Preparation and characterization of diethylnicotinamidium perchlorate

2008 ◽  
Vol 62 (5) ◽  
Author(s):  
Iveta Ondrejkovičová ◽  
Dušan Mikloš ◽  
Silvia Štefániková
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Ir Spectra ◽  
Title Compound ◽  
Linear Chain ◽  
Ionic Interactions ◽  
X Ray ◽  
Hydrolysis Of ◽  
Infinite Linear

AbstractThe title compound is the first example of N,N′-diethylnicotinamidium, [denaH]+, salt which has been characterized by X-ray analysis and IR spectra. [denaH]ClO4 was obtained from the reaction mixture prepared from N,N′-diethylnicotinamide (dena) and Fe(ClO4)3 in ethanol without any addition of HClO4. The proton required for protonation of dena is produced by hydrolysis of aquairon(III) cations. In the crystal structure, cations and anions are held together by ionic interactions. The cations are linked to each other by pyridinium-carbonyl N-H⋯O=C hydrogen bonds and an infinite linear chain along axis a is formed.

scholarly journals Powder study of 3-azabicyclo[3.3.1]nonane-2,4-dione form 2

2006 ◽  
Vol 62 (7) ◽  
pp. o3046-o3048 ◽  
Author(s):  
Ashley T Hulme ◽  
Philippe Fernandes ◽  
Alastair Florence ◽  
Andrea Johnston ◽  
Kenneth Shankland
Keyword(s):  
Crystal Structure ◽  
Simulated Annealing ◽  
Hydrogen Bonds ◽  
Powder Diffraction ◽  
Title Compound ◽  
Variable Temperature ◽  
Polycrystalline Sample ◽  
Asymmetric Unit ◽  
X Ray ◽  
Compound C

A polycrystalline sample of a new polymorph of the title compound, C8H11NO2, was produced during a variable-temperature X-ray powder diffraction study. The crystal structure was solved at 1.67 Å resolution by simulated annealing from laboratory powder data collected at 250 K. Subsequent Rietveld refinement yielded an R wp of 0.070 to 1.54 Å resolution. The structure contains two molecules in the asymmetric unit, which form a C 2 2(8) chain motif via N—H...O hydrogen bonds.

Systhesis, Characterization and Spectroscopic Properties of (2E,6E)-2,6-Bis(2,3,4-tri-methoxy-benzylidene)cyclohexanone

2011 ◽  
Vol 396-398 ◽  
pp. 2338-2341
Author(s):  
Xing Chuan Wei ◽  
Zhi Li Liu ◽  
Kun Zhang ◽  
Zhi Yun Du ◽  
Xi Zheng
Keyword(s):  
Crystal Structure ◽  
Acetic Acid ◽  
Hydrogen Bonds ◽  
Title Compound ◽  
Spectroscopic Properties ◽  
Spectral Studies ◽  
Double Bonds ◽  
X Ray ◽  
Π Interactions ◽  
X Ray Crystallography

In this paper, (2E,6E)-2,6-Bis(2,3,4-tri-methoxy -benzylidene)cyclohexanone (omitted as tmbcho) (1) was obtained by the reaction of acetic acid, tetrahydrofuran, cyclohexanone and 2,3,4-tri-methoxy-benzaldehyde. Three non-classic hydrogen bonds were observed in the compound. X-ray crystallography shows that the crystal structure is stabilized by intermolecular C-H•••π interactions and it contains plenty of conjugated double bonds. The title compound was characterized by UV-vis and fluorescent spectral studies.

Structural Systematics of Rare Earth Complexes. VII. Crystal Structure of Bis(2,2'/6',2␛-Terpyridinium) Octaaquaterbium(III) Heptachloride Hydrate

1994 ◽  
Vol 47 (2) ◽  
pp. 391 ◽  
Author(s):  
CJ Kepert ◽  
BW Skeleton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Rare Earth ◽  
Single Crystal ◽  
Structural Characterization ◽  
Title Compound ◽  
Room Temperature ◽  
Chloride Ions ◽  
Full Matrix ◽  
X Ray

The room-temperature single-crystal X-ray structural characterization of the title compound (tpyH2)2[Tb(OH2)8]Cl7.~2⅓H2O is recorded. Crystals are triclinic, Pī , a 17.063(5), b 16.243(3), c 7.878(3) Ǻ, α 84.78(2), β 84.39(3), γ 87.81(2)°, Z = 2 formula units; 3167 'observed' diffractometer reflections were refined by full-matrix least-squares procedures to a residual of 0.057. Notable features of interest of the compound are the 'chelation' of chloride ions by the terpyridinium cations , and the existence of a free [Tb(OH2)8]2+ cation in the presence of an abundance of chloride ions.

Boron Chelates and Boron-Metal Chelates, X [1]. 3-(2-Hydroxyphenyl)-2,2-diphenyl-1-oxa-3-azonia-2-borata-naphthalene-methanol (1/1): Synthesis, Spectroscopic Investigations and Crystal Structure

1982 ◽  
Vol 37 (11) ◽  
pp. 1450-1455 ◽  
Author(s):  
Rudolf Allmann ◽  
Eberhard Hohaus ◽  
Stanislaw Olejnik
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Structure Analysis ◽  
Title Compound ◽  
Chelate Ring ◽  
Boron Chelates ◽  
X Ray ◽  
Membered Chelate Ring ◽  
Compound C ◽  
Overall Ratio

The title compound, C25H20BNO2 · CH3OH, was examined by UV, IR, 1H, and 13C NMK spectroscopy as well as by thermogravimetry and X-ray structure analysis (Pbnb, a = 8.815, b = 17.309, c=28.992 Å, R= 5.5%). These investigations show the six-membered chelate ring (chelate A) to exist as formulated in [2] and not as a five-membered chelate ring B. One methanol molecule connects two chelate molecules by hydrogen bonds, resulting in an overall ratio of chelate to methanol of 1 : 1.

On the Origin of the Red Color of Aqueous-Solutions of 2,3-Dichloro-5,6-Dicyano-1,4-Benzoquinone (ddq). Crystal Structure of the Ammonium Salt of 2-Cyano-5,6-Dichloro-3-Hydroxy-1,4-Benzoquinone

1987 ◽  
Vol 40 (3) ◽  
pp. 625 ◽  
Author(s):  
HD Becker ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Aqueous Solutions ◽  
Single Crystal ◽  
Ammonium Salt ◽  
Structure Determination ◽  
Aqueous Ethanol ◽  
X Ray ◽  
Red Color ◽  
Hydrolysis Of

Hydrolysis of 2,3-dichloro-5,6-dicyano-1,4-benzoquinone in aqueous ethanol gives the deep-red coloured ammonium salt of a monocyano-dichloro-monohydroxy-benzoquinone which crystallizes in the tetragonal space group I41 /a, a 20.832(5), c 8.618(2) �, Z 16. Single-crystal X-ray structure determination (R 0.036 for 1185 'observed' reflections) show the presence of ammonium cations forming hydrogen bonds in the lattice alternatingly with the tautomeric anion of 2-cyano-5,6-dichloro-3-hydroxy-1,4-benzoquinone and 3-cyano-5,6-dichloro-4-hydroxy-1,2-benzoquinone.

Ammonium 4-chloropyridine-3-sulfonate

2006 ◽  
Vol 62 (4) ◽  
pp. o1488-o1489
Author(s):  
Tie-Han Li ◽  
Xin-Biao Mao ◽  
Qing-Bao Song ◽  
Chun-An Ma
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Title Compound ◽  
Three Dimensional ◽  
Dimensional Network ◽  
Hydrolysis Of

The title compound, NH4 +·C5H3ClNO3S−, was prepared by the hydrolysis of 4-chloropyridine-3-sulfonamide. In the crystal structure, a three-dimensional network is formed via N—H...O [H...O = 1.97 (3)–2.41 (2) Å] and N—H...N [H...N = 2.13 (3) Å] hydrogen bonds.

scholarly journals Crystal structure, synthesis and thermal properties of bis(4-benzoylpyridine-κN)bis(isothiocyanato-κN)bis(methanol-κN)iron(II)

2020 ◽  
Vol 76 (2) ◽  
pp. 276-280
Author(s):  
Carsten Wellm ◽  
Christian Näther
Keyword(s):  
Crystal Structure ◽  
Thermal Properties ◽  
Hydrogen Bonds ◽  
Title Compound ◽  
Aged Sample ◽  
X Ray Diffraction ◽  
Pure Sample ◽  
X Ray ◽  
Structure Synthesis ◽  
Solvent Molecules

In the crystal structure of the title compound, [Fe(NCS)2(C12H9NO)2(CH4O)2], the FeII cations are octahedrally coordinated by two N atoms of 4-benzoylpyridine ligands, two N atoms of two terminal isothiocyanate anions and two methanol molecules into discrete complexes that are located on centres of inversion. These complexes are linked via intermolecular O—H...O hydrogen bonds between the methanol O—H H atoms and the carbonyl O atoms of the 4-benzoylpyridine ligands, forming layers parallel to (101). Powder X-ray diffraction proved that a pure sample was obtained but that this compound is unstable and transforms into an unknown crystalline phase within several weeks. However, the solvent molecules can be removed by heating in a thermobalance, which for the aged sample as well as the title compound leads to the formation of a compound with the composition Fe(NCS)2(4-benzoylpyridine)2, which exhibits a powder pattern that is similar to that of Mn(NCS)2(4-benzoylpyridine)2.

scholarly journals First crystal structure of a Pigment Red 52 compound: DMSO solvate hydrate of the monosodium salt

2021 ◽  
Vol 77 (4) ◽  
pp. 402-405
Author(s):  
Lukas Tapmeyer ◽  
Daniel Eisenbeil ◽  
Michael Bolte ◽  
Martin U. Schmidt
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Dimethyl Sulfoxide ◽  
Double Layers ◽  
Ionic Interactions ◽  
Cooh Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Monosodium Salt ◽  
Printing Inks

Pigment Red 52, Na2[C18H11ClN2O6S], is an industrially produced hydrazone-laked pigment. It serves as an intermediate in the synthesis of the corresponding Ca2+ and Mn2+ salts, which are used commercially for printing inks and lacquers. Hitherto, no crystal structure of any salt of Pigment Red 52 is known. Now, single crystals have been obtained of a dimethyl sulfoxide solvate hydrate of the monosodium salt of Pigment Red 52, namely, monosodium 2-[2-(3-carboxy-2-oxo-1,2-dihydronaphthalen-1-ylidene)hydrazin-1-yl]-5-chloro-4-methylbenzenesulfonate dimethyl sulfoxide monosolvate monohydrate, Na+·C18H12ClN2O6S−·H2O·C2H6OS, obtained from in-house synthesized Pigment Red 52. The crystal structure was determined by single-crystal X-ray diffraction at 173 K. In this monosodium salt, the SO3 − group is deprotonated, whereas the COOH group is protonated. The residues form chains via ionic interactions and hydrogen bonds. The chains are arranged in polar/non-polar double layers.

The Last Missing Member of the AE2[BN2]Cl Series – Synthesis, Structural and Spectroscopic Characterization of Ba2[BN2]Cl

2008 ◽  
Vol 63 (5) ◽  
pp. 525-529 ◽  
Author(s):  
Olaf Reckeweg ◽  
Jesse Reiherzer ◽  
Armin Schulz ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Title Compound ◽  
Spectroscopic Characterization ◽  
X Ray ◽  
Fundamental Frequencies ◽  
Raman And Ir Spectra

Pale grey-blue, transparent single crystals of Ba2[BN2]Cl (I4132 (no. 214), a = 1462.88(1) pm, Z = 24) are obtained by the reaction of Ba, BaCl2, BN and NaN3 in arc-welded Ta ampoules at 1200 K. The crystal structure was determined by single crystal X-ray structure analysis. The Raman and IR spectra of the title compound show the expected fundamental frequencies (νs = 1038; νas = 1969 and 2087; δ = 616 / 636 cm−1) for a nitridoborate unit with D∞h symmetry. The [N-B-N] structure obtained by X-ray single crystal structure determination corroborates this finding within the standard deviations of the measurement with d(B-N) = 132.3(8) pm and ∡ (N-B-N) = 178.5(13)°. Our results compare well to the data reported for cubic and orthorhombic Ba3[BN2]2 as well as to the isotypic compound Ba2[BN2]Br.

Crystal and molecular structure of 9-(2,4,6-trinitroanilino)-carbazole, C18H11N5O6

1987 ◽  
Vol 65 (6) ◽  
pp. 1322-1326 ◽  
Author(s):  
Hong Wang ◽  
Richard J. Barton ◽  
Beverly E. Robertson ◽  
John A. Weil ◽  
Keith C. Brown
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Crystal And Molecular Structure ◽  
Linear Chain ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Adjacent Molecule ◽  
Neighboring Molecule ◽  
Infinite Linear

The crystal structure of 9-(2,4,6-trinitroanilino)-carbazole, C18H11N5O6, has been determined by X-ray diffraction. Crystals are monoclinic, space group P21/c, a = 14.686(11), b = 24.601(12), c = 10.047(5) Å, β = 107.76(5)° at 292 K, with Z = 8. The two nitrogen atoms in the central fragment have a staggered conformation with an N—N distance of 1.381(4) Å, which is considerably shorter than N—N distances in related N-picrylhydrazine molecules. The picryl moiety has a geometry similar to that of related N-picrylhydrazine molecules. The title compound contains an [Formula: see text] intramolecular bond to one of the ortho nitro groups on the picryl ring. The carbazole plane of one molecule and the picryl plane of a neighboring molecule overlap to form an infinite linear chain of the form … DhA:DhA … where D represents the carbazole donor, h the linear chain linkage within the molecule, and A represents the picryl acceptor of one molecule. The two interplanar distances between D of one molecule and A of an adjacent molecule are 3.28(13) and 3.34(13) Å, indicating a strong π-molecular interaction.

Sign in / Sign up

Export Citation Format

Share Document