c is strictly determined by Rigaku RAPID Weissenberg photographs and synchrotron radiation. Single-crystal X-ray diffraction experiments were performed at ambient conditions using a Rigaku AFC-5 four circle diffractometer. A total of 9383 reflections was measured and averaged in Laue symmetry 2/m to give 766 independent reflections used for the structure refinements. Final reliability factors converged smoothly to R = 0.029. The single-crystal diffraction analysis shows that the unusual bonding distances frozen in this metastable structure. The degree of kinking of the silicate tetrahedral chains is 1750for HT-CEn. The chain angle for HP-CEn is substantially smaller (1350) and the angle for L-CEn turned to the opposite direction at -1600(=2000). The degree of kinking increases by being curved in more than 1800in the transition from HT-CEn to L-CEn. As for the reverse change from the expansion to the stretch, a potential barrier exists in the point of the continuity. It is suggested that the reason which can quench structure under ambient conditions is the present HT-CEn single crystal was formed by the isosymmetric phase transition from HP-CEn. HT-CEn type single-crystals cannot be frozen without pressure.

Armstrongite at non-ambient conditions: An in-situ high-pressure single-crystal X-ray diffraction study

2019 ◽  
Vol 274 ◽  
pp. 171-175 ◽  
Author(s):  
Davide Comboni ◽  
Paolo Lotti ◽  
G. Diego Gatta ◽  
Maria Lacalamita ◽  
Ernesto Mesto ◽  
...  
Keyword(s):  
High Pressure ◽  
Single Crystal ◽  
Diffraction Study ◽  
Ambient Conditions ◽  
X Ray Diffraction ◽  
X Ray

In situ high temperature single crystal X-ray diffraction study of a natural omphacite

2000 ◽  
Vol 64 (6) ◽  
pp. 983-993 ◽  
Author(s):  
A. Pavese ◽  
R. Bocchio ◽  
G. Ivaldi
Keyword(s):  
High Temperature ◽  
Single Crystal ◽  
Diffusion Processes ◽  
Ambient Conditions ◽  
X Ray Diffraction ◽  
Structural Behaviour ◽  
X Ray ◽  
Thermal Expansion Coefficients ◽  
Using Data

AbstractIn situ high temperature single crystal X-ray diffraction (XRD) experiments have been performed on a chemically quasi-ideal omphacite sample up to 1000°C. The lattice parameters were studied as a function of temperature, and their thermal expansion coefficients determined. The b and c cell edges show discontinuities as a function of temperature which are interpreted here in terms of intracrystalline cation diffusion processes. Structure refinements have been carried out using data collected at room temperature, at 800°C and at ambient conditions after cooling. The structural behaviour as a function of temperature of chemically quasi-ideal omphacites is compared with those of jadeite and diopside.

Dehydration of the zeolite merlinoite from the Khibiny massif, Russia: an in situ temperature-dependent single-crystal X-ray study

2014 ◽  
Vol 26 (3) ◽  
pp. 371-380 ◽  
Author(s):  
Anna S. Pakhomova ◽  
Thomas Armbruster ◽  
Sergey V. Krivovichev ◽  
Victor N. Yakovenchuk
Keyword(s):  
Single Crystal ◽  
Temperature Dependent ◽  
X Ray ◽  
Khibiny Massif

Ternary Antimonides RE4T7Sb6 (RE=Gd–Lu; T =Ru, Rh) with Cubic U4Re7Si6-type Structure

2013 ◽  
Vol 68 (9) ◽  
pp. 971-978 ◽  
Author(s):  
Inga Schellenberg ◽  
Ute Ch. Rodewald ◽  
Christian Schwickert ◽  
Matthias Eul ◽  
Rainer Pöttgen
Keyword(s):  
Magnetic Susceptibility ◽  
Single Crystal ◽  
Magnetic Moment ◽  
Induction Furnace ◽  
X Ray Diffraction ◽  
Temperature Dependent ◽  
X Ray ◽  
Antiferromagnetic Ordering ◽  
Arc Melting ◽  
Intermediate Valent

The ternary antimonides RE4T7Sb6 (RE=Gd-Lu; T =Ru, Rh) have been synthesized from the elements by arc-melting and subsequent annealing in an induction furnace. The samples have been characterized by powder X-ray diffraction. Four structures were refined on the basis of single-crystal X-ray diffractometer data: U4Re7Si6 type, space group Im3m with a=862.9(2) pm, wR2=0.0296, 163 F2 values for Er4Ru7Sb6; a=864.1(1) pm, wR2=0.1423, 153 F2 values for Yb4Ru7Sb6; a=872.0(2) pm, wR2=0.0427, 172 F2 values for Tb4Rh7Sb6; and a=868.0(2) pm, wR2=0.0529, 154 F2 values for Er4Rh7Sb6, with 10 variables per refinement. The structures have T1@Sb6 octahedra and slightly distorted RE@T26Sb6 cuboctahedra as building units. The distorted cuboctahedra are condensed via all trapezoidal faces, and this network leaves octahedral voids for the T1 atoms. The ruthenium-based series of compounds was studied by temperature-dependent magnetic susceptibility measurements. Lu4Ru7Sb6 is Pauli-paramagnetic. The antimonides RE4Ru7Sb6 with RE=Dy, Ho, Er, and Tm show Curie-Weiss paramagnetism. Antiferromagnetic ordering occurs at 10.0(5), 5.1(5) and 4.0(5) K for Dy4Ru7Sb6, Ho4Ru7Sb6 and Er4Ru7Sb6, respectively, while Tm4Ru7Sb6 remains paramagnetic. Yb4Ru7Sb6 is an intermediate-valent compound with a reduced magnetic moment of 3.71(1) μB per Yb as compared to 4.54 μB for a free Yb3+ ion

Structure refinement of (Al, Zn)49Mg32-type phases by single-crystal X-ray diffraction

2000 ◽  
Vol 294-296 ◽  
pp. 327-330 ◽  
Author(s):  
W. Sun ◽  
F.J. Lincoln ◽  
K. Sugiyama ◽  
K. Hiraga
Keyword(s):  
Single Crystal ◽  
Structure Refinement ◽  
X Ray Diffraction ◽  
X Ray
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