Solvothermal synthesis, phase transition and crystal structure of β- and γ-CuPb3Br7

Author(s):  
Thorsten Oldag ◽  
Hans-Lothar Keller

AbstractSingle crystals of CuPb

Author(s):  
G. A. Govor ◽  
A. O. Larin ◽  
V. I. Mitsiuk ◽  
G. S. Rimskiy ◽  
T. M. Tkachenkа

The Stockbargard – Bridgman method yielded single crystals Mn0.99Fe0.01As. The effect of an external magnetic field with an intensity of up to 10 T on phase transitions in the single crystal Mn0.99Fe0.01As is studied. It is established that the magnetostructural phase transition in Mn0.99Fe0.01As is accompanied by a change in the entropy ΔSm, which is due to the transformation of the crystal structure. At temperatures above the temperature of the magnetostructural transition Tu = 290 K, the existence of an unstable magnetic structure is obtained. The magnetocaloric characteristics of the material under study are determined by an indirect calculation method based on the Maxwell thermodynamic relations and the Clapeyron – Clausius equation.


Author(s):  
L. Wiehl ◽  
X.-Q. Liu ◽  
S. Haussühl

AbstractElastic constants and thermal expansion were measured using large single crystals of monoclinic Na


1996 ◽  
Vol 51 (12) ◽  
pp. 1732-1738 ◽  
Author(s):  
Stefan Horstmann ◽  
Wolfgang Schnick

[(NH2)3PNP(NH2)3]Cl has been prepared by a three step synthesis. The last step is the ammonolysis of [Cl3PNPCl3]Cl. Single crystals of 1,1,1,3,3,3-hexaamino-1λ5, 3λ5-diphosphazenium chloride were obtained from an acetonitrile solution in a temperature gradient between 60 °C and room temperature. Between room temperature and -100 °C [(NH2)3PNP(NH2)3]Cl is subject to a phase transition. Therefore, the crystal structure was determined by single crystal X-ray methods at room temperature (P1̄, a = 584.7(1) pm, b = 732.1(1) pm, c = 1092.0(2) pm. q = 71.05(3)°, β = 76.36(3)°, γ = 89.83(3)°, Z = 2, R = 4.75 %, wR = 2.47 %). The cation [(NH2)3PNP(NH2)3]+ is built up by two corner sharing PN4 tetrahedra. Remarkably short P-N bonding distances have been observed and both PN4 tetrahedra exhibit a significant distortion resulting in two large and four small N-P-N bond angles.


2002 ◽  
Vol 57 (12) ◽  
pp. 1419-1426 ◽  
Author(s):  
Claudia Wickleder ◽  
Patrick Larsen

The dehydration of Ca(SCN)2∙4H2O yields single crystals of Ca(SCN)2 ∙ 2 H2O as well as of Ca(SCN)2. Ca(SCN)2 ∙ 2 H2O crystallizes with a hitherto unknown structure (orthorhombic, Pnma, Z = 4, a = 1280.1(2), b = 790.3(1), c = 726.9(1) pm, Rall = 0.0430). The Ca2+ ions are surrounded by four SCN− ions and four water molecules. The polyhedra are connected to chains along [010] via common oxygen atoms. The SCN− ions connect these chains to a three-dimensional network so that each thiocyanate group is linked to two Ca2+ ions. Hydrogen bonding with sulfur atoms as acceptors is observed. The crystal structure of Ca(SCN)2 (monoclinic, C2/c, Z = 4, a = 961.7(2), b = 642.4(2), c = 787.2(2) pm, Rall = 0.0673) consists of alternating layers of Ca2+ and SCN− ions. The cations are surrounded by four sulfur and four nitrogen atoms in form of a square antiprism. According to 3∞[Ca(SCN)8/4] each SCN− ion connects four Ca2+ ions with each other. Thermal investigations show a phase transition of Ca(SCN)2 ∙ 4 H2O followed by dehydration to Ca(SCN)2 which finally decomposes yielding CaS. IR and Raman measurements have been performed and the resulting frequencies assigned and discussed.


2001 ◽  
Vol 56 (1) ◽  
pp. 79-84 ◽  
Author(s):  
Michael Schur ◽  
Christian Näther ◽  
Wolfgang Bensch

Abstract Thioantimonates, Solvothermal Synthesis, Chalcogenides The reaction of elemental manganese, antimony and sulfur with ethylamine under mild solvothermal conditions yielded a thioantimonate(III) with composition Mn2(EA)2Sb2S5 (EA = C2H5NH2) that is a new member of a series of polymeric manganese thioantimo-nates(III). The structure of the title compound consists of layers of a neutral mesh-like Mn2Sb2S5 framework. The ethylamino ligands coordinated to the Mn centres separate the sheets and fill the voids within the layers formed by the interconnection of Mn2Sb2S4 hetero-cubane like building blocks. Below 273 K a reversible phase transition occurs, which is accom­panied by a doubling of the crystallographic a-axis.


2014 ◽  
Vol 70 (3) ◽  
pp. i12-i13 ◽  
Author(s):  
Andrzej Grzechnik ◽  
Christopher C. Underwood ◽  
Joseph W. Kolis

Single-crystals of CsCeF5were synthesized hydrothermally. The crystal under investigation was twinned by pseudo-merohedry with a twofold rotation around thecaxis as an additional twinning operation. The crystal structure is built of layers of distorted edge- and corner-sharing CeF8square-antiprisms. The Cs+cations are located between the layers and exhibit coordination numbers of nine. Upon compression, CsCeF5undergoes an irreversible phase transition at about 1 GPa.


Author(s):  
S. Haussühl ◽  
J. Schreuer

AbstractLarge optical quality, single crystals of triclinic ammonium hydrogen succinate have been grown from aqueous solutions. An X-ray structure analysis yields space group


2004 ◽  
Vol 59 (9) ◽  
pp. 958-962 ◽  
Author(s):  
Ina Krügermann ◽  
Mathias S. Wickleder

Single crystals of Er2(SeO4)3 ・ 8H2O were obtained by dissolving Er2O3 in selenic acid. The selenate crystallizes in the monoclinic space group C2/c (Z = 4, a = 1372.8(2), b = 687.51(7), c = 1860.2(3) pm, β = 101.85(2)◦, Rall = 0.0518) and contains the Er3+ ions in eightfold coordination of oxygen atoms that belong to two crystallographically different SeO42− ions and to four H2O molecules. According to DTA/TG measurements and temperature dependent powder diffraction data, Er2(SeO4)3 ・8H2O decomposes in several steps yielding finally Er2O3. Er2(SeO4)3 and Er2(SeO3)3 could be identified as intermediates, and for Er2(SeO4)3 a phase transition was detected.


Author(s):  
David C. Martin ◽  
Jun Liao

By careful control of the electron beam it is possible to simultaneously induce and observe the phase transformation from monomer to polymer in certain solid-state polymcrizable diacetylenes. The continuous change in the crystal structure from DCHD diacetylene monomer (a=1.76 nm, b=1.36 nm, c=0.455 nm, γ=94 degrees, P2l/c) to polymer (a=1.74 nm, b=1.29 nm, c=0.49 nm, γ=108 degrees, P2l/c) occurs at a characteristic dose (10−4C/cm2) which is five orders of magnitude smaller than the critical end point dose (20 C/cm2). Previously we discussed the progress of this phase transition primarily as observed down the [001] zone (the chain axis direction). Here we report on the associated changes of the dark field (DF) images and selected area electron diffraction (SAED) patterns of the crystals as observed from the side (i.e., in the [hk0] zones).High resolution electron micrographs (HREM), DF images, and SAED patterns were obtained on a JEOL 4000 EX HREM operating at 400 kV.


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