scholarly journals Trinodal Self-Penetrating Nets from Reactions of 1,4-Bis(alkoxy)-2,5-bis(3,2’:6’,3’’-terpyridin-4’-yl)benzene Ligands with Cobalt(II) Thiocyanate

Crystals ◽  
2019 ◽  
Vol 9 (10) ◽  
pp. 529 ◽  
Author(s):  
Giacomo Manfroni ◽  
Alessandro Prescimone ◽  
Stuart R. Batten ◽  
Y. Maximilian Klein ◽  
Dariusz J. Gawryluk ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Crystal Growth ◽  
Single Crystal ◽  
Crystal Lattice ◽  
1H Nmr ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
X Ray

The tetratopic ligands 1,4-bis(2-ethylbutoxy)-2,5-bis(3,2’:6’,3’’-terpyridin-4’-yl)benzene (1) and 1,4-bis(3-methylbutoxy)-2,5-bis(3,2’:6’,3’’-terpyridin-4’-yl)benzene (2) have been prepared and characterized by 1H and 13C{1H} NMR, IR, and absorption spectroscopies and mass spectrometry. Reactions of 1 and 2 with cobalt(II) thiocyanate under conditions of crystal growth at room temperature result in the formation of [{Co(1)(NCS)2}·MeOH·3CHCl3]n and [{Co(2)(NCS)2}·0.8MeOH·1.8CHCl3]n. Single-crystal X-ray diffraction reveals that each crystal lattice consists of a trinodal self-penetrating (62.84)(64.82)(65.8)2 net. The nodes are defined by two independent cobalt centres and the centroids of two crystallographically independent ligands which are topologically equivalent.

Die Kristall- und Molekülstruktur von Tris(dimethylamino)boran / The Crystal and Molecular Structure of Tris(dimethylamino)borane

1982 ◽  
Vol 37 (10) ◽  
pp. 1230-1233 ◽  
Author(s):  
Günter Schmid ◽  
Roland Boese ◽  
Dieter Bläser
Keyword(s):  
Molecular Structure ◽  
Crystal Growth ◽  
Single Crystal ◽  
Room Temperature ◽  
Crystal And Molecular Structure ◽  
Melting Process ◽  
Single Crystal Growth ◽  
Zone Melting ◽  
X Ray Diffraction ◽  
X Ray

Abstract Tris(dimethylamino)borane, X-ray The crystal and molecular structure of tris(dimethylamino)borane, a liquid at room temperature, has been determined by single-crystal X-ray diffraction methods at - 116°C. The single-crystal growth was accomplished by means of a miniature zone melting process on the diffractometer. The structure data are compared with those of other aminoboranes.

Single Crystal Growth and Thermoelectric Properties of Ce5Cu19P12

1998 ◽  
Vol 545 ◽  
Author(s):  
K. J. Proctor ◽  
F. J. DiSalvo
Keyword(s):  
Electrical Resistivity ◽  
Crystal Growth ◽  
Single Crystal ◽  
Single Crystals ◽  
Room Temperature ◽  
Single Crystal Growth ◽  
Room Temperature Resistivity ◽  
X Ray Diffraction ◽  
X Ray ◽  
Temperature Resistivity

AbstractSingle crystals of the known ternary cerium intermetallic Ce5Cu19P12were grown by Sn flux and I2transport methods. The long axis of the black hexagonal needles was confirmed to be the c-axis by single crystal X-ray diffraction. Electrical resistivity of both single crystals and a pressed pellet was measured from 4 - 300 K; the room temperature resistivity is about 400 μΩ-cm for the needle axis of the crystals and about 5 mΩ-cm for the pressed pellet. The thermopower of the pressed pellet was found to be 34 μV/K at room temperature.

Martensitic Transformation of Ni2.18Mn0.82Ga Single Crystal Observed by Synchrotron Radiation White X-Ray Diffraction

2005 ◽  
Vol 475-479 ◽  
pp. 2017-2020
Author(s):  
Kazuko Inoue ◽  
Yasuo Yamaguchi ◽  
Kazumasa Ohsumi ◽  
Katsuhiro Kusaka ◽  
Takeshi Nakagawa
Keyword(s):  
Crystal Growth ◽  
Martensitic Transformation ◽  
Synchrotron Radiation ◽  
Single Crystal ◽  
Room Temperature ◽  
Axial Direction ◽  
Tetragonal Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Twinning Plane

A Heusler-type Ni2.18Mn0.82Ga single crystal shows a shape memory effect. It makes a thermo-elastic martensitic transformation at around 340 K, which is coincident with a Curie temperature. We made a synchrotron radiation white X-ray diffraction of the single crystal by changing the temperature from 400 K to 103 K. We observed the change of Laue spots following the transformation. As a result of experiment, the single crystal shows one cubic Heusler structure at 400 K. The direction of the crystal growth is along cubic [010] direction. In the process of decreasing temperature, many tetragonal structures with small volume of different axial direction become to appear. At room temperature the transformation almost finishes and two tetragonal Heusler structures which are twin each other remain. One of them is nearly the same as the structure at the beginning room temperature. The direction of the crystal growth is [010] of this tetragonal structure. We found that the twinning plane of the tetragonal structure is (011) plane.

Single Crystal Growth of High-Pressure Phases of Ice and Salt Hydrate Far Below the Original Melting Point by Mixing Alcohol: Crystal Structure Determination of Magnesium Chloride Heptahydrate

2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Crystal Growth ◽  
Single Crystal ◽  
Room Temperature ◽  
Growth Technique ◽  
Salt Hydrate ◽  
X Ray

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.

scholarly journals Exploring the Structural Chemistry of Pyrophosphoramides: N,N′,N″,N‴-Tetraisopropylpyrophosphoramide

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 149-163
Author(s):  
Duncan Micallef ◽  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Room Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
X Ray

N,N′,N″,N‴-Tetraisopropylpyrophosphoramide 1 is a pyrophosphoramide with documented butyrylcholinesterase inhibition, a property shared with the more widely studied octamethylphosphoramide (Schradan). Unlike Schradan, 1 is a solid at room temperature making it one of a few known pyrophosphoramide solids. The crystal structure of 1 was determined by single-crystal X-ray diffraction and compared with that of other previously described solid pyrophosphoramides. The pyrophosphoramide discussed in this study was synthesised by reacting iso-propyl amine with pyrophosphoryl tetrachloride under anhydrous conditions. A unique supramolecular motif was observed when compared with previously published pyrophosphoramide structures having two different intermolecular hydrogen bonding synthons. Furthermore, the potential of a wider variety of supramolecular structures in which similar pyrophosphoramides can crystallise was recognised. Proton (1H) and Phosphorus 31 (31P) Nuclear Magnetic Resonance (NMR) spectroscopy, infrared (IR) spectroscopy, mass spectrometry (MS) were carried out to complete the analysis of the compound.

A comparison of room-temperature single-crystal neutron and x-ray diffraction studies of the bis(triphenylphosphine)iminium salt of the .mu.-hydro-decacarbonyldichromate(1-) monoanion

1978 ◽  
Vol 17 (12) ◽  
pp. 3460-3469 ◽  
Author(s):  
Jeffrey L. Petersen ◽  
Paul L. Johnson ◽  
Jim O'Connor ◽  
Lawrence F. Dahl ◽  
Jack M. Williams
Keyword(s):  
Single Crystal ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
X Ray ◽  
Iminium Salt

Evolution of crystal structure of dual layered molecular conductor (ET)4ZnBr4(C6H4Cl2) with temperature

CrystEngComm ◽  
2021 ◽  
Author(s):  
Gennady V. Shilov ◽  
Elena I. Zhilyaeva ◽  
Sergey M. Aldoshin ◽  
Alexandra M Flakina ◽  
Rustem B. Lyubovskii ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Electrical Resistivity ◽  
Single Crystal ◽  
Room Temperature ◽  
Organic Conductor ◽  
X Ray Diffraction ◽  
X Ray ◽  
Resistivity Measurements ◽  
Molecular Conductor ◽  
Abrupt Changes

Electrical resistivity measurements of a dual layered organic conductor (ET)4ZnBr4(1,2-C6H4Cl2) above room temperature show abrupt changes in resistivity at 320 K. Single-crystal X-ray diffraction studies in the 100-350 K range...

scholarly journals A Covalent Organic Cage Compound Acting as a Supramolecular Shadow Mask for the Regioselective Functionalization of C60

2020 ◽  
Author(s):  
Viktoria Leonhardt ◽  
Stefanie Fimmel ◽  
Ana-Maria Krause ◽  
Florian Beuerle
Keyword(s):  
Mass Spectrometry ◽  
Single Crystal ◽  
High Selectivity ◽  
Shadow Mask ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Cage Compound ◽  
Vis Spectroscopy ◽  
Regioselective Functionalization

<div><div><div><p>A trigonal-bipyramidal covalent organic cage compound serves as an efficient host to form stable 1:1-complexes with C60 and C70. Fullerene encapsulation has been comprehensively studied by NMR and UV/Vis spectroscopy, mass spectrometry as well as single-crystal X-ray diffraction. Exohedral functionalization of encapsulated C60 via threefold Prato reaction revealed high selectivity for the symmetry-matched all-trans-3 addition pattern.</p></div></div></div>

scholarly journals Magnetically Oriented Powder Crystal to Indexing and Structure Determination

2014 ◽  
Vol 70 (a1) ◽  
pp. C1560-C1560
Author(s):  
Fumiko Kimura ◽  
Wataru Oshima ◽  
Hiroko Matsumoto ◽  
Hidehiro Uekusa ◽  
Kazuaki Aburaya ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Lattice ◽  
Powder Diffraction ◽  
Diffraction Method ◽  
Lattice Parameters ◽  
X Ray Diffraction ◽  
X Ray ◽  
Crystal Lattice Parameters

In pharmaceutical sciences, the crystal structure is of primary importance because it influences drug efficacy. Due to difficulties of growing a large single crystal suitable for the single crystal X-ray diffraction analysis, powder diffraction method is widely used. In powder method, two-dimensional diffraction information is projected onto one dimension, which impairs the accuracy of the resulting crystal structure. To overcome this problem, we recently proposed a novel method of fabricating a magnetically oriented microcrystal array (MOMA), a composite in which microcrystals are aligned three-dimensionally in a polymer matrix. The X-ray diffraction of the MOMA is equivalent to that of the corresponding large single crystal, enabling the determination of the crystal lattice parameters and crystal structure of the embedded microcrytals.[1-3] Because we make use of the diamagnetic anisotropy of crystal, those crystals that exhibit small magnetic anisotropy do not take sufficient three-dimensional alignment. However, even for these crystals that only align uniaxially, the determination of the crystal lattice parameters can be easily made compared with the determination by powder diffraction pattern. Once these parameters are determined, crystal structure can be determined by X-ray powder diffraction method. In this paper, we demonstrate possibility of the MOMA method to assist the structure analysis through X-ray powder and single crystal diffraction methods. We applied the MOMA method to various microcrystalline powders including L-alanine, 1,3,5-triphenyl benzene, and cellobiose. The obtained MOMAs exhibited well-resolved diffraction spots, and we succeeded in determination of the crystal lattice parameters and crystal structure analysis.

The structures and phase transitions in 4-aminopyridinium tetraaquabis(sulfato)iron(III), (C5H7N2)[FeIII(H2O)4(SO4)2]

2019 ◽  
Vol 75 (6) ◽  
pp. 1144-1151
Author(s):  
Tamara J. Bednarchuk ◽  
Wolfgang Hornfeck ◽  
Vasyl Kinzhybalo ◽  
Zhengyang Zhou ◽  
Michal Dušek ◽  
...  
Keyword(s):  
Phase Transitions ◽  
Single Crystal ◽  
Room Temperature ◽  
Variable Temperature ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Hybrid Compound ◽  
Space Group ◽  
X Ray

The organic–inorganic hybrid compound 4-aminopyridinium tetraaquabis(sulfato)iron(III), (C5H7N2)[FeIII(H2O)4(SO4)2] (4apFeS), was obtained by slow evaporation of the solvent at room temperature and characterized by single-crystal X-ray diffraction in the temperature range from 290 to 80 K. Differential scanning calorimetry revealed that the title compound undergoes a sequence of three reversible phase transitions, which has been verified by variable-temperature X-ray diffraction analysis during cooling–heating cycles over the temperature ranges 290–100–290 K. In the room-temperature phase (I), space group C2/c, oxygen atoms from the closest Fe-atom environment (octahedral) were disordered over two equivalent positions around a twofold axis. Two intermediate phases (II), (III) were solved and refined as incommensurately modulated structures, employing the superspace formalism applied to single-crystal X-ray diffraction data. Both structures can be described in the (3+1)-dimensional monoclinic X2/c(α,0,γ)0s superspace group (where X is ½, ½, 0, ½) with modulation wavevectors q = (0.2943, 0, 0.5640) and q = (0.3366, 0, 0.5544) for phases (II) and (III), respectively. The completely ordered low-temperature phase (IV) was refined with the twinning model in the triclinic P{\overline 1} space group, revealing the existence of two domains. The dynamics of the disordered anionic substructure in the 4apFeS crystal seems to play an essential role in the phase transition mechanisms. The discrete organic moieties were found to be fully ordered even at room temperature.

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