scholarly journals Solid-state motion of OTeF5− compounds: detection by 19F NMR and IR spectroscopy and correlation with the X-ray structure of an orthorhombic crystalline modification of [C14H19N2+][OTeF5−] (C14H19N2+ = protonated 1,8-bis(dimethylamino)naphthalene)

1989 ◽  
Vol 67 (11) ◽  
pp. 2023-2029 ◽  
Author(s):  
Patti J. Kellett ◽  
Oren P. Anderson ◽  
Steven H. Strauss ◽  
Kent D. Abney
Keyword(s):  
Solid State ◽  
Nmr Spectra ◽  
Room Temperature ◽  
Variable Temperature ◽  
Structural Parameters ◽  
Crystalline Modification ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Triclinic Modification

An orthorhombic crystalline modification of [(PS)H+][OTeF5−] was studied by single crystal X-ray diffraction ((PS)H+ = protonated 1,8-bis(dimethylamino)naphthalene): orthorhombic, space group Cmcm, a = 8.607(2), b = 14.048(3), c = 13.365(2) Å, Z = 4, T = −130 °C. The structural parameters for the anion and cation in this modification (Mod-B) are very similar to those for the previously reported triclinic modification of this salt (Mod-A). However, variable temperature IR spectra for Mod-B suggest that the OTeF5− anion is exhibiting a two-site O/Fax interchange above −70 °C. Solid-state 19F NMR spectra suggest that this interchange may be as rapid as 104–105 s−1 at room temperature. Keywords: crystal structure of protonated 1,8-bis(dimethylamino)naphthalene)pentafluorotellurate(VI), polymorphism, solid state 19FNMR.

Low-temperature X-ray diffraction studies on [Cu(4-Xpz)2]x linear chain polymers (where X = Cl, Br, CH3, H; pz = pyrazolate)

1993 ◽  
Vol 71 (3) ◽  
pp. 331-334 ◽  
Author(s):  
Martin K. Ehlert ◽  
Alan Storr ◽  
Robert C. Thompson ◽  
Frederick W. B. Einstein ◽  
Raymond J. Batchelor
Keyword(s):  
Low Temperature ◽  
Room Temperature ◽  
Copper Ions ◽  
Structural Parameters ◽  
Linear Chain ◽  
Crystallographic Axis ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Cell Parameters

Room temperature and low-temperature (110–140 K) powder diffractograms have been obtained for the polymeric compounds [Cu(4-Xpz)2]x (where X = H, CH3, Cl, and Br), and values of the unit cell parameters (orthorhombic, space group Ibam) a, b, and c have been obtained at both high and low temperatures. A single crystal X-ray diffraction study of the X = H compound at 116 K was completed and the results compared with a published study done at room temperature. The structures of these complexes involve extended chains of pyrazolate-bridged copper ions extending along the c crystallographic axis. The X-ray studies indicate little change in the c parameter with decreasing temperature and small but significant changes in the a or b parameters reflecting changes in interchain packing. This study permits some evaluation of how structural parameters are affected by these variations in interchain packing and how these variations may be affecting the magnitude of magnetic exchange in the compounds.

Local Structure of Molten CdCl2 Systems

2004 ◽  
Vol 59 (11) ◽  
pp. 819-824 ◽  
Author(s):  
Y. Okamoto ◽  
H. Shiwaku ◽  
T. Yaita ◽  
S. Suzuki ◽  
K. Minato ◽  
...  
Keyword(s):  
Fine Structure ◽  
Solid State ◽  
Local Structure ◽  
Room Temperature ◽  
Structural Parameters ◽  
Molten State ◽  
Tetrahedral Coordination ◽  
X Ray Diffraction ◽  
X Ray ◽  
X Ray Absorption

The local structure of molten CdCl2 was investigated by X-ray absorption fine structure (XAFS) and X-ray diffraction(XRD) analyses. The nearest Cd2+-Cl− distance decreases from 2.61 Å in the room temperature solid state to 2.47 - 2.50 Å in the molten state. The coordination number decreases from 6 in the solid to 4 in the melt. The obtained structural parameters from the XAFS and the XRD analyses suggest that a tetrahedral coordination (CdCl4)2− is predominant in molten CdCl2. The XAFS result of a molten 50%CdCl2-KCl mixture shows that the 4-fold (CdCl4)2− structure holds also in the mixture

scholarly journals Synthesis and structure of the donor-free potassium silanide K[SiPh3]

2019 ◽  
Vol 74 (2) ◽  
pp. 153-158 ◽  
Author(s):  
Edith Alig ◽  
Isabelle Georg ◽  
Inge Sänger ◽  
Lothar Fink ◽  
Matthias Wagner ◽  
...  
Keyword(s):  
Solid State ◽  
Room Temperature ◽  
State Structure ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Solid State Structure ◽  
X Ray ◽  
Phenyl Rings ◽  
Short Contacts

AbstractThe donor-free potassium silanide K[SiPh3] was prepared by the reaction of hexaphenyldisilane, Ph3Si–SiPh3, with potassium metal in benzene at room temperature. The solid-state structure, determined by powder X-ray diffraction consists of {K[SiPh3]}2 units, which interact with adjacent dimers to form an infinite chain along the crystallographic c axis (orthorhombic, space group Cmc21, Z=4). The structure features short contacts between the π system of the phenyl rings and the potassium atoms of neighbouring K[SiPh3] units.

Variable-temperature X-ray diffraction study of structural parameters of NH---S hydrogen bonds in triethylammonium and pyridinium silanethiolates

2016 ◽  
Vol 72 (5) ◽  
pp. 763-770 ◽  
Author(s):  
Agnieszka Mielcarek ◽  
Marek Daszkiewicz ◽  
Katarzyna Kazimierczuk ◽  
Anna Ciborska ◽  
Anna Dołęga
Keyword(s):  
Hydrogen Bond ◽  
Solid State ◽  
Potential Energy ◽  
Variable Temperature ◽  
Structural Parameters ◽  
X Ray Diffraction ◽  
X Ray ◽  
Wide Range ◽  
Ft Ir ◽  
Thermochemical Parameters

Two hydrogen-bonded, well defined compounds were synthesized from tris(2,6-diisopropyl)phenoxysilanethiol (TDST) and triethylamine (TDST–TEA) or pyridine (TDST–py). The crystalline compounds were characterized in the solid state by variable-temperature X-ray diffraction measurements and ATR FT–IR spectroscopy. The toluene solutions of TDST–TEA and TDST–py were studied by NMR spectroscopy. The total hydrogen-bond energies and FT–IR spectra were calculated with the use of BLYP-D/TZP and B3LYP/6-31G(d,p)/GD3BJ methods. Thermochemical parameters and potential energy scans were calculated at the B3LYP/6-31G(d,p)/GD3BJ level. All results point to the higher energy of bonding in TDST–TEA both in the solid state and in solution. At the same time the potential energy scan reveals a very broad double-well hydrogen bond in TDST-py, indicating good stabilization of the system for a wide range ofD—H...Adistances.

scholarly journals Investigation of Solvatomorphism and Its Photophysical Implications for Archetypal Trinuclear Au3(1-Methylimidazolate)3

Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4404
Author(s):  
Shengyang Guan ◽  
David C. Mayer ◽  
Christian Jandl ◽  
Sebastian J. Weishäupl ◽  
Angela Casini ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Density Functional ◽  
Bulk Material ◽  
Variable Temperature ◽  
Active Phase ◽  
Solvent Free ◽  
X Ray Diffraction ◽  
X Ray ◽  
Aurophilic Interactions

A new solvatomorph of [Au3(1-Methylimidazolate)3] (Au3(MeIm)3)—the simplest congener of imidazolate-based Au(I) cyclic trinuclear complexes (CTCs)—has been identified and structurally characterized. Single-crystal X-ray diffraction revealed a dichloromethane solvate exhibiting remarkably short intermolecular Au⋯Au distances (3.2190(7) Å). This goes along with a dimer formation in the solid state, which is not observed in a previously reported solvent-free crystal structure. Hirshfeld analysis, in combination with density functional theory (DFT) calculations, indicates that the dimerization is generally driven by attractive aurophilic interactions, which are commonly associated with the luminescence properties of CTCs. Since Au3(MeIm)3 has previously been reported to be emissive in the solid-state, we conducted a thorough photophysical study combined with phase analysis by means of powder X-ray diffraction (PXRD), to correctly attribute the photophysically active phase of the bulk material. Interestingly, all investigated powder samples accessed via different preparation methods can be assigned to the pristine solvent-free crystal structure, showing no aurophilic interactions. Finally, the observed strong thermochromism of the solid-state material was investigated by means of variable-temperature PXRD, ruling out a significant phase transition being responsible for the drastic change of the emission properties (hypsochromic shift from 710 nm to 510 nm) when lowering the temperature down to 77 K.

The Adsorption and Chemistry of Tripropyl phosphate (TPP) into Microporous and Mesoporous NaX Zeolites

2011 ◽  
Vol 1304 ◽  
Author(s):  
Qingguo Meng ◽  
David C. Doetschman ◽  
Apostolos K. Rizos ◽  
Min-Hong Lee ◽  
Jürgen T. Schulte ◽  
...  
Keyword(s):  
Solid State ◽  
Structural Properties ◽  
Nmr Spectra ◽  
Nitrogen Adsorption ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nax Zeolite ◽  
Stoichiometric Amount ◽  
Polydiallyldimethylammonium Chloride ◽  
Adsorption Analysis

ABSTRACTAdsorption and chemistry of tripropylphosphate (TPP) in mesoporous NaX zeolite, which was templated by cationic templated polymer (polydiallyldimethylammonium chloride, PDADMAC) with two different length chains, was investigated. The structural properties of the zeolites were characterized by X-ray diffraction (XRD) and nitrogen adsorption analysis. The chemical activities of different zeolites toward the decomposition of TPP were determined with solid state 31P NMR spectra. After exposure of zeolites to TPP was sufficient and equilibrium was reached, a stoichiometric amount of water was also adsorbed and hydrolysis was observed. The TPP decomposition yields in different NaX zeolites were compared.

scholarly journals X-ray diffraction study of structure of CaO-Al2O3-SiO2 ternary compounds in molten and crystalline states

2020 ◽  
Vol 56 (2) ◽  
pp. 269-277
Author(s):  
V.E. Sokol’skii ◽  
D.V. Pruttskov ◽  
O.M. Yakovenko ◽  
V.P. Kazimirov ◽  
O.S. Roik ◽  
...  
Keyword(s):  
Short Range ◽  
Room Temperature ◽  
Short Range Order ◽  
Structural Parameters ◽  
Range Order ◽  
Reverse Monte Carlo ◽  
X Ray Diffraction ◽  
Xrd Pattern ◽  
X Ray ◽  
Ternary Compounds

Anorthite and gehlenite crystalline structure and short-range order of anorthite melt have been studied by X-ray diffraction in the temperature range from room temperature up to ~ 1923 K. The corresponding anorthite and gehlenite phases were identified as well as amorphous component for anorthite samples having identical shape to XRD pattern of the anorthite melt. The structure factor and the radial distribution function of atoms of the anorthite melt were calculated from the X-ray high-temperature experimental data. The partial structural parameters of the short-range order of the melt were reconstructed using Reverse Monte Carlo simulations.

scholarly journals Structure and electric properties of cerium substituted SrBi1.8Ce0.2Nb2O9 and SrBi1.8Ce0.2Ta2O9 ceramics

2016 ◽  
Vol 10 (3) ◽  
pp. 183-188 ◽  
Author(s):  
Mohamed Afqir ◽  
Amina Tachafine ◽  
Didier Fasquelle ◽  
Mohamed Elaatmani ◽  
Jean-Claude Carru ◽  
...  
Keyword(s):  
Dielectric Constant ◽  
Solid State ◽  
Room Temperature ◽  
Single Phase ◽  
Solid State Reaction Method ◽  
X Ray Diffraction ◽  
Reaction Method ◽  
X Ray ◽  
Lcr Meter ◽  
Curie Temperature Tc

SrBi1.8Ce0.2Nb2O9 (SBCN) and SrBi1.8Ce0.2Ta2O9 (SBCT) powders were prepared via solid-state reaction method. X-ray diffraction analysis reveals that the SBCN and SBCT powders have the single phase orthorhom-bic Aurivillius structure at room temperature. The contribution of Raman scattering and FTIR spectroscopy of these samples were relatively smooth and resemble each other. The calcined powders were uniaxially pressed and sintered at 1250?C for 8 h to obtaine dense ceramics. Dielectric constant, loss tangent and AC conductivity of the sintered Ce-doped SrBi2Nb2O9 and SrBi2Ta2O9 ceramics were measured by LCR meter. The Ce-doped SBN (SBCN) ceramics have a higher Curie temperature (TC) and dielectric constant at TC (380?C and ?? ~3510) compared to the Ce-doped SBT (SBCT) ceramics (330?C and ?? ~115) when measured at 100Hz. However, the Ce-doped SBT (SBCT) ceramics have lower conductivity and dielectric loss.

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.

Synthesis and Crystal Structure of a Cadmium(II) Complex with 2-(4΄-Chlorine-Benzoyl)-Benzoic Acid and 1,10-Phenanthroline

2011 ◽  
Vol 339 ◽  
pp. 313-316
Author(s):  
Xiu Mei Li ◽  
Zhi Tao Wang ◽  
Qing Wei Wang
Keyword(s):  
Benzoic Acid ◽  
Room Temperature ◽  
Supramolecular Network ◽  
X Ray Diffraction ◽  
Organic Complex ◽  
Orthorhombic Space Group ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Metal Organic Complex ◽  
Metal Organic

A new metal-organic complex Cd2(cbba)4(phen)2 (Hcbba = 2-(4΄-chlorine-benzoyl)- benzoic acid, phen = 1,10-phenanthroline) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, fluorescence spectrum and single-crystal X-ray diffraction. The compound crystallizes in orthorhombic, space group Pbcn with a = 12.0976(4), b = 18.0925(6), c = 31.6829(10) Å, V = 6934.6(4) Å3, C80H48Cd2Cl4N4O12, Mr = 1623.82, Dc = 1.555 g/cm3, μ(MoKα) = 0.8365 mm1, F(000) = 3264, Z = 4, the final R = 0.0396 and wR = 0.0960 for 5372 observed reflections (I > 2(I)). It exhibits a 3D supramolecular network through π-π interactions and shows green luminescent property at room temperature.

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