New crystal structures in the realm of 5,5′-azotetrazolates

2015 ◽  
Vol 70 (2) ◽  
pp. 125-134 ◽  
Author(s):  
Martin Lampl ◽  
Gerhard Laus ◽  
Doris E. Braun ◽  
Volker Kahlenberg ◽  
Klaus Wurst ◽  
...  

AbstractThe preparation of six new 5,5′-azotetrazolates with organic cations is reported. Differential scanning calorimetry of all compounds showed exothermic decompositions. The crystal structures of the six 5,5′-azotetrazolates were determined by single-crystal X-ray diffraction analyses. The phase purities of the bulk samples were confirmed by Pawley fits of the experimental and calculated powder X-ray diffraction patterns.

1999 ◽  
Vol 52 (3) ◽  
pp. 219 ◽  
Author(s):  
Philip A. Reynolds ◽  
Brian N. Figgis ◽  
Alexander N. Sobolev

The crystal structures of KOs(NH3)3(ClO4)2Cl2 and KCr(NH3)6(ClO4)2Cl2 were determined at 10 K by X-ray diffraction, and for the osmium salt also at 293 K. At 293 K the osmium salt is trigonal, space group R 3m, with the same simple structure as others of this class of double salt. At 10 K, in agreement with previous radius ratio predictions, both crystals are best described as remaining R 3m. All previously studied members, with larger alkali metal cations, are twinned R 3 at low temperatures, with small, symmetry-breaking rotations of the hexaamminemetal(III) and perchlorate ions about the threefold axis. Differential scanning calorimetry on CsRu(NH3)6(ClO4)2Cl2 suggests that the R 3m to R 3 change is very extended in temperature with only a small discontinuity at the transition temperature.


2012 ◽  
Vol 68 (3) ◽  
pp. 287-296 ◽  
Author(s):  
Boris A. Zakharov ◽  
Evgeniy A. Losev ◽  
Boris A. Kolesov ◽  
Valeri A. Drebushchak ◽  
Elena V. Boldyreva

The occurrence of a first-order reversible phase transition in glycine–glutaric acid co-crystals at 220–230 K has been confirmed by three different techniques – single-crystal X-ray diffraction, polarized Raman spectroscopy and differential scanning calorimetry. The most interesting feature of this phase transition is that every second glutaric acid molecule changes its conformation, and this fact results in the space-group symmetry change from P21/c to P\bar 1. The topology of the hydrogen-bonded motifs remains almost the same and hydrogen bonds do not switch to other atoms, although the hydrogen bond lengths do change and some of the bonds become inequivalent.


Crystals ◽  
2020 ◽  
Vol 10 (2) ◽  
pp. 106 ◽  
Author(s):  
Hisashi Konaka ◽  
Akito Sasaki

Structural changes of chloride and bromide complexes, [Ni(Et2en)2(H2O)2]Cl2 (designated as 1a) and [Ni(Et2en)2]Br2 (2a), have been investigated by using simultaneous measurements of powder X-ray diffraction (XRD) and differential scanning calorimetry data under the temperature and humidity controls. The hydrate form of chloride complex 1a was transformed into an anhydrate form (1b) by heating at a temperature of 361 K. Then the 1b was reversibly returned to the original 1a by humidification at 25% relative humidity (RH) and temperature of 300 K. On the other hand, the anhydrate form of the bromide complex 2a was first transformed into a hydrate form (2b) at 30% RH and 300 K. On heating, the 2b turned to a new anhydrate form (2c) at 344 K, and then it returned to the original form 2a on further heating. In the present experiments, a series of reactions of 2a proceeded via 2c, which was newly found with the benefit of differential scanning calorimetry (DSC) measurements performed in parallel to the XRD measurements. Crystal structures of new crystalline forms of 1b, 2b, and 2c were determined from the powder XRD data.


Author(s):  
P. Vojtíšek ◽  
I. Císařová ◽  
J. Podlaha ◽  
Z. Žák ◽  
S. Böhm ◽  
...  

AbstractCrystal structures of the title compounds were determined by single crystal X-ray diffraction. Absolute configuration of the barium salt of (+)-(


2021 ◽  
pp. 095400832110055
Author(s):  
Yang Wang ◽  
Yuhui Zhang ◽  
Yuhan Xu ◽  
Xiucai Liu ◽  
Weihong Guo

The super-tough bio-based nylon was prepared by melt extrusion. In order to improve the compatibility between bio-based nylon and elastomer, the elastomer POE was grafted with maleic anhydride. Scanning Electron Microscopy (SEM) and Thermogravimetric Analysis (TGA) were used to study the compatibility and micro-distribution between super-tough bio-based nylon and toughened elastomers. The results of mechanical strength experiments show that the 20% content of POE-g-MAH has the best toughening effect. After toughening, the toughness of the super-tough nylon was significantly improved. The notched impact strength was 88 kJ/m2 increasing by 1700%, which was in line with the industrial super-tough nylon. X-ray Diffraction (XRD) and Differential Scanning Calorimetry (DSC) were used to study the crystallization behavior of bio-based PA56, and the effect of bio-based PA56 with high crystallinity on mechanical properties was analyzed from the microstructure.


2009 ◽  
Vol 73 (3) ◽  
pp. 359-371 ◽  
Author(s):  
G. D. Gatta ◽  
N. Rotiroti ◽  
M. Zucali

AbstractThe crystalch emistry and crystal structure of naturalky anite crystals from the Eclogitic Micaschists Complex of the Sesia-Lanzo Zone, Western Italian Alps, have been investigated by means of optical microscopy, wavelength dispersive X-ray microanalysis, and single-crystal X-ray diffraction. The association of kyanite + garnet + phengitic-mica + chloritoid suggests that the eclogite-facies stages occurred at P ≤ 2.1 GPa and T ≤ 650ºC. Kyanite grains are large (cm-sized) porphyroblasts grown dynamically during one of the deformational events related to the subduction of the Austroalpine continentalcr ust. Under the polarizing microscope, kyanite grains show almost homogeneous cores, whereas rims are sometimes symplectitic aggregates of quartz and kyanite, confirming at least two stages of growth most likely related to the multistage deformational history of these rocks. Chemical analysis shows that Fe3+ is the major substituting cation for Al3+, ranging between 0.038 and 0.067 a.p.f.u.The single-crystal X-ray diffraction investigation of the kyanites shows severely textured patterns on the (h0l)*-plane. Such evidence is not observed in the unwarped diffraction patterns on (0kl)* and (hk0)*. The most significant difference between the structuralp arameters refined in this study, with respect to those of previously published unstrained gem-quality crystals, concerns the displacement parameters. The anisotropic displacement ellipsoids of all the atomic sites are significantly larger than those previously described, and systematically oriented with the largest elliptical section almost perpendicular to [010]. The larger ellipsoids in the kyanite crystal investigated here reflect the displacement of the centre of gravity of the electron distribution, rather than an anomalous atomic thermal motion. The magnitude and orientation of the displacement parameters and the textured/strained diffraction pattern may be the result of two combined effects: (1) that the kyanite crystals are actually composed of several blocks; (2) the crystals are affected by a pervasive residual strain, as a result of tectonometamorphic plastic deformations and re-crystallization.


1991 ◽  
Vol 46 (5) ◽  
pp. 566-572 ◽  
Author(s):  
Axel Gudat ◽  
Peter Höhn ◽  
Rüdiger Kniep ◽  
Albrecht Rabenau

The isotypic ternary compounds Ba3[MoN4] and Ba3[WN4] were prepared by reaction of the transition metals with barium (Ba3N2, resp.) under nitrogen. The crystal structures were determined by single crystal X-ray diffraction: Ba3[MoN4] (Ba3[WN4]): Pbca; Z = 8; a = 1083.9(3) pm (1091.8(3) pm), b = 1030.3(3) pm (1037.5(3) pm), c = 1202.9(3) pm (1209.2(4) pm). The structures contain isolated tetrahedral anions [MN4]6- (M = Mo, W) which are arranged in form of slightly distorted hexagonal layers and which are stacked along [010] with the sequence (···AB···). Two of the three Ba atoms are situated between, the third one is placed within the layers of [MN4]-groups. In this way the structures can be derived from the Na3As structure type.


2012 ◽  
Vol 8 ◽  
pp. 371-378 ◽  
Author(s):  
Katharina C Kress ◽  
Martin Kaller ◽  
Kirill V Axenov ◽  
Stefan Tussetschläger ◽  
Sabine Laschat

4-Cyano-1,1'-biphenyl derivatives bearing ω-hydroxyalkyl substituents were reacted with methyl 3-chloro-3-oxopropionate or cyanoacetic acid, giving liquid-crystalline linear malonates and cyanoacetates. These compounds formed monotropic nematic phases at 62 °C down to ambient temperature upon cooling from the isotropic liquid. The mesomorphic properties were investigated by differential scanning calorimetry, polarizing optical microscopy and X-ray diffraction (WAXS).


1990 ◽  
Vol 45 (7) ◽  
pp. 1084-1090 ◽  
Author(s):  
Klaus Praefcke ◽  
Bernd Kohne ◽  
Andreas Eckert ◽  
Joachim Hempel

Six S,S-dialkyl acetals 2a-f of inosose (1), tripodal in structure, have been synthesized, characterized and investigated by optical microscopy and differential scanning calorimetry (d.s.c.). The four S,S-acetals 2c-f with sufficiently long alkyl chains are thermotropic liquid crystalline; 2 e and 2 f are even dithermomesomorphic. Each of these four inosose derivatives 2c-f exhibits monotropically a most likely cubic mesophase (MI); in addition 2e and 2f show enantiotropically a hexagonal mesophase (Hx) with a non-covalent, supramolecular H-bridge architecture. Whereas the nature of the optically isotropic mesophase MI needs further clarification the stable high temperature mesophase Hx of 2 e and 2 f has been established by a miscibility test using a sugar S,S-dialkyl acetal also tripodal in structure and with a Hx phase proved by X-ray diffraction, but in contrast to 2 with an acyclic hydrophilic part. Similarities of structural features between the Hx-phases of 2e and 2f as well as of other thermotropic and lyotropic liquid crystal systems are discussed briefly.


Sign in / Sign up

Export Citation Format

Share Document