Polysulfonylamine, CXLVII [1]. Die ersten N,N-disulfonylierten Thioharnstoffe: Synthese von (RSO2)2N-C(S)-NMe2 (R = Me, 4-Me-C6H4) und Kristallstruktur der Ditosylverbindung / Polysulfonylamines, CXLVII [1]. The First N,N-Disulfonylated Thioureas: Synthesis of (RSO2)2N-C(S)-NMe2 (R = Me, 4-Me-C6H4) and Crystal Structure of the Ditosyl Compound

2001 ◽  
Vol 56 (11) ◽  
pp. 1188-1195 ◽  
Author(s):  
Jörg Dalluhn ◽  
Hans-Heinrich Pröhl ◽  
Oliver Moers ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Molecular Structures ◽  
Dimensional System ◽  
The Novel ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Mean Values ◽  
Guest Species ◽  
Weak Hydrogen Bonds

The moisture-sensitive title compounds were obtained in good yields by treating the corresponding silver salts AgN(SO2R)2 with the thiocarbamoyl chloride Me2NC(S)Cl in acetonitrile. In the NMR solution spectra of the novel thioureas, as recorded at room temperature for 13C and up to 120 °C for 1H, the Me2N group invariably gives rise to two distinct resonances, reflecting unusually high barriers to rotation about the C(S)-NMe2 bond. The crystal structure of the ditosyl compound (triclinic, space group P1̅, X-ray diffraction at -130 °C) contains two independent molecules A and B, in which the bond lengths and angles are nearly identical, whereas the conformations exhibit pronounced discrepancies. The amide N and thiocarbonyl C atoms have trigonal-planar environments, but the S -N -S planes are strikingly rotated into approximately perpendicular orientations relative to the planar C2N-C(S)-N moieties. Other remarkable features of the molecular structures are the exceedingly long C(S)-NS2 bonds [mean: 145.4(3) pm] and the concomitantly short C -S and C(S)-NC2 bonds [mean values: 164.8(2), 132.6(3) pm]. The packing is governed by a three-dimensional system of weak hydrogen bonds and may be viewed as a self-clathrate, in which (B)2 dimers constructed from C-H···S=C interactions are inserted as guest species into parallel tunnels between (A)∞ tapes based upon short C-H···O=S contacts.

A novel representative in the rare family of trivanadates, KMn2V3O10: synthesis, crystal structure and magnetic properties

2018 ◽  
Vol 74 (1) ◽  
pp. 97-103 ◽  
Author(s):  
Olga Yakubovich ◽  
Larisa Shvanskaya ◽  
Zlata Pchelkina ◽  
Olga Dimitrova ◽  
Anatoliy Volkov ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Exchange Interactions ◽  
Potassium Ions ◽  
The Novel ◽  
First Principles Calculations ◽  
X Ray Diffraction ◽  
Magnetic Exchange ◽  
Cell Parameters ◽  
Magnetic Couplings

Potassium dimanganese trivanadate, KMn2V3O10, was synthesized hydrothermally and its crystal structure was determined from single-crystal X-ray diffraction data. The novel phase crystallizes with triclinic symmetry in space group P\bar 1 with unit-cell parameters of a = 6.912 (5), b = 6.993 (5), c = 9.656 (5) Å, α = 101.858 (5), β = 102.627 (5), γ = 100.669 (5)°, Z = 2 and V = 432.6 (5) Å3. Its structure is built from tetramers of MnO6 octahedra sharing edges and trimers of VO4 tetrahedra sharing vertices. These main structural fragments are linked in a three-dimensional framework with channels occupied by potassium ions. The transformation of this structure to that of interconnected NaCa3Mn(V3O10)(V2O7) is discussed. The title compound orders antiferromagnetically at T N = 8.2 K due to the magnetic exchange interactions between tetramers of Mn octahedra through VO4 tetrahedra. First-principles calculations show the magnetic couplings via Mn—O—Mn and Mn—O—V—O—Mn pathways.

A fourfold interpenetrating diamond-like three-dimensional zinc(II) coordination polymer: synthesis, crystal structure and physical properties

2019 ◽  
Vol 75 (5) ◽  
pp. 504-507 ◽  
Author(s):  
Hui-Ru Chen
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
Three Dimensional ◽  
Fluorescence Emission ◽  
Crystal Structure Analysis ◽  
The Novel ◽  
X Ray Diffraction ◽  
Metal Compounds ◽  
X Ray ◽  
Coordination Framework

Excellent fluorescence properties are exhibited by d 10 metal compounds. The novel three-dimensional ZnII coordination framework, poly[[{μ2-bis[4-(2-methyl-1H-imidazol-1-yl)phenyl] ether-κ2 N 3:N 3′}(μ2-furan-2,5-dicarboxylato-κ2 O 2:O 5)zinc(II)] 1.76-hydrate], {[Zn(C6H2O5)(C20H18N4O)]·1.76H2O} n , has been prepared and characterized using IR spectroscopy, elemental analysis and single-crystal X-ray diffraction. The crystal structure analysis revealed that the compound exhibits a novel fourfold interpenetrating diamond-like network. This polymer also displays a strong fluorescence emission in the solid state at room temperature.

Crystal and molecular structure of Octacarbonylbis(diphenylarsino)-methanedimanganese(0)

1983 ◽  
Vol 36 (4) ◽  
pp. 683 ◽  
Author(s):  
BF Hoskins ◽  
RJ Steen
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Parent Compound ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Fourier Methods ◽  
X Ray

The crystal structure of the complex Mn2(CO)8(dam) (dam = Ph2AsCH2AsPh2) has been determined by three-dimensional X-ray diffraction methods. The crystals are triclinic, space group P1, with a 11.191(1), b 16.498(5), c 9.455(1) �, a 93.64(2), β 109.08(2), γ 89.36(2)� and contain two discrete, binuclear molecules of Mn2(CO)8(dam) per unit cell. The structure, solved by direct and Fourier methods, was refined by a least-squares procedure to R and Rw of 0.065 and 0.082 respectively for 1907 independent, statistically significant reflections collected by counter methods. The feature of particular interest in this compound is the accommodation of the bridging bidentate dam ligand [As.. .As separation 3.242(2) �] across a shorter Mn�-Mn� bond [2.962(3) �] which constrains the molecule so that a much less staggered configuration of the two manganese coordination octahedra is observed relative to the parent compound Mn2(CO)10, the rotation of the two equatorial planes in the former being 30�.

scholarly journals Crystal structure and spectral characterization of dimethylthallium (III) complexes with 2-mercaptonicotinic acid and esters

2004 ◽  
Vol 2 (3) ◽  
pp. 534-552 ◽  
Author(s):  
Monica Toma ◽  
Agustín Sánchez ◽  
María García-Tasende ◽  
José Casas ◽  
José Sordo ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Weak Interactions ◽  
Three Dimensional ◽  
Bidentate Ligand ◽  
Molecular Structures ◽  
Polymeric Chain ◽  
X Ray Diffraction ◽  
Methyl Nicotinate ◽  
Dimensional Network ◽  
Distorted Octahedral

AbstractSynthesis, spectral properties and crystal structure of dimethylthallium(III) complexes with 2-mercaptonicotinic acid (2mna), 2-mercapto-methyl-nicotinate (2mmn), 2-mercapto-ethyl-nicotinate (2men) and 2-mercapto-isopropyl-nicotinate (2min) are reported. The compounds were characterized using IR, multinuclear NMR (1H,13C,205Tl) and mass spectrometry (electrospray, ES-API). The molecular structures of [TlMe2(2mna)]·H2O, (1), [TlMe2(2mmn)], (2), [TlMe2(2men)], (3) and [TlMe2(2min)], (4) were determined by the single-crystal X-ray diffraction. In 1, the monodeprotonate O,S-bidentate ligand chelates one dimethylthallium (III) unit and simultaneously bridges (O and S) between two of these organometallic units. The Tl-O1′ and Tl-S″ interactions are leading to polymeric chain linked in a three-dimensional network by the hydrogen bonds formed between the water molecule and the oxygen O (2) atom of the acid. The thallium atom is in a distorted octahedral environment with a [TlC2O2S2] kernel. Compounds 2, 3 and 4 are similar, in all the cases already mentioned the ligand is NH deprotonated and is strongly coordinated to two dimethylthallium (III) units through the N and S atoms. Two additional weak interactions with the O and S atoms lead to a [TlC2NOS2] kernel for the metal atom, in which the coordination polyhedron is a very distorted octahedron with the methyl groups occupying the apical positions.

Crystal structure and spectra of the mixed-ligands complex 1-(2-thenoyl)-2-(2,2′-dipyridyl methylene)hydrazino-acetato lead (II)

1994 ◽  
Vol 209 (12) ◽  
Author(s):  
P. C. Christidis ◽  
I. A. Tossidis ◽  
C. A. Hondroudis
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Title Compound ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Mixed Ligands

AbstractThe crystal structure of the title compound has been determined from three-dimensional X-ray diffraction data. The crystals are triclinic, space group

A Three-dimensional Manganese(II) 1,2,4-Benzenetricarboxylate Hydroxide Framework with Mn–O Inorganic Sheets: Hydrothermal Synthesis and Crystal Structure

2008 ◽  
Vol 63 (11) ◽  
pp. 1339-1342 ◽  
Author(s):  
Shuxi Zhou ◽  
Yanxiong Ke ◽  
Hongliang Zou ◽  
Tianhua Liu ◽  
Fang Zhu ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrothermal Reaction ◽  
Three Dimensional ◽  
Transition Metal Ions ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Cell Parameters ◽  
3D Framework

Abstract Utilizing unsymmetrical 1,2,4-benzenetricarboxylate (1,2,4-BTC) as a ligand, a complex [Mn2.5(1,2,4-BTC)- (OH)2(H2O)] was synthesized by hydrothermal reaction and characterized by single crystal X-ray diffraction. The coordination polymer crystallizes in the triclinic space group P1̅, with cell parameters a = 5.7702(5), b = 8.0269(6), c = 12.1378(9) Å, α = 88.000(1)°, β = 81.493(1)◦, γ = 88.569(1)°, and Z = 2. In the the crystal, there are Mn- O-Mn sheets which are further connected through the 1,2,4-BTC ligands into a 3D framework, which is rare in the coordination chemistry originating from transition metal ions and unsymmetrical polycarboxylates.

scholarly journals Tetraaquabis(pyridine-3-carbonitrile-κN 1)nickel(II) benzene-1,4-dicarboxylate tetrahydrate

2021 ◽  
Vol 77 (1) ◽  
pp. 14-17
Author(s):  
Monsumi Gogoi ◽  
Birinchi Kumar Das
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Three Dimensional ◽  
Free Water ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Coordination Environment ◽  
X Ray ◽  
Graph Set

A nickel(II) terephthalate complex, viz. [Ni(C6H4N2)2(H2O)4](O2CC6H4CO2)·4H2O, has been synthesized and studied by single-crystal X-ray diffraction. It crystallizes in the triclinic space group P\overline{1}. The crystal structure shows an approximately octahedral coordination environment of the complex with the [Ni(H2O)4(3-NCpy)2]2+ (3-NCpy is pyridine-3-carbonitrile) cation associated with four free water molecules and hydrogen bonded to a terephthalate dianion [graph set R 2 2(8)]. The supramolecular structure of the compound is stabilized by a three-dimensional array of O—H...O and O—H...N hydrogen bonds, along with π–π stacked pyridine-3-carbonitrile rings and C—H...O interactions.

scholarly journals Crystal structure of bis{1-phenyl-3-methyl-4-[(quinolin-3-yl)iminomethyl-κN]-1H-pyrazol-5-olato-κO}zinc methanol 2.5-solvate from synchrotron X-ray diffraction

2017 ◽  
Vol 73 (8) ◽  
pp. 1208-1212
Author(s):  
Anatoliy S. Burlov ◽  
Valery G. Vlasenko ◽  
Pavel V. Dorovatovskii ◽  
Yan V. Zubavichus ◽  
Victor N. Khrustalev
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Complex Molecules ◽  
Triclinic Space Group ◽  
Dimensional Network ◽  
Coordination Spheres ◽  
Solvent Molecules ◽  
Zinc Cations

The title compound, [Zn(C20H15N4O)2]·2.5CH3OH, I, was synthesized via the reaction of zinc acetate with the respective ligand and isolated as a methanol solvate, i.e., as I·2.5CH3OH. The crystal structure is triclinic (space group P-1), with two complex molecules ( A and B ) and five methanol solvent molecules in the asymmetric unit. One of the five methanol solvent molecules is disordered over two sets of sites, with an occupancy ratio of 0.75:0.25. Molecules A and B are conformers and distinguished by the conformations of the bidentate 1-phenyl-3-methyl-4-[(quinolin-3-yl)iminomethyl]-1H-pyrazol-5-olate ligands. In both molecules, the zinc cations have distorted tetrahedral coordination spheres, binding the monoanionic ligands through the pyrazololate O and imine N atoms. The two ligands adopt slightly different conformations in terms of the orientation of the terminal phenyl and quinoline substituents with respect to the central pyrazololate moiety. The molecular geometries of A and B are supported by intramolecular C—H...O and C—H...N hydrogen bonds. In the crystal of I, molecules form dimers both by secondary intermolecular Zn...O [3.140 (2)–3.553 (3) Å] and π–π stacking interactions. The dimers are linked by intermolecular hydrogen bonds through the solvent methanol molecules into a three-dimensional network.

Synthesis, crystal structure and magnetic properties of diaquabis(2,6-diamino-7H-purin-1-ium-κN 9)bis(4,4′-oxydibenzoato-κO)cobalt(II) dihydrate

2018 ◽  
Vol 74 (1) ◽  
pp. 37-44 ◽  
Author(s):  
Ana María Atria ◽  
José Parada ◽  
Yanko Moreno ◽  
Sebastián Suárez ◽  
Ricardo Baggio ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Variable Temperature ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Complex Molecules ◽  
Orbital Contribution ◽  
Triclinic Space Group ◽  
Crystal Field Strength ◽  
Monodentate Coordination ◽  
Expected Position

The title mononuclear CoII complex, [Co(C5H7N6)2(C14H8O5)2(H2O)2]·2H2O, has been synthesized and its crystal structure determined by X-ray diffraction. The complex crystallizes in the triclinic space group P\overline{1}, with one formula unit per cell (Z = 1 and Z′ = 1 \over 2). It consists of a mononuclear unit with the CoII ion on an inversion centre coordinated by two 2,6-diamino-7H-purin-1-ium cations, two 4,4′-oxydibenzoate anions (in a nonbridging κO-monodentate coordination mode, which is less common for the anion in its CoII complexes) and two water molecules, defining an octahedral environment around the metal atom. There is a rich assortment of nonbonding interactions, among which a strong N+—H...O− bridge, with a short N...O distance of 2.5272 (18) Å, stands out, with the H atom ostensibly displaced away from its expected position at the donor side, towards the acceptor. The complex molecules assemble into a three-dimensional hydrogen-bonded network. A variable-temperature magnetic study between 2 and 300 K reveals an orbital contribution to the magnetic moment and a weak antiferromagnetic interaction between CoII centres as the temperature decreases. The model leads to the following values: A (crystal field strength) = 1.81, λ (spin-orbit coupling) = −59.9 cm−1, g (Landé factor) = 2.58 and zJ (exchange coupling) = −0.5 cm−1.

Crystal structure determination of the conformation of two bicyclo[3.3.1]nonan-ones

1985 ◽  
Vol 63 (6) ◽  
pp. 1166-1169 ◽  
Author(s):  
John F. Richardson ◽  
Ted S. Sorensen
Keyword(s):  
Crystal Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Molecular Structures ◽  
Boat Conformation ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Final Agreement

The molecular structures of exo-7-methylbicyclo[3.3.1]nonan-3-one, 3, and the endo-7-methyl isomer, 4, have been determined using X-ray-diffraction techniques. Compound 3 crystallizes in the space group [Formula: see text] with a = 15.115(1), c = 7.677(2) Å, and Z = 8 while 4 crystallizes in the space group P21 with a = 6.446(1), b = 7.831(1), c = 8.414(2) Å, β = 94.42(2)°, and Z = 2. The structures were solved by direct methods and refined to final agreement factors of R = 0.041 and R = 0.034 for 3 and 4 respectively. Compound 3 exists in a chair–chair conformation and there is no significant flattening of the chair rings. However, in 4, the non-ketone ring is forced into a boat conformation. These results are significant in interpreting what conformations may be present in the related sp2-hybridized carbocations.

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